Lecture 21 - Fabrication of Ceramic Matrix Composites (CMCS) - Merged

Manufacturing of Composites
Prof. J. Ramkumar
Department of Mechanical Engineering
Indian Institute of Technology, Kanpur
Lecture – 21
Fabrication of Ceramic Matrix Composites
Welcome to lecture number 21. So, in this lecture, we will more focus towards
fabrication of ceramic matrix composite before getting into the different processes.
(Refer Slide Time: 00:27)
Let me once again reiterate the different toughening mechanisms which are playing a
very predominant rule in ceramic matrix composite. So, as I told you in the last class,
ceramic matrix composite is more focused towards enhancing the toughness and as well
as enhancing their high temperature behavior; so, for this, we always go for ceramic
matrix composite though the quantum wise polymeric matrix composite still dictates, but
the amount of ceramics matrix composite which are getting fabricated for various
applications in aerospace and automobile where high temperature is involved.
So, they have started moving towards ceramic matrix composite in ceramic matrix
composite the important thing is the toughening mechanism. So, there are different types
of toughening mechanism which we saw last class. So, let me write to you in detail. So,
this is one is crack bridging this is one type of toughening mechanism the next
mechanism is fiber pull out the third mechanism is going to be the de-bonding and crack
deflection next one is going to be crack pinning and the last one is going to be going to
be transformation toughening. So, these are the 5 predominant toughening mechanisms
which are involved in ceramic matrix composites. So, here because of the introduction of
reinforcement particle these are the benefits which we get. So, when we try to talk about
crack bridging yesterday we went through little bit.
So, I will just draw suppose if we have a ceramic matrix composite and these are the
fibers which run along. So, fibers run along. So, here are the cracks which are getting
bridged by the; or this reinforcing fiber tries to hold back these two parts together and
this is called as crack bridging the next one is fiber pull out. So, fiber pull out is all where
and which you have these fibers which are involved. So, here, if we are trying to have a
crack which grows like this; so, here you see the fibers are getting pull out and then the
toughening mechanism happen.
So, that the cracks do not go fast. So, you get the toughening mechanism. The next one
which we have already seen is de-bonding and crack deflection I made several figures in
the last class the SCM figured what we were discussing is on de-bonding and crack
deflection crack pinning is the other one crack pinning is these are particulate types
reinforcement. So, here are some particulates which tries to stop the crack which is
further growing.
So, these things are called as crack pinning the recent one which people have been
talking about is transformation toughening this happens predominantly by adding
zirconia as a particulate in the ceramic matrix composite.
So, let us see that in detail. So, this is the phase transformation toughening this happens
by adding tetragonal zirconium particles first point the next point is the tetragonal Zr gets
transformed under goes martensitic transformation martensitic transformation to what to
mono clinical phase this transformation which happens because of stress because of
external stress whatever we apply this transformation happens and so, because of this
transformation there is a volume expansion and this volume expansion leads to crack
arresting.
So, here the particle size is critical so; that means, to say you are supposed the it does not
happen in all zirconium size particles lesser than a critical size only this happens. So, if
you look at the schematic diagram, this is the tetragonal zirconia getting changed in the
volume and you can see these are the monolithic zirconia particles which are present in
the ceramic matrix. These are mono clinic not monolithic monoclinic monoclinic
zirconia; monoclinic zirconia. So, this is a transformation toughening mechanism this is
a fifth transformation toughening mechanism all these mechanisms are used while
building up the ceramic matrix composites.
So, this is very important why are we going to ceramic matrix composites is only to
enhance the fracture toughness behavior and then on high temperature bringing in some
changes. So, these are the two necessary things which pushes as hard to go to ceramic
matrix composite of course, ceramic matrix composites are very light as compared to
that of polymer matrix composite today the aero the complete turbine g turbines there all
completely moving toward ceramic matrix composites.
Now, let us go into the fabrication; fabrication of ceramic matrix composites. So, the
classification of infiltration what is infiltration there is a free space you are trying to push
some material inside. So, here what happens we make we try to take a ceramic powder
then we try to compact that ceramic powder into some pre-form shape and then when we
try to compact we make sure that we live enough of force through this force you can try
to push in whatever material you want. For example, you can push in polymer you can
push in metal whatever you want you can push it depends on the 4 size as well as what is
the principle of capillary action you bring in there.
So, this is; what is a basic mechanism in ceramic matrix composites fabrication. So, the
classification of infiltration method of ceramic matrix composites fabrication all the
infiltration techniques incorporates the following stages of fabrication. So, one as I told
you, we make a pre-form of whatever shape you want for example, let me take the
aluminum metal matrix composite where and which on the top alone, they have the
ceramic ceramic crown which is given for the piston further very high temperature
applications we do. So, what we do we make the piston by casting process or high
pressure die casting process then the top most potion were the crown where that it is
going to be exposed to very high temperature. So, what we do is we try to make a pre-
form. So, this pre-form can be made out of powder or it can be made out of slightly
longer fiber.
So, that is what is a pre-format a pre form is of required shape is prepared by laying and
molding the fiber reinforced phase then what we do is we deposit the inter-phase which
we discuss last time the fiber are coated with inter-phase during either the filament
production or after the pre-form formation. So, what is this I told you about the capillary
action to suck through this force? So, now, what you do is you can pressurize the other
way round is you can also give it some coating such that it of its own tries to catalyze the
processes.
So, that is deposition of interface, then third thing is infiltration; infiltration is a process
which I was talking to you about the fibrous pre-form is in filtered with a pre ceramic
fluid. So, if it does metal you take it to a liquid state ceramic if you want to take it to a
liquid state what we do we try to mix the ceramic and the form of slurry in a slurry what
we do if we try to mix it with a with a polymer substance plus we also try to mix it up
with water or alcohol. So, what happened during infiltration process we try to push the
infiltrate inside and the water can be evaporated and the polymer also can be burnt.
So, now what you get is ceramics slurry which was there; now all the burning goes up
now the ceramic gets retained. So, now, that is a how you former a ceramic matrix
composite. So, when the ceramic states that the ceramic can former reaction or it can
exist on the stage generally for what happens is it forms a small reaction there to get a
very good adhering in between the matrix and reinforcement the fluid containing either
ceramic matrix particles that that is a slurry or any other substance is mixed which is
then converted into ceramic as result of the chemical reaction and finally, what you get is
still green. So, you want to increase the hardness. So, we always go for a thermal
processing. So, the thermal processing is done the ceramic matrix forms in the space
between the fiber when the pre ceramic fluid incorporated into the reinforcing structures
heated.
So, once it is heated this ceramic returns there it forms a very good inter-phase and that is
how you make a ceramic matrix composites. So, when I said thermal process majority of
the thermal process when you do with polymer we always do pyrolysis reaction. So,
pyrolysis reaction we do. So, convert the polymer into a required ceramic material. So,
we do that or we try to do it with very high temperature isostatic process hip and other
thing where high temperature is applies. So, that we get the very good composites.
So, polymer infiltration and pyrolysis process which is otherwise called as PIP. PIP; this
is a very common process in ceramic matrix composites; so, the polymer infiltration and
pyrolysis. So, here are the steps which are there whatever I have dealt earlier the same
steps are followed step one a ceramic pre-form is formed step tow you see that you have
a infiltration with pre ceramic polymer. So, then the polymer the polymer matrix
composites is formed then what you do is you do pyrolysis; pyrolysis at 800 degrees to
1300 degrees you try to take a furnace and then try to take the temperature to that
anything about 1000 degree Celsius it demands a special kind of furnace.
So, as and when you go higher and higher and higher the furnace becomes very
expensive. So, anything about thousand the furnace cost goes high. So, 1300 degrees,
you try to maintain and then what happens all the polymer whatever is there is converted
into ceramic matrix composites whatever you get here need not be very perfect. So, what
you do is you repeat this process 3 4 times n times. So, here I have said 4 to 10 times, if
you want to have really a very good ceramic components ceramic matrix composite. So,
people have done even hundred times to get a very good output. So, if you look at the
plan view, you see the pre-form is there then infiltration polymer is done. So, then what
happens is these polymer matrix composite. So, they are form and then these the burning
happens because of pyrolysis and what you get this. So, polycarbosilane is converted into
SiC the polymer whatever was there. So, this process is called as pip. So, if you go back
to the previous slide I said the deposition inter-phase and then interface.
So, the in deposition inter-phase is some coating which is given and infiltration it has to
be a liquid which flows through. So, we always try to mix this ceramic or take a polymer
and convert it into a ceramic by pyrolysis process. So, PIP is the method of fabrication of
ceramic matrix composite comprising and infiltration of a low viscous polymer into the
reinforcing ceramic structure which is a fabric followed by pyrolysis; pyrolysis is heating
the polymer precursor in the absence of oxygen that is important if you do with any other
gas you will not be able to land up with a ceramic matrix composite. So, pyrolysis means
heating it in the absence of oxygen. So, what do we get we get a ceramic matrix
composites.
So, this process is PIP process where in which polymer use you use. So, the
polycarbosilane is covered into sic and please keep that in mind; this step is also very
important if you do not repeat the re infiltration then.
You will not be able to get the required output when you will have lot of force. So, what
is the major advantage fiber; fiber damage is prevented due to the process at a relatively
low temperature good control of the matrix composition and the microstructure can be
got the reinforcing face of different types particulate and fibers may be used particulate
when I say means you make a green you put it in a die and try to make it then the net
shaping is done. So, it is; it leads to near net shaping. So, people call this as a green
manufacturing process where and which you get the output to the required shape
dimensional and the strength properties in one shot the matrix of various composition is
silicon carbide silicon nitride and silicon can be done by changing the polymer matrix
depending upon your requirement no residual silicon is present in the matrix after
conversion.
The disadvantages it is relatively time consuming process why because you have to do
multiple re infiltration and the second thing is as we have already discussed non
destructive testing of composites since we have multiple face it is also very difficult to
find out whether we are getting hundred percent consolidation by this infiltration process
are there is a residual porosity decreasing the mechanical property because if you are not
pretty sure you stop the multiple in infiltration after six times or eight times. So, then you
might lead to force this will lower mechanical properties and it is relatively expensive
because pyrolysis furnaces are always expensive.
The next process of discussion is going to be chemical vapor deposition. So, in this
process the ceramic matrix is composite is fabricated with reactant gas this gas what
happens it undergoes a process of diffusion this diffusion in a ISO thermal porous
reform.
So; that means, to say there is a heat and you can use here long fibers long fibers ceramic
fibers can be used for making the deposition. So, here are reactant gas is used for
example, we try to form CH3Cl3Si which gives you silicon carbide plus 3 HCl. So, here
what happens this is used for making sic matrix. So, here as I said diffusion is involved.
So, it is very similar to that of this process is similar to that of CVD chemical vapor
deposition; this process is very similar to the that of chemical vapor deposition in which
there is a gas reactant gas which gets deposited on to the substrate to give a coating in
chemical vapor deposition here it is pushed into a pre-form ceramics whatever is there.
So, this one I will write the name it is methyl tri chloro silane is the gas it reacts with a
very high temperature and then it tries to form SiC; SiC is a very commonly used
ceramic matrix for various applications. So, this is otherwise also called as MTS.
So, let me write down some of the steps here. So, the deposition the pre form is filled
with gas. So, when I say gas this MTS will also sometimes we will also use some carrier
gas. So, that with this will this will try to help in deposition of faster weight. So, the
vapor reagent is generally supplied in the presence of H 2 or argon gas or helium gas in
the presents these gases are allowed to deposit and then ceramics on this reaction it tries
to form. So, this process is called as chemical vapor infiltration. So, this is the induction
heating coil where the pre-form is heated then we have this is a hot region.
So, these are the pre-forms this is the hot region whatever is there. So, vapor reagent is
pushed in from the bottom that is the MTS here. So, it is pushed in from the water. So,
the bottom and then you have a cooling a cold bottom there. So, that the gas goes inside
gets deposited and you form. So, here the temperatures are very high we always use a
graphite crucible or graphite holder is used.
So, after the reaction the gas is allowed to exhaust and it goes into the atmosphere
generally it is not in the pre atmosphere, but in into an exhaust. So, there are different
types of chemical vapor infiltration process. So, one is called as isothermal or isobaric.
So, isothermal constant temperature isobaric is also there constant pressure we can do it
that is called as I-CVI you can also I have temperature gradient TGCVI; you can also
have isothermal forced to flow IF-CVI. So, these are all variants of the process where
and which it is used for used to make the ceramic matrix composite in a high quality
output. So, the thermal gradient forced. So, if you see that it is all combination of the
isothermal and thermal gradient isothermal forced flow. So, these are some of the
different types of chemical vapor infiltration process which is used for making ceramic
matrix composite.
So, the advantages are the low fiber damage is due to low infiltration temperatures that is
one and second thing since it is gas.
So, not much of the high pressure is applied there then the matrix of the high purity can
be fabricated because it basically depends upon the gas reactant gas CVD process it is a
reaction. So, here we use than MTS for making sic the low infiltration temperatures
provides a low residual mechanical stresses which are there the enhancement in
mechanical properties in terms of strength elongation toughness can be done a good
thermal shock resistance is brought in. So, ceramic matrix composite is why is ceramic
converted into CMC is because of 2 reasons one is fracture toughness and the other one
is thermal shock resistance these 2 are the are a very valid points which are trying to
push ceramic to ceramic matrix composites.
So, in that case if you see CVI process gives you a very good thermal shock resistance
then creep and oxidation resistance the matrix of various compositions can be fabricated
sic we saw an example using MTS which gets the gas along with the reagent of hydrogen
it gets into the pre-form forms SiC plus it releases HCl also. So, you can have carbon you
can have silicon nitride you can have boron nitride boron carbide and zirconium carbide
as the matrix the inter-phases may be deposited in-situ.
So, the disadvantages are this is a slow process the porosity even after all these things
there is a porosity which is coming up 10 to 15 percent all the ceramic matrix composite
fabrication process is highly capital intensive.
And the production cost is extremely high the next process of discussion is going to be
liquid silicon infiltration process which is otherwise called as LSI liquid silicon
infiltration process is a type of reactive melt infiltration RMI technique in which the
ceramic matrix form as a result of a chemical interaction between the liquid metal
infiltrate into a porous reinforced pre-form and the substance surrounding the melt.
So, what you are trying to do is we are trying to take a we are already have a pre-form
which is made out of ceramic and then we try to react with the pre-form with the matrix
which is in liquid right and then it tries to form this composite ceramic matrix composite
for example, in LSI infiltration is used in fabrication of sic matrix composite the process
involves an infiltration of carbon micro porous pre-form into the with melt silicon at a
temperature exceeding its melting point of 1414 degree Celsius.
So, this is what it is. So, liquid silicon infiltration process polymer impregnated fiber I
told you the common steps. So, that is there from there what happens it goes to pyrolysis
it gets converted into a carbon. So, you form a carbon matrix composites right the next
one is we try to put this carbon matrix composite inside liquid silicon and then through to
capillary reaction this Si goes into this carbon matrix composite and forms SiC matrix.
So, this process is called as silicon liquid infiltration process and it is it is one of the
classification of RMI. So, it is reactive melt infiltration it tries to react. So, now, the
silicon whatever enter inside tries to react with the carbon and tries to form a silicon
carbide matrix. So, this is used. So, the reinforcement fiber can be carbon also. So, it can
be SiC dash C ceramic matrix composites and if you see all these fiber which are getting
reinforced. So, the mechanisms which we discussed in the beginning of the lecture on
wearing types of mechanism fiber breakage fiber pulled out bridging of cracks all this
things can happen in this ceramic matrix composites.
So, the advantages going to be this is low cost the production it needs a very short
production time it has very low residual porosity because you first do the polymer matrix
convert to pyrolysis and then that step also can be reiterate; for example, if you this step
can be reiterate several times to get the packing of carbon in the in between the
reinforcement.
So, thermal conductivity is very high electrical conductivity is done then it is also made
to near net shape fabrication. So, the disadvantages are the high temperature molten
silicon we are talking about a temperature of 1414 right. So, 1414; so, if you want have
1414 degree Celsius in a crucible. Now you have to see what should be the temperature
of the crucible and next on top of it what should be the heating mechanism for this
crucible. So, that you try to maintain a 1414 degree Celsius. It is really expensive and the
technology is IP it is protected technology. So, the molten silicon is maintained at a
temperature exceeding its melting point of 1414. So, the residual silicon is present in the
carbide matrix that is one problem and it has a low mechanical property.
So, that it as compared to the others the next one process is called as direct oxidation
process in direct oxidation process this is also one kind of RMI. So, here in which we
involve of formation of the matrix in the reaction of a molten metal with an oxidizing gas
that is why it is called as direct oxidation process. So, here RMI reactive metal
infiltration is done. So, here the matrix which is getting which is which is pushed into the
pre-form reacts of a molten metal reacts and then in the presence of oxygen it forms a
ceramic matrix composite.
So, the pre form of the dispersed phase is placed on a surface of a parent and molten
metal in an atmosphere where oxygen is reach. So, there are 2 conditions are necessary
for conducting this direct oxidation process one is dispersed phase is wetted by the melt
dispersed phase does not oxidize in an atmosphere of oxygen the dispersed phase; that
means, to say the pre-form; pre-form must be wetted. So, that you bring in good inter-
phase and the next thing is if it is oxidized then it will not allow the liquid metal to flow
through.
So, the liquid metal oxidizers when it is in contact with the oxygen forming a thin layer
of ceramic with some dispersed phase incorporated. So, these 2 conditions are again very
very important. So, one the dispersed phase the ceramic should be wetted and then it
should not react the liquid metal when coming in contact with the oxygen forms a thin
layer of ceramic with the silicon with the dispersed phase which brings in the ceramic
matrix composites.
So, the figure is like this molten metal. So, here are the pre-form kept here is a molten
metal. So, what we do is we try to pressure put oxygen on top right. So, then what
happened the due to capillary action or due to force this metal slowly gets inside his
mood by capillary action inside this pre-form and then in the oxygen which is there the it
reacts with the oxygen and then it tries to form a ceramic matrix composites. So, this is
the barrier. So, here is the oxygen which is reach. So, the 2 important points are is the
dispersed phase is wetted by the melt right the dispersed phase is wetted by the melt
disperse phase does not oxidize in the presence of oxygen next is the liquid metal
oxidized when comes in contact with the oxygen forms a thin ceramic layer with some
dispersed phase in incorporated into it.
So, this is a process for direct oxidation process. So, this is also part of r reactive melt
infiltration RMI. So, if you see that RMI is direct oxidation processes is a RMI process
and liquid silicone infiltration is also and RMI process.
So, what are the advantage it has low shrinkage near net shape can be made, it is
inexpensive because you do not need to have very high pressures and pushing and the
raw material is also inexpensive, it has a good mechanical property at very high
temperature in the presence and due to the absence of impurities.
It is very good, it has very low residual and porosity in it the disadvantages are going to
be it has low productivity and the residual aluminum may be present in the oxide which
tries to react and form oxides and this will try to reduce.
The mechanical properties the next process for fabrication is going to be slurry
infiltration. So, what is slurry infiltration?
So, I here; what we do if we try to make this slurry which is pre coated and then on to a
fiber. So, here is a fiber which passes through here is a slurry tank which has a mixture
slurry tank which has a mixture of polymer which has alcohol plus it tries to mix with
some ceramic. So, this is slurry. So, this slurry the fiber passes through the slurry and
then the fiber gets dried up the slurry gets dried up and then it gets into a tape form. So,
you here it is 1 D. So, you can also have 2 D; that means, to say a cloth along this
direction you can have one more which goes like this. So, you can this is. So, this is
something like a something like a mat all. So, you can have. So, this passes through and
then it goes through the die. So, in this die what happens is consolidation happens
consolidation means the slurry and the fiber they get properly wet and the excess slurry
is removed and then what we do.
Is we try to make it into a tape this tape is now cut in depending upon the orientation like
polymer matrix composite it is cut and then they are stacked on one above each other and
then they are pressed in their pressed in at; in a compression in a compression die
compression die it is pressed like a compression molding process it is press at 500 degree
Celsius and all the binders are removed once it is all removed. So, then what do we do is
we try to take the pre-form put it in a hot press at 800 to 925 degrees C and then what
happened; it tries.
Now whatever is that then this one whatever we get is a glass composite which we get
and this is called as slurry infiltration method? So, through this what we get is we get a
ceramic matrix composite; it is like your prepaid you can get the steps also their
available in market. So, here you put according to the orientation and then you try to
remove the binder first round and you can try to do why are you doing are 2 stages
because if you can directly do it at a high hot press right, but the problem is if these
binders are not removed and at hot press if it is getting removed it might stick on or it
might create force.
So, that is why we do step by step removals. So, binder is removed in the first the gases
can go away all the polymers can go away water can go away or whatever alcohol. So,
alcohol not aluminum it is alcohol the alcohol can go up and then this ceramic is residue
there and now you press it. So, all the small pores are removed.
So, you get a clear composite ceramic matrix composite. So, this slurry infiltration can
be the you can use these are the fabrics for fabrication of ceramic and ceramic glass and
glass matrix alumina can be thought of silicon; silica can be thought of glass mullite
which is the form of a glass, then I SiC and then you can also have silicon nitride Si
silicon nitride is also used in the in this slurry to; so that we can make the composites.
So, the slurry infiltration process it as an advantage of low porosity and it is has a good
mechanical properties can be achieved because of this the disadvantages are the
reinforcing fiber may be damaged because we are applying very high pressure and the 2
stages then the hot press generates relatively needs are relatively high cost equipment
and they are used for making very simple and small parts using this process.
So, the other process which is called as selective laser sintering process this is part of
rapid prototyping which is part of rapid prototyping technique. So, this is also used for
making ceramic matrix composite. So, here what do we do is we you can see here there
are 2 powder feed units are there 2 powder feed units are there. So, in between what you
have is a table. So, this is the table what you have. So, predominantly what we do is we
try to take the ceramic powder and mix it with the reinforcing powder we do the
reinforcing powder or what we do is we try to take the ceramic and try to coat the
ceramic with for example, in a slurry form we tried to coat with the reinforcing and then
we allow it to dry and keep the powder here. So, this is a powder supply if powder feed
supply is done here and here it is also there. So, what happened is there whenever the; in
rapid prototyping is always called as layer manufacturing layer manufacturing in layer
manufacturing what we do is we try to build the product layer by layer by layer.
So, layer means it one layer. So, suppose you have a cup. So, this cup is made layer by
layer it is built layer by layer by layer. So, this layer has a z has a thickness. So, this
thickness will be the layer thickness here. So, every time when you try to sink that table
by z the thickness. So, then what will happen the powder the powder feed supply unit
this will advance by a certain height and then the powder will be moved from here to the
center table that is done by a roller the roller is otherwise called as leveling roller; the
leveling roller tries to move the powder which is a ceramic and reinforcing mixed
powder into the center table.
So, now, in the center table what will happen is we will use a laser this is a laser which
comes and the laser power depends upon the material. So, the laser hits on a Galvo stage.
So, then that the information whatever was there one layer information is now
transferred to the table and the laser hits at the table and sinters the shape whatever you
have in one layer. For example, if this is a cup this is one layer, if you see the cross
section; this will be something like this something like a ring.
So, now what has happened the laser will try to establish a boundary and then it will try
to generate the thickness and then also try to have a inner boundary. So, with this one
layer information is made. So, the laser is used to hit at the work piece and then at the
table and then create a layer of information by this way you can also selectively use laser
and follow a sintering process to get a ceramic matrix composite. So, selective laser
sintering is the; is a new process which is coming to existence and people find lot of
application here we directly; since we directly make it from a from a cad. So, in rough in
selective laser sintering in rapid prototyping the steps involve on first we make a cad
model from a cad model we try to take an STL file; STL file to layer information layer
information layer information to machine to post processing if anything is required and
then we get the output.
So, since it follows this; so, any product which you want to make it into ceramic matrix
composite. So, we draw the drawing we give the figure converted into some other STL
and other formats and then bring that layer by layer information moment we have this
layer by layer information then I have explain to you how does this work. So, layer by
layer information a laser hits at one layer and tries to sinter selectively whichever places
you wants to have a material, he just burnt that and tries to do a sintering process gets
one layer of information. Now this is feed to a machine in this machine you have a laser
to do it.
So, this process is used for making near net shape manufacturing. So, instead of this
ceramic powder you can also use metal power you can also use polymer powder to get
the required output. So, here if in case you want to generate a porous structure a pre-form
can be fabricated through this process. So, that you can try to use any of the previously
discussed process where in which you infiltrate a slurry or you infiltrate a polymer to get
require ceramic matrix.
So, the matrix use for different processing route are for example, chemical vapor
deposition CVI we use matrix of carbides nitrides nitro car carbon oxides and boride. So,
these are some of the matrices used. So, viscous 2 D form that is a hot pressing and other
things we use glasses ceramics and glasses mix to use sol gel process we have not
discussed. So, sol gel process we will avoid thus it is not very popular. So, sol gel
process we use oxides; so, then polymer precursor route which we have seen for SiC si.
So, this is silicon nitride silicon carbon nitride this is what it is then liquid metal
infiltration Si to sic then gas metal reaction this is nothing, but CVI which we have
oxides then solid state hot pressing we can get SiC; Si silicon nitride prepreg curing and
polymer pyrolysis process you can have sic and silicon nitride hot pressing we can have
oxides.
So, these are the different processing routes and these are the different matrices which
we can try to get the output sol gel route which is not very popular.
So, I am not covering it in this lecture. So, here are some of the ceramic matrix; matrix
composite flame tubes which are made. So, you can see here this is oxygen ceramic
matrix composite flame tube under operation. So, this is metallic flame tubes these are
metallic flame tube after 1000 hours of operation metallic, right and this is oxygen
ceramic matrix composite flame tube after to 20000 hours you can see this high
temperature whatever was undergoing here we have used the same this is the processing
under operation.
So, when you use metal what happens after 10,000 hours when you use ceramic after
20,000 are also we do not see any change in the shape. So, this is the beauty of ceramic
matrix composites with this we will come to an end to ceramic matrix composite
processing we will see in the next lecture about nano composite; how are polymer nano
composites fabricated?
Thank you.
Prof. J. Ramkumar
Lecture - 22
Carbon - Carbon Composites
Lecture number 22. So, today we will be looking into Carbon-Carbon Composite, which
is one of the star requirement in aerospace industry. And automobile also slowly we have
started taking care of these carbon-carbon composites. Carbon-carbon composites are
where in which the matrix is a carbon the reinforcing agent is also made out of carbon.
So, in this lecture we will have a content introduction to CCC, and then we will have
different matrices. Then we will see the processing techniques, advantages and
applications.
These will be the content.

So, here a composite you are trying to use fibre, which is made out of which is made out
of carbon material. Then you will also have a matrix which is made out of carbon
material, these 2 put together we try to get a carbon-carbon composite. The function of
the filament here is to give high strength high stiffness, and it also tries to give you low
density. The matrix it has to have good shear strength property and low density. So, you
see here this is also low this is also low.
Naturally the composite what we get is going to have a very low density. So, it will have
good shear strength property from the matrix, high stiffness and high strength comes
from the fibre what we use. So, we will use fibre which is made out of carbon. So, it can
be a single wire, it can be a mat a 2 d or it can also be a 3 d. So, depending upon the
requirements we choose a proper reinforcement matrix is made out of carbon and then
we try to make composites. So, when I said matrix is made out of carbon.
So, quickly since we have studied about the ceramic matrix composite, what should
come to your mind is we will try to use a polymer we will try to do pyrolysis and we get
converted into carbon. So, this which should be the basic thought we will see the process
whatever we have lined up here.
So, matrix the matrix can be polymer matrix composite, metal matrix composite, ceramic
matrix composite, the most interesting and which is finding lot of applications are
carbon-carbon composites. Then we also have bulk metallic glass composites. This is a
next field which is coming up which is called as BMG composites. In this lecture we will
more focus towards about a CC composites.
So, a matrix; so what are the different types of carbon matrix. They are thermosetting
resins since can be thought of phenolic resins. You have furan resins, then oxidized
polystyrene we have. Then we have pan resin then we have polyvinylidene chloride. So,
this under etcetera you have many more resins which are available these are all the
possible matrix for carbon. So, you in the carbon fibre can be made out of rayon based,
can be made out of pan based, can be made out of pitch based; so rayon and pitch.
These three are the starting materials which are used for making a carbon fibre even
today the it is a state of the art technologies are available, only with few people for
making highly pure carbon fibres. Up to 90 92 percent or 95 percent it is easy to make
pure carbon fibres it is easy to make anything, above that it is IP rides it is a preparatory
item. Only very few companies across the globe hold the rights for making this carbon
fibre, they make it out of rayon pan or pitch.
These are the set of matrices where and which this can help in making a carbon matrix.
So, matrix reinforcement put together forms a carbon-carbon composites.
So, it is a family of complex advanced materials that consists of carbon fibre embedded
in a carbon matrix. So, carbon-carbon composites are those special composites in which
both the reinforcing fibre and the matrix are made out of pure carbon. They are made out
of woven mesh of carbon fibre they are used for very high strength to modulus of rigidity
they get.
And here they are they can withstand up to 3000 degree Celsius. This is very, very
important. This property makes CC composite quite usable in aerospace industries. The
space shuttle which comes back are now a day’s made out of carbon-carbon composites
which are light and weight, which can withstand very high temperatures and apart from
that lot of filaments which are used for very high temperature furnaces they are also now
a day’s made out of carbon-carbon composite because they withstand very high
temperatures. So, CC composite can be tailored to meet whatever is a customer
requirement.
And today what has happened is they put carbon-carbon fibre and then they have another
material up and down. So now, CC composite is used also as an insert. They are added in
between sandwich. So, these assume this is a metal. So, you have 2 metals and then in
between you have carbon-carbon composites for required application. Again as I told you
here it can be in the form of a woven mesh. So, this is a 3 dimensional version. So, in
this is a pre form where and which is made out of carbon-carbon-carbon fibres and
through which the carbon matrix is infused.
The carbon fibre which is used in the CC composite are tailored for to the mechanical
properties of the final structure. So, for this the carbon fibre place a very, very important
role. So, carbon fibres are having vey high strength of modulus, intermediate modulus
fibre also available in this in carbon fibre. So, this is a human hair. And this is a carbon
fibre typically the human hair goes from 60 microns 60 microns to 100 microns. This is
the size of a human hair. It varies in this range, but you look at it this will be
approximately 5 to 10 microns.
So, this is how the carbon fibre is made. So, here is the comparison between human hair
and carbon fibre.
The reinforcement, these fibres are the carbon fibres first are prepared from pitch or pan.
The carbon atom bonded together to form a long chain. So, in pitch are pan what we do
is we try to take it the carbon atoms are bonded together to form a long chain. This super
strong material that also extremely light weight is a carbon fibre. They have 5 times
stronger than steel, 2 times stiffer and about, two-third times less weight as compare to
that of steel. So, this is carbon fibre. So, you see this is an interface right fibre interface.
And this is the matrix. Carbon fibre has very good mechanical properties.
So, how is the carbon fibre prepared? So, in a pan process, we take pan and then we try
to stretch the fibre pass this fibre through a thermoset, and then we try to carbonize it.
Then graphitize it, then we try to do a surface treatment, then epoxy sizing we do and
then finally, we wind it in a spool. So, about 90 percent of the carbon fibre which are
produced today are made out of pan process. The 10 percent is made from rayon process,
and this is a very well established process.
So, because of this carbonizing and graphitizing, we need very high very high quality
processing here. So, basically it has to be a furnace, and then there has to be gas carrier
media which is there. So, these two should make sure that proper output is given. So, rest
all treatment are straight forward. So, pan they will passes through spool. So, the carbon
fibres are stretched. So, they are brought to high strain, and then it under goes in a
thermoset. It expands and it is series of rollers, then carbonizing then graphitizing. Then
you undergo this surface treatment epoxy sizing and then you try to do with spool.
So, the processing of carbon fibre; so we have carbon fibres; so these are carbon fibres
which are there you can say rough laminates. So, these are carbon fibres which are with
rough laminates. You can also see with a smooth laminar you can also see with isotropic
properties. So, these are the different processing of carbon fibres. So, with this you can
see his are the microstructures which are made, and then carbon with laminate structure,
laminar structure this is the smooth structure and isotropic structure is possible.

So, when you talk about carbon matrix. The carbon matrix in CC composite basic
function is to transfer the mechanical load between the fibres, it has to bind the fibres.
These 2 are well known. So, it acts as a binder to maintain alignment of the fibre fibres
and the fibre bundle at the same time isolate the fibre from one and other. So, this is the
basic function of a carbon matrix. The other important criteria for the selection of a
polymer precursors to form, a carbon matrix should be the there it has to have a very
high carbon yield. Why is that? Because I have, but a big list of polymers where and
which you tried to do a proper processing it gets converted into carbon matrix.
So now, what should be the selection criteria? So, that is what we have listed it here.
High carbon yield it should give it should have as minimal shrinkage during pyrolysis
process. It should be amenable with all type of polymer matrix composite, when it
follows a route of resin transfer moulding or filament winding. It should it should use
low solvent content, it should have the highest high degree of pre polymerization with
low viscosity. It should have the ability for multiple sources. It should be low cost it is
part life that the storage lifetime should be very long.
So, these are the conditions which are put in front of before choosing the polymer
precursor.
If you look at it this is a composite carbon-carbon composite, this is a carbon matrix.

And these are the fibres which are used.
If you generally the CC composite is has a nomenclature. So, this is the CCM it is
written as carbon-carbon composite it says 1 or 4. So, one stands for continuous fibre, 4
stands for chopped fibre. So, you can put that signature digit there, then 90 is the
orientation 0 90 the alignment can be put as 90 45 30 whatever it is. So, this is 0 0 means
2 d random and if you put 90 it is 0 90 orientation you can also have 45 the c is
represent. This digit represents the heat treatment temperature. C means it is processed at
a temperature between 2000 to 3632 degree Fahrenheit; if u put M, then M it is 2000
degree Celsius to 4532 degree Fahrenheit. Or it is 2000 degree Celsius, and M is 2500
degree Celsius.
So, this h represents purity how pure is the carbon-carbon composite regular grade is
purified grade SH is super purified grade. So, these are the grades. So, CCM composites
can this is the signature which it follows the first digit talks for reinforcement next digit
talks for alignment. Next digit talks for heat treatment and the last digit talks for purity of
the composite.
So, you can see here in plane and cross plane. So, here this is the product. So, you can
see in plane, and this is also in plane, this is cross plane. So, you can choose this in plane
and cross plane depending upon your requirement depending upon your final product
you choose whether to go in plane or you go for cross section; so in plane and then you
have cross section.
So, structures are there. So, what is the advantage of carbon-carbon composite. It is very
light and weight you look at it is one point to 2 grams per centimetre cube. It has very
high strength at very high temperatures. For example, cutting tools and all you look you
can (Refer Time: 13:52) they do not need strength at room temperature strength at room
temperature, strength at high temperature. This is very important. Today our requirement
are strength at high temperature requirements. Room temperature you can see the
strength will be good hardness will be good, but very high temperature the strength the
material get deformed moment at deforms.
Then it loses it is functional properties. So, high strength at high temperature is another
big advantage it is for CC composite in a non oxidized atmosphere. Then it has to have
low coefficient of thermal expansion, it has to have high thermal conductivity and it also
has to have high thermal shock resistance. When we look at ceramic matrix composite,
we said 2 properties are very important. One is the toughness property has to be
enhanced or fracture toughness property to be enhanced. That is why we go from
ceramics to ceramic matrix.
And the next is high thermal shock resistance. For a ceramic matrix composite when you
go for carbon-carbon composite also we keep this as one of the biggest criteria, or this is
one of the biggest advantage for choosing carbon-carbon composite. It has very low
weight it has very high strength at high temperatures it has very low coefficient of
expansion it has very high thermal conductivity. Today people are looking forward for
heat exchangers made out of carbon-carbon composite.

But what are the disadvantages the disadvantages are the fabrication cost is extremely
high. Because all the processes need furnaces these furnaces have should have gases in
the absence of oxygen that is one the temperature what it operates should be very high
which cannot be normally used in a in a furnace where heating coil is made out of steel
or tungsten.
Next the process leads to lot of porosities. This process is followed is very similar to that
of ceramic matrix composite. We will see that then it has poor oxidation resistance. So,
when it is done when there is a few trace of oxygen, immediately the carbon-carbon
composites the carbon matrix loses it is functional properties. It has very poor inter
laminar shear strength. So, we have to be very careful before you seek it for structural
applications. It has low oxidation resistance it reacts with oxygen even as slow at 500
degree Celsius it reacts and it form different compounds. So, the major disadvantages
cost porosity and oxygen presence puts this carbon-carbon composite into still a very
difficult component for manufacturing.
So, if you look at it Europe uses the maximum the north America uses maximum of 35
followed by Europe, which they use carbon fibre to a large extent then we use Japan uses
15 percent and the rest of the worlds uses 20 percent. So this is; what is the consumption
of carbon fibre in the global markets. So, slowly it is being used in Asian countries.
So, the applications of CC composites are it can be used for braking system where there
it is going to be a high temperature. It can be used as a refractory material. It can be used
as a hot pressed die for a turbo jet engine components they are today made out of carbon-
carbon composite. So, wherever you can replace mat ceramic matrix composite we go
for carbon-carbon composite. Ceramic has a fracture toughness property. So, here it does
not have that, but; however, making CC composite also a challenge.
So, heating elements are made out of CC composite because they can withstand very
high temperature missile cone tip because when it enters inside or when it goes outside
the atmosphere it does a huge friction coming out. So, missile cones are made out of
cone tips are made out of CC composite. The rocket motor throats are made out of it
leading edge of space shuttles are made out of it heat shielding are made x rays targets
are made out of it aircraft brake. This braking system is an automobile today even in
bikes people are started using CC composites. Aircraft brakes re-entry vehicles
biomedical implants engine piston because very high combustion if you want to have.
So, the temperature which has to be withstand by the piston should be very high. So, they
are started using CC composites then we have electronic sinks, and other automobile and
motor bike bodies are made out of carbon-carbon composites.
If you look at Boeing dreamliner 787, the composites are 50 percent made out of this,
and then we will have carbon-carbon composites carbon laminate composites are used in
the tailed region. It is also used in the wings. The carbon sandwich composites are again
used in the tails, and as well as in the wings we can see. And then it is also used in the
turbo charge the casing is all made out of it. So, the components that are used for used
uses the composite structures are almost the fuselage is made out of composite.
They are some are made out of glass fibre also, but now they are replacing it with carbon
fibres of light weight. Then upper and the lower wings wing skin are made out of it
radom is made out of it. Radom is in the front portion the wing flap elevators and the
ailerons are made out of it; the vertical fins and the horizontal stabilizers. So, these are
the horizontal vertical stabilizer which are made out of it. So now, the complete plane are
moved towards carbon-carbon are made out of carbon fibre composites, and they are also
slowly moving towards carbon-carbon composites.
So, if you look at LCA airframe, these LCA airframes, they are made out of carbon
composites you can see these are the portions which are made out of carbon composite.
And slowly they are trying to replace this carbon composite with carbon-carbon matrix
composites. So, here it was carbon composites where it was not carbon-carbon; that
means, to say here only fibre was used. And polymer was used and slowly when in the
high temperature engine. And other places they are replacing this carbon composite with
carbon-carbon fibre composite.
So, significant weight reduction is there. Significant reduction in the part count also since
it is going to composite complex shapes can be made and integration of inserts in the
parts can be made of number of parts are gone down. So, the fasteners are reduced
because basically when you use composite materials you can think of using adhesives
rather than making a hole. So, when we look into machining you will understand when
you drill a hole there will be a lot of de laminations coming into. So now, a days it has
gone to a adhesion bonding, when fatigue life is improved because we try we try to
choose proper interface between the matrix and the fibre. So, we try to enhance the
fatigue life that crack growth can be arrested. And to large extent the signatures are
reduced in the LCA frame. So, this is the carbon fibre composites 45 percent it is tried
using.
So, this is the rocket nozzle tip which is made out of carbon-carbon composite.
So, this withstands very high temperature. So, a space shuttle nose tip are made out of
carbon-carbon composites. (Refer Time: 21:34) of very high temperature.
So now slowly let us get into the fabrication methods of making CC composites. So, here
there are 4 methods which are predominantly used. Four routes sometimes a combination
of the two routes are also used. See manufacturing there is nothing called as a unique
solution. So, depending upon the availability resources depending upon the output
required. A combination is always thought of and we tried to get the required output.
So, here now we have the 4. So, one is impregnation and pyrolysis using thermosetting
resin impregnation and pyrolysis, using thermoplastic pitch precursors then we have a
CVI route we have CVD route.
So, fabrication Method here is a schematic diagram which is given; so the schematic
mechanism of pore filling and pore blocking by liquid impregnation and CVD process.
So, here what we do is we these are the pores pore entry entrance diameter, and this is
the cross section of a single pore.
So, this is pitch impregnated. So, what we have is this is pitch impregnated pore is there.
So, then what we do is we try to graphitize this pitch coke we try to do it. So, what we do
is we take this pitch impregnated, then we heat it to 2500 degree Celsius. So, then the
resin is impregnated. Then this pyrolitic carbon is formed and then the gas impregnation
early stage is like this. So, then what we do is graphitization of the pyrolitic carbon
happens, then after heating at 2500 degree Celsius, there is a graphitized pyrolitic carbon
which is getting formed and the gas impregnation final stage heat treatment to 2500
degree Celsius, we make a carbon-carbon composites by this process.
So, here is a pore this is a cross section of pore. So, this can be done by 3 routes. So, one
we tried to put the pitch here. And the pitch is impregnated here right and then what we
do is here we try to graphitize the pitch coke. Then how do we get this done we heated to
whatever it is we heated 2000 we heated to higher temperature 2500 degree Celsius, then
we it forms like this. And then we try to pitch coke is formed. Then here what we do is
we try to use the cured resin right. And then this cured resin is graphitized pyrolytic
carbon is pushed into. So, we get something like this.
So, then pyrolytic carbon is like this and this is the earliest stage of impregnation and this
gas impregnation final stage after 2500 degrees we get the required carbon-carbon
composite.
So, the fabrication method generally each of the 3 processes are carried out at a
temperature between 800 degree Celsius to 1500 degree Celsius. The final heat treatment
goes up to 3000 degree Celsius these 3 methods lead to different micro structures in the
composite partially, because of the difference in the method or the formation of carbon
from the 3 different types of precursors, but mainly because of the formation of carbon
forms having different structures and properties for different precursors. So, these are the
3 precursors with these precursors. We are trying to get different types of CC composites.
The thermosetting resin based processor for carbon-carbon composite.
The resin are usually dissolved in an organic solvent, with a catalyst slash curing agent
before infiltration the resin in the impregnated composite is cured, and then pyrolized by
heating it to a temperature of 350 to 800 degree Celsius. Frequently hot pressing at high
pressures up to 10 mega pascals and the temperature from 150 to 350 degree Celsius for
a period of 10 hours it is done had to get intense density in the curing process. Then the
final pyrolysis of the composite is subsequently graphitized at 1000 degree Celsius we
get a CCC composite. So, in this if you see very clearly time pressure and temperature.
Are very important and then here in the absence of oxygen is very, very important.

So, if you look at it following is the flow diagram for CC composite using thermosetting
resin. You have a fibre preform this is resin is getting impregnated into it, then we do up
curing. The next stage is get a prepreg then stacking of the prepreg you do curing. So,
prepreg is where already polymer is fitted into the resin. So, you have a continuous fibre
then resin impregnated. We do filament winding and then we do curing. So, when all
these things are cured you go to pyrolysis. So, pyrolysis is done up to a temperature of
800 degree Celsius, then what we do is moment the pyrolysis is over then there might be
pores or some gap in between.
So, again what we do is we try to do a resin infiltration. And this process is repeated
multiple times until you get the final required dimensions strength or thickness or
whatever it is. Then once it is done then finally, we do one more heating from 1000
degrees to 3000 degree Celsius to get the required output. Through this processing route
we try to get a carbon-carbon composites manufacture using thermosetting resin. So,
preform pre peg and then we use continuous to get the carbon-carbon composite made.
So, we can also use thermoplastic pitch based processing, so for carbon-carbon
composites.
So, the pitch impregnated preform is subjected to 2 pyrolysis carbonisation; in an inert

atmosphere to convert the organic compound to coke, and the high temperature treatment
at thousand to 2000 degree Celsius for graphitization of the coke. So, first it forms pitch
into is converted into organic component to coke, then we try to do this coke to get
graphitized of this coke to get the required output.
So, the densification process is carried out at atmospheres at atmospheric or at reduced

pressure is repeated several times to get desired density, it is more efficient process the
coke yield of for pitch increases from 50 percent to 85 percent by weight. The pressures
which are used are 70 mega pascal the pressures are also very high.
So this is; what is the route flow chart for making it. So, fibre is taken in a preform and
then we put the molten pitch in filtration is done fibre preform, molten pitch infiltration
is done then pyrolysis is taken care the molten pitch infiltration happens. Then we do one
more round of pyrolysis and we keep adding repeating the steps n number of times. And
then finally we do a final treatment at this at 2000 to 2000 2200 to 2700 degree Celsius,
to get the required output by this way we try to make carbon-carbon composites.
So, basically the resin is taken to a very high temperature. It is graphitized to get the
required output. So, this is for thermoplastic pitch based processing.
The next one is chemical vapour infiltration process. In chemical vapour infiltration
process the gaseous precursors is infiltrated into the fibre preform. This is driven by
either diffusion process or it is imposed by a external pressure. So, either you push it or
there is some phenomena which succeed capillary action. You get it done the deposition
filling fills the space between the fibre forming and the composite matrix in which the
resin is the is the deposited material. And the dispersed phase is the carbon phase the
chemical vapour infiltration is a very similar process to that of chemical vapour
deposition which we have seen in ceramic matrix composites.
So, we use here precursor gas then we use carrier media carrier gas and then what we get
is CVD. And this CVD is done on a substrate. So, on a substrate or on a fibre we try to
get the required output. So, this is c v this is CVD process or CVI process here. So, what
is the difference between the previous process and this process, in the previous process
what we do is we take a fibre we take molten pitch which is infiltrated. So, all this things
happen somewhere close to room temperature itself. But here in CVI what we do is we
try to take the precursor the precursor is a gaseous precursor which is tries to pass
through the resin fibre.
So, I said told you last time in ceramic matrix composites, we have a isothermal CVI
process, we have a thermal gradient CVI process, we have a pressure gradient CVI
process, we also have a rapid CVI process for making carbon-carbon composites.
So, here through this the reactant gas is passed through. Here is the preform carbon fibre
which is kept, this gas goes into reacts and then makes a carbon-carbon composite when
they reacts. Whatever happens is only at a nation stage or in a green stage then after this
it has to undergo 1 or 2 times of more graphitization. So, that the carbon-carbon
composites is formed. And here these vapours are infiltrated at regular intervals. So, that
you try to have a proper densification of the carbon-carbon composite.
So, these are the induction coil for heating. This is the hot region preform is used and this
is a graphite holder so that the graphite can withstand very high temperature otherwise
they would have gone for a metal one metal or a steel 1. So, and here in the bottom they
use a water jacket and then for cooling.
So, what is major advantage low fibre damage happens here, then highest purification
can be done low infiltration temperatures are required, enhanced mechanical properties
can be done. Good shock resistance happens increased creep and oxidation behaviour
comes. Interface can be deposited in-situ we want to enhance.
What are the disadvantages of this process? It is a slow process. It can take even several
weeks to have it. It has a porosity is always part of the product. So, this porosity will try
to give a very less or this will have to compromise a mechanical property. It is capital
intensive.
In CVI process this is how the CVI growth mechanism is there. You have initial fibre
which are erase these are initial fibre erase. These are initial matrix infiltration happens
right. And then what happens is this is first let us take this is one stage, and in the next
stage you keep on pumping it second time third time 4th time. So, you see that this initial
matrix which was infiltrate the thickness increases. And we were talking about the
residual pores of 10 to 15 4 percent these are the pores which are there because
completely this portion is locked.
So, once it is locked the further gases cannot go through. So, this portion is a residual
pores which is prone to happen here in CVI process the best pore; that means, to say the
lowest porosity what you can get is around about 6 percent which are reported in the
research publication, but generally it is 10 to percent.
So, what is isotherm which we are discussing? There were 4 different types of CVI. So,
what is isotherm CVI, isotherm CVI is the most widely used process and it is very
similar to that of a ceramic matrix composite. So, hear the fibre preform are heated in a
CVI reactor up to a infiltration temperature in the range of 800 degrees to 1200 degree
Celsius.
So, the in the fibre preform is heated reactor up to and infiltration temperature where the
temperature ranges from 800 degree Celsius to 1200 degree Celsius are also deposition
rate can be achieved by operating the reactor under reduced pressure, and a lower
temperature of 1050 degree Celsius.
So, this is a isotherm CVI. So, you have a process temperature of 10, 50 degrees Celsius.
The pressure is 50 millibar, the flow rate is 2 point 2 S L M. And then h 2 is to M t s ratio
is 10 is to 1. So, here this is an isotherm we push in gas inside the furnace and we start
using it.
So, if you look at the density evolution of CVI. So, over a period of time we see that 100
percent the densification keeps on increasing. So, the process duration you see here it is
almost 355 hours it is done. So, that you tried to get a final shape. So, this is the product
which was supposed to be made. So, for making this process it takes it take 355 hours.
So, the initial preform was round about point 7 k g’s the final proform mass was around
about 4.88 k gs, around about 5 k g’s.
So, there are 50 steps which are involved. So, every time what we do is we keep on
pushing gas inside after every densifique after one cycle we try to push the gas once
again. And then we start improving the densification. So, you can see the densities which
is increase from 300 to 2135 millimetre cube.
The thermal gradient CVI process in order to reduce the processing time; so if you see
here it takes isothermal it is round about 355 hours. So, in order to reduce that time what
we do is the thermal gradient under pressure gradient has been developed. So, in thermal
gradient CVI is normally performed as a cold wall CVI process. This process is very
suitable for large carbon composites such as the rocket nozzle are made out of it. The
fibre preform is placed around a mandrel here. And which is heated. The outer surface is
exposed to a cooler environment, because the proximity of water cooled cooling is
possible here.
So, this is; what is the schematic diagram for thermal gradient CVI process. This is a
graphite mandrel. So, you place your preform the gas is flown from the top. So, the
heating is maintained in the furnace. So, this is a fibre freeform this is a schematic
diagram of thermal gradient CVI process. The cooling jackets are here. You can see the
induction is given the circles are induction, and then after that you will have cooling,
then you have a preformed fibre carbon fibre preform is reinforced preform is there you
have a mandrel on which the preform is bound.
So now, you pass gas through it. So, you try to get the carbon getting infiltrated into the 3
form. So, you produce a carbon-carbon composites.
So, you also have a pressure gradient which is a small variation modification of the
isothermal CVI process. So, here are carbon fibre is placed in an isothermally heated
furnace with an outer graphite tool, which only leaves a small gap for the forced gas to
flow forced gas of the precursor to flow through. The pressure difference that forces the
gas flow through the pores is created across the walls of the structure. The process is also
limited to the production of a single or a simple shape only done here this method may
not be suitable for commercial production of CC composite parts for a large area. So, this
method is not used.

So, the schematic diagram is seen here. So, you have this is a fibre preform. This is the
gas in, this is the gas out. So, you have heating coils and here it is sir tight. So, that you
try to make simple geomentries out of it. So, there is a pressure gradient which is
maintained such that you get the CVI done for making carbon-carbon composite.
The next process is called as rapid CVI process. Rapid CVI process technique developed
by France this is still in a very, very nation states can be applied for industries language
that densification which is done is very good. In this process of the precursor of carbon
fibre preform acts as a carbon susceptor, and is fully immersed in a liquid hydrocarbon
such as cyclohexane or a toluene. So, it is immersed inside and then we do the process.
Out of the 2 hydrocarbon the carbon yield is higher toluene. The complete densification
of CC breaks can be achieved within 10 hours by this process.
So, what we do is we try to take a porous carbon fibre preform, which acts as a susceptor
and it is fully immersed inside a hydro liquid hydrocarbon and then you dry It to get the
process done very fast.
So, the other one is chemical vapour deposition. So, it is infiltration here it is deposition.
Infiltration is pushing through, deposition is you deposit on top of it. So, here the
preparation of CC fibre preforms of a desired shape and structure is done. The
densifications by the densification of the composite by CVD techniques are pretty good.
The infiltration from the pressurized hydrocarbon gas is around 900 degrees to 1200
degree Celsius. The gas is pyrolyzed from the deposition on a fibre surface. The process
duration depends upon the thickness of the preform.
The heat treatment increases the modulus of elasticity and strength, this process gives
highest strength and modulus of elasticity when we use is CVD process.
In a CVD process we use gases, and then we use a career gas. It is passed through a
furnace and where and which there is a maintained temperature of 720 degree Celsius.
This is a quartz tube and there is a quartz boat which is their parent with sample is given
by CVD the carbon is getting deposited on the fibre and we make a carbon-carbon
composite. In this process this is quite slow and second thing is here there is a possibility
of other impurities coming from.
So, there has to be a proper control on the output. The limitation of this the hydrocarbon
gas which is infiltrated into the inter filament surface and it also it forms an
interfilamental surface and a crack. Sometime this gas deposits on the outer shell and
leaves lot of pores. The infiltration and the densification is required at the it takes a long
time to do this process.
So, if you look at the properties of the CCC composite. It has excellent thermal shock,
low coefficient of expansion, high modulus high conductivity, low density high strength,
high coefficient of very low coefficient of friction, high resistance in non-oxidized
atmosphere, high operation resistance electrical conductivity. And non brittle fracture,
these are some of the properties which are good for carbon-carbon composites.
So, if you look at temperatures polymer matrix composite it can with stand a thermoset
can go up to 300 or 400 degree Celsius. This can go up to 5 degree Celsius when you
look at metal matrix composite, it can go from 400 degrees Celsius, it can go depending
upon your matrix requirement it can go up to 1000 degree Celsius. This is the service
condition where it can work. Ceramic matrix composite it can go up 1300 degree
Celsius, it can silicon nitride silicon carbide. Aluminium can go up slightly higher
temperature of 1400 degree Celsius.
Look at carbon-carbon composite, it can go up to 1500 degree Celsius service condition

easily a temperature around and when you do a graphitisation, when it is graphite it can
go up to 2000 degree Celsius. So, this makes it a very, very viable matrix for high
temperature applications.
So, if you look at specific strength at varying temperatures, you can see that carbon-
carbon composite the specific strength is almost constant up to 2000 degree Fahrenheit,
whereas aluminium there is a decline. Titanium you can see over a period of time it is
decline inconel for slightly higher temperature, and nodular iron with also there is a
decline which happens over a period of time.
So, the carbon-carbon composite maintains the strength specific strength to a for a very
high temperature as constant. So, it also depends upon the orientation. If you have this is
a flexural strength for short fibres for cloth type and then for roving type plus minus
forty roving type, plus minus 15 unidirectional fibre carbon fibre we use, and then we
tried to have multiple orientations, we can go have a flexural strength as high as 700
Newton per millimetre square.
So, if you look into it, this is as a climax for this carbon-carbon composite. So, if you see
here carbon fibre reinforced plastics strength, versus temperature the carbon fibre false
here. And moment you convert this matrix into a carbon. So, this is carbon fibre
reinforced this is carbon fibre reinforced in a carbon matrix you can see here it works
very nice from thousand 4, 1000 to 2000 degree Celsius it works excellently well. There
is no compromise in strength and. In fact, you see here this is the major advantage of
carbon-carbon composites used in very high service temperature conditions. With this we
come to the end of this carbon-carbon composites fabrication, and we have seen different
properties.
So, predominantly here we use thermoset matrix thermoplastic matrix, then we use CVI.
In CVI we have seen 4 different variations to reduce the cycle time, and to enhance the
quality of the output. We can also do exclusively CVD, but there is lot of limitation in
this process. So, that is why we do not use CVD to a large extent, we follow only CVI
process to get the carbon-carbon composites.
Thank you much.

Prof. J. Ramkumar
Lecture – 23
Polymer Matrix and Nano Composites
So, lecture number 23. So, in this lecture we will be more focused towards polymer
matrix and nano composites. So, basically what are we trying to focus is we are trying to
focus on nano materials getting integrated into the polymer matrix for producing a
composite. So, when we were talking about forms that is fibre forms or forms which are
getting reinforced, we were looking into which are like fibre, we were looking into
particulate, we were looking into whisker and nano is one more particulate type where
and which the dimensions one of the dimension will be in nanometre scale.
So, why is that required because there are certain requirements where in which we would
like to add more interface in the material. So, when we add more interface in the material
fracture toughness increases in ceramic matrix composite, as far as polymer matrix
composite is concerned it enhances the toughness property as well as wear resistance
property people have added nano materials which are conducting inside it. So, this has
led to conducting polymers.

So, in this lecture we will have the following content. So, it will be polymer composites
and the factors affecting their property, nano composites and there fillers, synthesis of
nano composite I have put in 4 processing routes, then advantage of nano composites
applications and finally, we will have conclusions.
So, factors affecting the properties of a polymer matrix composite is more towards
interfacial adhesion. So, interfacial adhesion has to be very strong, let it be a fibre let it
be a particulate or let it be nano materials. So, the interfacial factor; that means, to
adhesion factor should be very strong, the shape and the orientation plays a very
important role of the dispersed phase for example, when we talk about fibre we talk
about orientation of the fibre 0 degrees, 45 degrees, 90 degrees and the orientation which
is made so that we get a required output.
So, when we talk about shape and orientation of particulates the spherical nature of the
sphericity cubic platelet size; that means, to say we are talking about the aspect ratio it
can be regular or it can be irregular geometries, can be thought of the shape and the
orientation of the dispersed phase inclusion place a very very important role. The last one
is going to be the property of the matrix show the property of the matrix is also plays a
important roles because it has to give enough of space for a particulate to go sit there
properly to meet out the requirements.
So, here when the properties of the matrix we put costing easy process ability for
example, all thermo sets are easy to process, thermoplastic are difficult to process. Good
chemical resistance low specific gravity all those things are properties of the matrix
which are very important factor while deciding polymer matrix nano composites for
required application.
On the other hand low strength, low modulus and low operating temperature limits the
usage of a particular polymer. So, based upon the requirement we look into all those
properties and decide a polymer whether it has to be a thermo set, whether it has to be a
thermoplast or it has to be an elastomer.
When we talk about matrix so you have thermoplastic polymers, you have thermosetting
polymers, you have elastomers and their blends today we have matrices where and which
a thermo set is mixed with thermoplastic, a thermo set is mixed with elastomer to meet
out requirements. So, when we talk about thermoplastic polymers, thermoplastic
polymers consists of a linear or a branched chain molecule having strong intra molecular
bond, but weak intermolecular bond, intra and inter please have a note of it. So, intra is
within the same and inter is between 2 different particles, reshaped by application of heat
and pressure is a very common feature of thermoplastic polymers, the example for
thermoplastic polymers we have seen enough. So, I have just put down the list it is PE,
PP polystyrene polycarbonate and then so on and so forth.
When you look into thermo set polymer they have cross linked or network structure with
covalent bond with all molecules, they do not soften, but they directly decompose with
heat, once solidified the cross link process they cannot be reshaped. So, the examples are
polyester, epoxy, phenolic, furious and silicon are some of the examples of thermoset
polymer, when we talk about the composite.
So, you can see that you have un reinforced polymer which is the bend displacement, we
have we had looking into force versus bend displacement and then the next one is we are
looking at fibre reinforced composite and then the last one what we are seeing is
particulate reinforced composites. In particulate reinforced composites you see there is a
gradual fall of the force.
So, what are the advantage of polymer matrix composite? It has a very high e by r ratio.
So, a r is the density or it can be considered as row, you can make it as row its row e by
row is very important. So, you can see polymers fall in this region polymer matrix
composites fall in this region ceramics much, ceramics much higher and metal alloys fall
in this region. So, this makes polymer matrix composite more prominent for applications
where weight is an important factor.

So, if you see metal matrix composite, in metal matrix composite it increases creep
resistance. So, you can see a whisker reinforced this is the alumina whisker reinforced s i
c you can see the creep resistance behaviour this is a typical aluminum alloy, 6061
response.
So, when you look at nano composite these are the classifications, the nano composite it
can be polymer based composite due to small size of the nano particles of the structural
unit and high surface area to volume ratio this we are talking about the nano. So, nano
materials will have a very large surface area, but a very small volume. So, s by v so s is
large and volume is small. So, here what happens is we do not talk about gravitational
force we talk about, we talk about van der Waals bond, we talked about surface tension
all this small surface phenomena’s get into action and they try to dictate the process.
So, gravity is no more important when we talk about nano, density is no more important
when we talk about nano, we talk more in terms of surface to volume ratio because the
signs changes. So, due to small size of the structural units and high surface to volume
ratio these nano composites are finding, this nano particles included in nano composites
are finding large utilisation. So, when we talk about shape, these are various shapes
which are given, spherical particles will have 3 by r the fibres particle will have 2/l + 2/r,
the layered matrix will have 2/t + 4/l.
So, here r l and t represents the radius, length and the thickness respectively, note the
surface energy increases as we move macro to nano. So, if you go to macro the surface
area becomes, if you assume the surface area is the same, but volume increases. So, now,
you see the gravitational force starts playing important role. So, when you go towards
nano the surface energy the s by v ratio plays a very very important role, when you talk
about here it is non polymer based and a small amount of 5 percent of nano filler loading
resulting in a pronoun improvement in the thermal and mechanical properties. So, when
we are talking about fibre reinforcement we talk about 30 percent, 40 percent and when
you do automatically talk about 60 percent and 70 percent, but when you work on this
nano composite adding 5 percent nano fillers into the matrix itself brings in a drastic
improvement in thermal and mechanical properties.
The filler can be 0 d; that means, to say a nano particle can be 1 d which can be a nano
wire or a nano tube can be 2 d thin film coating on quantum wells or 3 d which is
embedded network or copolymers these are some of the fillers which are possible by
nano materials which are getting integrated into the composite ok.
So, what is the processing difficulty with this nano composite, nano particles have large
amount of surface charges. So, moment you have large amount of surface charges they
quickly go get agglomerated, moment it gets agglomerated then the functional property
is not uniformly distributed all across the matrix. So, you will have chunks of nano
particles loaded at few spots and some area it will be exclusively polymers. So, here in
order to break the agglomeration we always try to functionally coat the nano particle. So,
that we play with the charges, they always stay little far away and then they do not
agglomerate, this is a huge challenge.
See for example, when you have 2 huge challenges one is agglomeration, 2 the density
nano particles are always very light. So, when you try to disperse it in a polymer matrix
they will always try to come to the top and they will try to stand there and get frozen. So,
in order to have a uniform distribution we have to think of novel mechanisms where and
which these particles enter into the polymer and get dispersed then it gets cured. So,
these 2 are the major challenges.
So, this is what is a nano this is a cauliflower structure which is there of nano particles,
these are small nano particles which are dispersed in a polymer and here you can see
fibre, nano fibres which are dispersed in a polymer and this is a CNT which is dispersed
in a in a polymer CNT is carbon nano tubes and you can have single wall, multi wall. So,
you can get it done.

So, in nano composites very high surface area to volume ratio in nano structures are
there, the nano composites provides a very large interface area between the constituent
and the intermixed phase. So, the interfacial area is more, moment the interfacial area is
more when the crack grows it gets arrested very fast, it allows significant property
improvement with a very low loading at very low loading levels because the density is
low, second you will have more amount of particles individual particles present when
you try to wait.
So, you will see lot amount of particles present even at a very low loading. So,
traditionally micro particles additives require a much higher loading levels as compared
to that of nano particles; this controls the degree of interaction between the filler and the
matrix thus influencing the property. It alters the chemistry the polymer chain mobility
degree of cure and the crystallinity etcetera all these things are changed because of
adding this nano particles inside a polymer. So, that is nothing, but the nano composite
what we make.

The surface and the interfacial properties example adhesion and friction forces becomes
very critical as the material is very small, I have told discuss this point high surface area
materials have application in energy storage, catalysis battery and capacitor elements,
gas separation, filtering biochemical separations etcetera these are the areas where today
nano composite polymer matrix nano composite are used exhaustively. So, for energy
storage catalysis reaction in chemistry what we do battery and capacitor elements for
storing charges, today we talked about super capacitors where and which within very
short period of time it stores and discharges very slowly.
Then gas separation people are talking about for water filtration they will, they are trying
to have a polymer matrix composite made and they have functionalised CNT and then
they have dispersed it inside a polymer matrix these are CNTs which are functionalized
so they are dispersed in a matrix. Now what they do is they try to make small holes and
through these holes they try to pass gases and these gases are used for separation of and
then these functionalized CNT might attract the grass elements all along the way and it
releases whatever is in the pure form. So, water filtering is also done in a very similar
way to get the required output.

So, if you look at it the surface volume atomic ratio to cubic side. So, you can see that
there is a decrease in the trend and there is a increase in the trend. So, this trend is move
towards total number of atoms present and this is surface to volume atom ratio
percentage you can see it decreases with respect to cube size which is all in nanometres.
What is the unique nature of the filler which we use it is small in size very small nano
particles do not scatter light significantly possibly to make the composite with an alt
which alters electrical and mechanical properties that retains optical clarity. So, what we
are trying to tell is we are trying to say electrical property and mechanical property can
be can be changed by retaining the optical clarity; that means, to say you will have a
transparent material. So, transparent polymer which is very which will be used for vision
application, but it will also try to become electrically and mechanically stronger.
Do not create large stress concentration. So, do not compromise on the ductility of the
polymer. So, the sizes are very small. So, to a large extent that ductility sacrifices not
there. So, leads to a unique property of the particle by them self it is single valve nano
tubes are essentially molecules free from defects having modulus as high as 1 tera
Pascal, the strength as high as 500 giga Pascal, which is very difficult to get in a single
material which is got in single valve nano tubes. It leads to exceptional large interface
area in the composite the interface controls the degree of interaction between the filler
polymer and the control properties.
These are some of the unique properties which we get by using this nano in nano
particles while making composites.
In the interfacial regions this is a region beginning at a point in the fibre at which the
property is differ from those of the bulk filler and ends at the point in a matrix at which
the property becomes equal to those of the matrix. So, this is very important. So, the
property differs from those of the bulk filler and ends at the point in a matrix at which the
property equal becomes equal to that of the matrix.
So, you will have a very smooth interfacial changes that is what we trying to say, it can
be a region that alters chemistry, polymer chain, mobility and alters degree of cure and
crystalinity. The interfacial size can vary from 2 nanometre can go up to 50 nanometre,
the biggest challenge for us is to visualise this 2 nanometre it cannot be done by optical,
it cannot be majority of the time it can also be not done by electron. So, we always go
for, we always go for transmission electron.
So, here I mean to say scanning electron and this is optical microscope, scanning
electron microscope, and transmission electron microscope. So, if you want to see the
agglomeration and other things. So, it is very difficult to do in scanning electron so we
always go for transmission electron microscope. So, here we try to see very small
particles and then we also try to look at that twist anality how is it we get to see the
distribution.
So, the advantage electrical property can be changed by adding CNT, the mechanical
property can be changed because you have lot amount of toughness and the elastic
modulus and the strength of the vinyl ester component can be changed by adding
alumina particles of 40 nanometre size this also can be done. So, mechanical electrical
properties can be changed by adding these fillers.

So, the in the factors influence the microstructure and the properties of a nano composite
the surface modification of the filler and its interaction with a polymer, the filler volume
fraction, the aspect ratio of the filler and the filler alignment whether it is oriented in one
direction or it is it is randomly distributed. These are factors which tries to influence the
nano composite properties, the surface modification of the filler that is what I said
fictionalization of the so if this is a.
So, here you will add some charged particle and these charged particles try to change the
interaction with a polymer, the number of particles present is the volume fraction aspect
ratio. So, here s by v aspect ratio is very very important, the filler alignment it can be
random element or it can be oriented in one direction.

So, what are the most common synthesis route for nano composite, these are the 4 or 5
very common preparation route for nano composite solution casting, melts blending in
situ polymerization, electro spinning and electro deposition, in situ polymerization when
you do polymerization the particles gets generated of its own. So, these are nano in
shape. So, it gets dispersed.
In solution casting a polymer a solution and a nano reinforcement are combined

thoroughly mixed by ultrasonification. So, what is ultrasonification? We use a ultrasonic,
we use ultrasonic agitator, ultrasonic tool where and which we fill the polymer. So, that
tool is there. So, it tries to vibrate in 21 kilohertz with a small amplitude and creates lot
of cavities. So, these cavity bubbles keep moving towards the top and dispersing. So,
where at this we will try to disperse the nano particles and there are several tricks for
example, when you do epoxy the temperature might go very high. So, we put it in a ice
bath. So, this is an ice bath we put. So, in order to maintain the temperature of the
polymer we put it in a ice bath right.
So, it can be done, people use to disperse polyester epoxy resin and all the liquid resins
can be dispersed for example, elastomers you can also choose elastomers and dispersed
nano particles like this. So, here ultrasonification is very important because that creates
cavitation when this cavitation bubble burst then there is a space for a nanoparticle to get
inside and it gets properly mix all around. So, thoroughly mixed by an ultrasonification
and the solution or solvent is allowed to evaporate leaving behind the nano particles
typically as a thin film right.
So, ultrasonification and the solutions are solvent is allowed to evaporate leaving along
the things. So, all these nano particles will form a thin film or it can be uniformly
dispersed, now you pour it inside a die you get a nano composite. The solvent or the
solution chosen should completely dissolve and the polymer as well as disperse the nano
particles, the solution solvent used with the help in the mobility of the polymer chain
which in turn helps in inter calcination of the polymer chain with the layered nano
reinforcement leads to a nano composite.
So, you can do like this or you can try to have polymer which is blend in a solvent, nano
particles blend in a solvent both the solvents mix together evaporated form a thin film get
a nano composite. So, this is what it is. So, this is called as solution casting.
So, the major advantage is going to be the great the greater the film thickness uniformity
will be there, wide range of films can be made the film that are gel and a pin hole free.
The excellent flatness and dimension stabilities can be got isotropic property orientation
as film is not stretched during manufacturing you get a very good isotropic orientation,
then absence of extrusion process lubricants and then it is suitable the suitability of the
polymer solution casting is evaluated case by case cases according to the product
formation.

So, this is what is a solution casting u c p u it is getting formed. So, you heat it to a
certain temperature, measure the stir the particle the new nano sonicated then you add all
the nano particles into it then you stir it and then you heat it. So, you allow all the
solvents to evaporate or you leave it as a polymer. So, it gets uniformly dispersed then
finally, you do degassing and then from the degassing you try to pour it on a spin coating
and then its forms a small thin uniform layer you can either do it in the spin coating
machine or if you want you can even go ahead casting it. So, this is what it is so here p u
then it is mixed with a solvent so you mix it here then it is stirred.
So, uniform dispersion this is a stirring action, stirring action is uniform dispersion of
solvent and polymer or polymer inside everything then you try to take the nano valve
whatever CNT or nano material and then disperse it in a in a liquid. So, this liquid is
again dispersed is inside the polymer. So, it sonicated for 15 minutes and you say 70
percent amplitude they have set. So, 70 percent of maybe 10 microns are 50 microns they
do it and then they try to vibrated it then pour this solvent, this solvent then you allow it
to cure de gas it get it and then this can be casted or it can be spin coated. So, that you
get a thin film of whatever polymer you want.
The manufacturing process advantage of polymer solution casting over the traditional
film extrusion method is included, the process the processing happens at low temperature
it is valuable for thermally activated films or application incorporating temperature
sensitive active ingredients. The ability to produce high temperature resistant films from
non thermoplastic, but soluble raw materials can be done simplified incorporation of
additives and fillers can be done in this quicker change over for platforms which may,
which many part numbers that are differentiated based on the formulas can be done here
single pass manufacturing of multilayer films can be done. So, you can also make
functionally graded materials also can be done, every spin coat layer can have varying
volume fractions and you can have a functionally graded material, wided range of
material choice with casting from either acquiescent or solvent based solutions can be
done.
The basic material intended to use and numerous other considerations are specific
benefits are realised for the following applications is acrylic and the other polymer films
deliver superior optical properties and thicker and thickness uniform. When you talk
about polyurethane film improves mechanical properties such as elimination of pin holes
or voids also ensures film uniformity high optical clarity and production of thin films
which can be easily customised with added functional layer and properties. The
thermoset additive films where melt extrusion is not feasible we try to do it the thermal
interfacial material addition of more concentration thermally conductive fillers than the
feasible of the melt extrusion process can be done here, electro active polymer films can
also be made by this process.
So, the melts blending is the other process we take a polymer, we take a nano material it
is extruded it is intensive mixing is happened then it is pressing using a die and then you
get a nano composite in this method the polymer mobility simply comes out from the
thermal energy.
So, this is melts blending process schematic diagram. So, here you try to take the
polymer and then what you do is you try to extrude it at 240 degree Celsius 100 r p m
you try to do this and then you try to mix it up, you put it in a compression mould and
then you try to pressing at 240 degrees for 5 minutes and what you get is a thin film
which is done by melt blending.
So, this is a thermo plastic polymer which is taken it is extruded and then you try to get
it, there are twin screw extruder which are used where and which you can even dispersed
solid nano particles and then you try to dispersive it to get it is extruded. It is like an
injection moulding machine, twin screw extruders injection moulding you directly
injected into a die to get the required part.
So, this is a model of the experimental line for preparing PET functional foils making a
nano dispersion liquid by blend milling. So, here we make PET granulars wire melt
blending process and the preparation of the infrared shielding foil by adding a PET
granular above. So, here you can see that. So, we make a powder dispersion in a liquid
granules are made these granules are rolled and then when you roll we try to add this
here we add nano particles, granules nano particles is added you roll and then you stretch
it and then you get PET foils and then this foils are rolled up into this. So, that it can be
sold at commercial applications.

So, what is the advantage here, naturally the advantages going to be it is going to have
higher strain and the number of defects are going to be less in melt blending. So, shows a
higher gas barrier performance compared to that of solution casting, the here formed
exfoliated nanostructure while those prepared with the solution exhibits inter calcinated
structures only. So, here it is much more stronger than the solution casting, the melt
blending film shows higher creep resistance than the inter calcinated once. T he nano
composite films show superior physical properties and can be prepared with m b method
are easy and environmental friendly techniques can be used. So, melt blending method is
always beneficial than the solution casting method.
The next topic of discussion is going to be in situ polymerization. So, in situ means I
think it is getting developed while the process is going on by adding 2 independent
elements you add together and then it mixes it tries to generate a polymer nano
composite.

So, in situ polymerization as you all know lot of mass together to form a polymer. So, in
situ polymerization in this there are 2 important discussions to be carried out this is with
regard to the nano material which is getting reinforced inside the polymer material. There
are 2 process one is called as inter calcination the other one is called as exfoliation, as
you know in nano composites they are charged there if lot of charge around the nano
composite it is going to create agglomeration. So, I have to separate these nano particles.
So, basically I try to do functionalization and in the same thing a nano particle can have
multiple layers and each layer it will be a nanometre. So, I want to separate these layers
one from each other such that the agglomeration does not happen, for this what we go
ahead is we do this inter calcination and exfoliation.
Inter calcination is the reversible process like reversible inclusion or insertion of

molecule or ion into the material with layered structure. So, this is very clear inter
calcination and extra exfoliation can happen only with layered nano particles or layered
nano materials. So, what I try to do here is I tried to separate these layers for example; I
have several layers of some materials stack to each other. So, what I do is I tried to put
spacer in between. So, what has happened I have now separated the layers so that is what
is happening in inter calcination. So, I tried to add a material such that this material is
getting included into the nano layers and it separates out nano layers, the inter calcination
expands the van der Waals gap. So, as I told you in nano materials all the van der Waals
forces surface tension all these things play a very very important role, the van der Waals
gap between the sheets which is which requires energy what we do is we try to push in
this material this ion or a molecule inside such that it separates out usually this energy is
supplied by charge transfer between the guest and the host solid.
So, guest these are these are the guest these are the host solids I try to have separations
such that you can now get layers of nano structure. Exfoliation is nothing, but an extreme
case of inter calcination, in inter calculation if you still see that there is an attachment
between the layers now I get layer by layer by layer material. So, all these layers are in
nanometre dimension, one of the dimensions are in nanometre. So, exfoliation an
extreme case of inter calcination where the complete separation of the layer of the
material happens. So, how do you do it, after you put this inside still there will be
sticking. So, I aggressively try to break the bond. So, the typical aggressive conditions
are required to remove the highly polar solvent and the aggressive reagents they react
and then this fellow gets disintegrated such that I get layer by layer by layer now each
layer is of nano material dimension.
So, what I explained you is given in clear picture here. So, these are the layers. So, it is
layered structure with gallery. So, now, in this layer it is all attached to each other just for
schematic representation we have given the spacing, now what I do is inter calcination
something flows in between and it tries to separate out a distance right. In exfoliation
what happens this distance is further enhanced and we separate out layer by layer by
layer.
So, in situ polymerization method was first reported by Toyota researches from the
synthesis of a polyamide nano composite that led to the exponential growth in the nano
composite research, for generation of polymer nano composite by this method a layered
silicates mineral is swollen in a monomer. So, what have you done? The layered silicate
is insert or its it is dissolved or it is put inside a liquid. So, this liquid will try to swell or
it will try to separate out. So, after swelling the polymerization of the monomer is
initiated. So, now, it is swelled.
So, once moved apart there is enough space for polymer whatever it is to happen as
monomers is present in and out of the of the filler interlayer the generated structure is
exfoliated or significantly inter calcinated removed a layer out and the polymerization
happens. Rate or the mechanism of polymerization in and out of the filler interlayer
maybe different therefore, it is important to control the inter gallery or the extra gallery
polymerization reaction for getting uniform reaction. So, what I am trying to say is I am
trying to say this is separated by a monomer and after this, this is added to or in this what
happens you try to have a reaction to form in situ polymerization of generating
polyamide nano composite.
(Refer Slide Time: 36:20).

If you look at the schematic diagram so you can see in situ polymerization I add a
monomer, I add grapheme, CNT or inorganic filler whatever it is which has a layered
structure. So, then it is put together in a solvent, now in a solvent what we do is you have
to somehow push the layer in between. So, if you have to push the layer in between you
have to aggressively create a space and push inside. So, this can be done by
ultrasonification, in ultrasonification process what we do is we try to vibrate, we vibrate
the solvent at 21 kilo hertz, it creates cavity small small bubbles these cavities are broken
or it is blast and then when it is blast it creates so much of pressure there.
So, it is easy for a material to go inside or it can get inside some material without any
problem. So, that is why we always go for ultrasonification, ultrasonification is always
used for homogenising the reinforcement in a viscous material we go for
ultrasonification, if the viscosity is slightly low then we also go for magnetic stirring. So,
this 2 is done only to get uniform dispersal then afterwards the mixing, the mixture that
is the swelling of the happens and then we add initiators these initiators are added for
initiating the polymerization then I have to accelerate my polymerization. So, I tried to
give heat rather than giving a heat by a laser and other things which is for a spot we
always try to give for radiations. So, this radiation can be uv can be infrared such that the
polymerization happens.
The in situ polymerization is this. So, here what we do is we are trying to work on
thermoset polymer matrix composite. So, you have a solvent, mixture is there
polymerization can happen after this polymerization surfactant s d s under continuous
stirring happens and then you form micro emulsions. So, by this way we try to form this
is micro emulsion polymerization by this way we try to form in situ polymerization,
since thermosets are liquid in nature this process is very easy, to a large extent it is easy
to get uniform homogenisation of the reinforcement in a polymer.
So, the schematic diagram I have just put here. So, inorganic filler is used and then we
add polymer to it we allow it to swell. So, it is swelled. So, this monomer goes inside.
So, polymerization happens I apply heat, heat in the form of light I apply. So, inter
calcination of the platelets happens and then this is a polymer which is formed the
monomer is converted into a polymer and that is how you get a polymer nano composite
in the in situ polymerization process, now I think it should be very clear for you.

So, I have put one more example. So, in this example you can see the in situ micro
emulsion, what is this micro emulsion? This micro emulsion what we were talking about
micro emulsion polymerization right the same thing we are trying to take in situ micro
emulsion polymerization technique for polystyrene and graphene, what is graphene?
Graphene is another form of a carbon. So, we are trying to graphene is trying to pushed
is being pushed into polystyrene. So, maybe they wanted to have a conducting property
so they do it or they would like to have a better fracture toughness property they are
doing it. So, there are several applications.
So, e g is taken so graphene is taken and then these graphene are expanded and moment
it is expanded they are expanded by applying very high temperature by this what we
have is we try to take a single layer of grapheme, now the single layer of graphene at
room temperature is dispersed in a water bath. So, what are you doing you want to add
something into the graphene layer or if you want to delete something into the graphene
layer you can get it done. So, when you want to add it is called as functionalization,
when you want to remove certain things which you do not want. So, then also we try to
do this water, water is something which is easy to handle and it is low viscous. So, it is it
can be easily mixed with graphene. So, when you want to mix with graphene we always
use a process called as ultrasonification, ultrasonification process.
So, in this process we try to add some functional agents then at room temperature the s d
s what are s d s, s d s are nothing, but surfactants you see that s d s at surfactants under
the continuous stirring. So, this surfactants are added again it is getting functionalized.
So, now, you see uniformly it is all dispersed then at 0 degree celsius what we do is we
try to add styrene droplets polystyrene what you want is polystyrene supposed styrene
droplets, styrene droplets are added then at 85 degrees Celsius you again sonicate you
see that this polystyrene particles are formed and this s d s is also added.
So, they try to mix each other properly and try to get whatever is the output. So, now,
these are polystyrenes which are there, polystyrene are made and then we try to pore it
inside a die or extrude it in a strip whatever it is we try to get the polymer nano
composite that is polystyrene grapheme impregnated polymer nano composite for
various applications, you can see the red dots are polymers polystyrene and the
functional parts also mixed. So, you get the graphene is also mixed. So, you get a host
matrix and then you get the final output.
The next interesting processes electro spinning, what is electro spinning? electro
spinning what we do is we try to generate nano fibres, how do we generate nano fibres
we try to take the liquid what you want to convert it into a fibre. So, in this syringe what
we do is we apply pressure here and slowly the liquid which is here is through this
syringe is try to flow out and simultaneously what I do is I try to create an ambience
where and which there is a very high potential. So, when the liquid comes out and when
there is a very high potential done its try to generate nano fibres, these nano fibres are
stuck on or are grown on top of a rotating mandrel or a flat mandrel. So, what is
happening is it gets uniformly rotated.
So, all around the mandrel you will have now nano fibres which are getting impregnate
or which are getting formed, which just in gets stuck physical sticking happens. So, this
is what is electro spinning process it is it is a very interesting process, now lot of things
are getting electro spin and then they get try to get the output for example, today they
make fibres. These fibres are used for water treatment they have they functionalized
these fibres with the with such a, with the such an element or with the such a
functionalizing agent it tries to attract arsenic and it completely absorbs arsenic and you
get a to a large extent you tried to remove arsenic from the drinking water.
So, for this we use this man of fibres and their fibres are dispersed in a polymer. So, it is
nothing, but a polymer matrix nano fibre reinforced nano composite is there. So, this is
having lot of roll today. So, here in the schematic standard horizontal you can have this
horizontal or you can have this vertical standard horizontal electro spinning setup is
shown a for at least a syringe pump. So, this is a syringe pump. So, through this syringe
you have a pump which gives the pressure. So, that it tries to eject out very small
quantity of a polymer solution.
So, this is at a very high voltage is applied at the electrode sources and then it is and a
collector shows a very high potential is applied and then you try to generate this nano
fibres, out of this syringe out of the syringe you will have needle tip you can see there is
a Taylor cone which is formed and this Taylor cone is will help in making nano fibres.
So, the entire process goes in making this Taylor cone and this Taylor cone confirmation
is a big challenge, moment it is formed then the fibre is a continuous process it produces
lot of things.

So, in electro spinning electro spinning can be used to prepare fine composite nano fibres
with a diameter from nanometre to micrometre range you can have the diameter and
length can be long, the preparation of the precursor mixture involves dissolving the
polymer matrix and the graphene in the solvent. So, we mix it and then put it in the
electro spin the mixture is then elerctrospun. So, what are we trying to do? We are trying
to mix polymer, we are trying to mix graphene and then we are trying to eject it out. So,
the mixture is then electro spun by applying a very high voltage of 5 to 20 kilo volt on
the syringe needle.
During the typical process the polymer solution held by its surface tension please note,
during the typical process the polymer solution held by its surface tension at the end of
the syringe needle is subjected to a very high voltage field where by a charge is induced
on the liquid surface as a result of high voltage applied and the mutual charge repulsion
induces of force directly opposing to the surface tension. So, something pulls out and
there is a resistance something pulls out and then you try to form a Taylor cone.
So, here where by a charge is induced on the liquid surface, what liquid comes out what
liquid comes out there is a there is a force which is given. So, this will try to restrict the
flow as a result of the high voltage applied and mutual liquid charge repulsion induces a
force directly opposite to the surface tension and such high voltages increases forms a
hemispherical surface at the tip of the needle which is eventually elongated and forms a
Taylor cone, there is a lot of science which goes for the formation of this Taylor cone.
So, this is very important process and here we try to mix it with a polymer and try to get
it required output.
(Refer Slide Time: 47:43) .
When a critical voltage is voltage value is reached the repulsive forces overcomes the
surface tension of the solution and the charge jet of the solution is eject out the tip of the
tip of the Taylor cone itself. The high voltage application leads to the formation of ultra
fine composite fibres with diameter micrometre range to nanometre range, while which
are electrospun as a solvent evaporates when the jet is travel through air and then a
behind a polymer fibre on the collector is done.
So, you can have a polymer fibre fit it can be beautifully done you can have a polymer
fibre on a, polymer fibre matrix and then you can spun everything and then you can all
have one more polymer layer then you can you can spin. So, what you have as you have
functionally graded materials or you can also have functionally controlled or tweak
materials. So, the voltage applied leads to the formation of ultra fine composite fibres
with a diameter in a micrometre or nanometre range and then when it is spun if there are
solvents because the solvents are generally used for flowing. So, the solvent evaporates
while it comes into the free air contact and leaves behind a polymer fibre on the
collector.
The electro spun fibre presents an interesting property has high surface volume to
volume ratio leading to low density high pore volume and outstanding mechanical
strength can be brought in when you do electro spinning process and generate a polymer
nano composite. However, the process parameters as well as the choice of the system
includes the type and the molecular weight of the polymer the polymer viscosity, solvent
used, voltage applied, needle of the collector distance and the polymer flow rate often
plays a crucial role in achieving the desired properties in the nano fibre composite
procedure.
So, this is another process which is electro deposition. So, in electro deposition,
deposition means I tried to deposit nano materials on top of polymer and try to make a
composite out of it. So, the electro deposition the schematic diagram of a different CO
OH twice architecture de corrected carbon cloth produced using a 3 electrode system
based electro deposition method with diverse voltage scanning rates can be done.
So, you have an electrolyte which is having a metal oxide precursor, you have a platinum
a platinum is a neutral one. So, you have a platinum electrode wire which is there then
we have a reference which is a silver wire a g slash a g a g silver chloride and then you
have a working electrode which is a carbon cloth right. So, then this is a carbon cloth.
So, if you try to scan it with different different voltages you try to get different different
nano particles which is getting embedded on a polymer matrix or on a cloth which can be
used for applications.

So, electro deposition is a simple and a fast approaching to prepare nano composites
using electrochemical reaction, this process involves electro polymerization of a polymer
slash a graphene composite from an aqueous precursor solution of a monomer doping
agent and a graphene oxide. So, you need to do electro polymerization and electro
polymerization, polymerization process in presence of electrical energy it is called as
electro polymerization of what of a polymer slash a polymer or a graphene mixed
polymer graphene composites. So, this 2 is mixed from a aqueous precursor solution of a
monomer doping agent and graphene oxide all these things are mixed together.
Usually the electro deposition cell has 3 electrodes one is called as a working electrode
one is called as a reference electrode one is called as the counter electrode. Counter
electrode is generally polymer and the working electrode on which the layer is to be
deposited the reference electron is a g c l whatever is there.
So, the working electrode consists of an electrically conducting material or a substance

which is nothing, but glassy carbon electrode, the electroce deposition of the polymer
occurs at a specific potential and stops when an appropriate amount of charge has passed.
So, you can also control the process as a result a nano composite film is formed on the
surface on the of the conducting material and if you stack all these things you can try to
make a thick layer of nano composites.
(Refer Slide Time: 52:45).

So, if you look into the properties mechanical property the effect obtained is tensile
enhancement and hardness finds its application in automotive industry and textile
industry. The chemical highly reactive catalysis and anti bacterial size for
functionalization, barrier properties, packing material, medical devices and smart textiles
are coming up today. Smart textiles are textiles wear and which it tries to change the
colour then filtration membrane is also coming up, physico and chemical super
hydrophobicity is thought about, self cleaning coatings are coming up today. So, if you
want to make a shirt and if there is a stain it gets cleaned of its own; that means, to say
basically does not allow the particles to enter inside then thermal flame retardant is there.
So, it is used as a protective coating insulating panels optical. So, refractive index and
transmittance fluorescence it is there. So, it is used for optical imaging lenses.

So, if you look at a car these are nowadays several parts of a car is now replaced by nano
composite, lightweight graphene based materials are used for structural applications in
the engine. Graphene nano fibres are used for integrated sensors than functional textiles
are used for detecting the sensors for pollution detection and safety is also there, smart
adhesions are coming up today. So, where and which it can expand and contract
depending upon the temperature and then you have nano fluids which are coming up for
maintaining the thermal temperature friction and thermal management which is done by
nano fluids and nanostructure thermal emmitive materials which are used for thermal
energy materials which are used for cooling and heat recovery are being considered. So,
that these are some of the applications where polymer nano composites are exhaustively
used in automobile.

So, some more examples power train, timer belts, engine cover, inverter cover, coatings,
headlamps, tires and then interiors all these things are made out of nano composites and
they are finding it applications.
So, polymer nano composites are finding out for environmental remedial measures,
energy storage, electromagnetic shielding sensing and activation transportation and
safety defence systems information and electronic industry are using it o LED a LCD are
using polymer nano composite and novel catalysis are done for nano pigments are also
coming up, these are the areas where polymer matrix nano composites are used in a very
big way.
In conclusion many high highly hyped technology products polymer nano composites are
coming up into the market, polymer nano composites exhibits superior property in
mechanical thermal barrier optical etcetera moving to the polymer nano composites how
a presence omnipresence in various fields of applications seen. Polymer nano composites
finds various applications could be synthesized by proper selection of matrix, nano
reinforcement synthetic method and the process surface modification is also very
important many products based on term polymer nano composites have been
commercialized today therefore, we can conclude that various types of nano composites
and their surface modification procedure some unique properties of nano composite and
its offer for various technology applications can be achieved.
Thank you very much.

Prof. J. Ramkumar
Lecture - 20
Ceramic Matrix Composites
Welcome to lecture number 20. In this lecture we will try to cover about ceramic matrix
composites. Ceramic is one material, which has been used for centuries together. In fact,
the earthen part is a very simple example for ceramic materials being used in the history.
So, ceramic materials has its own advantage, and in the past itself; for example, in the
previous century, self-people started using ceramics as a matrix, and then reinforced with
some soft materials, and then they have. Now recently we have move to hard materials
also. So, in this lecture, we will primary focus on introduction to ceramic matrix
composites, what are different types of ceramic matrix composite, property of ceramic
matrix composite, interfaces. Then we will go through some of the fabrication
techniques, and finally, application of ceramic matrix composite

So, a recap till now whatever we have done, we have we have studied of manufacturing
of composites. In manufacturing of composites, we had three matrices; one is polymer
matrix composite, metal matrix composite and ceramic matrix composite. In polymer
matrix composite we have seen thermoplast, thermoset, and to some extent we also have
seen elastomers. Metal matrix composite, we have seen aluminium based, and then to
some extent magnesium based composite materials right. So, now, we will focus on
ceramic matrix composite.
So, before getting into, little bit of fundamental what is the typical difference between a
metal and the ceramic material metal are crystal structure ceramics are also of crystal
structures in metals. You have large number of free electrons. So, that is why it is
predominantly conducting material. Here it is captive. Electrons are there in metals we
have metallic bond here. It is ionic or covalent bond; that means, to say it is very strong.
So, since it is metallic and it has free electrons, it is good conductor. Here ceramics are
poor conductors. Majority of the metals are crystalline or polycrystalline in structure. So,
they are opaque, and here you have amorphous material also in ceramic. So, that is why
it is transparent and of course, you have crystalline, semi crystalline and amorphous
ceramics all three, but if it amorphous is also one. So, amorphous we have transparent a
simple example is your glass, then it has uniform atoms here, different size of atoms are
there; that means, to say for semi crystalline materials can also be possible. So, it has a
very high ductile strength here. It has very poor ductile strength; since its alcohol and
bonded the bond is very strong. So, it is tensile strength, very high tensile strength, here
it is very poor tensile strength.
So, here since they have free electrons, and this free electrons and metallic bond they
give you some amount of ductility, here there is no ductility. So, that is why it has very
poor tensile strength, it has very low shear strength, it has very high shear strength, it is
good in ductility, it is poor, it can plastically flow here that property itself is not there. It
is very good in impact strength, it has very poor in impact strength. So, that is why it is
brittle, it is relatively, it has a high heavy weight or high weight, or it has a higher
density. Here it is low weight or low density, hardness is moderate, hardness is extremely
high. So, predominantly if you look at ceramics extreme high hardness, poor ductility,
poor tensile strength. So, it is non-porous. Here you can also have porosity in ceramics. It
has very high density, it has very low density.
So, now, with this you can try to identify very clearly what is the difference between
metals and ceramics, when to go for metal matrix, when to go for ceramic matrix, where
ever you have very high temperature application, we always prefer to have ceramics.
Where ever you would like to have very light, and where there is not much of impact
load, we always go for ceramic matrix composite, ceramic matrix and ceramic matrix
composites are made, if you look at ceramics.

Ceramics are divided into two; one is called as traditional ceramics, the other one is
called as advanced ceramics. So, traditional ceramics you have white wares, and then
you have structural clay products, bricks and tiles abrasives, which is used in grinding,
which is used in water jet cutting, which is used for lapping, polishing, all those things
you have refractories and you have cement. These are the traditional ceramic materials,
which we know and lot of products have been used, and when you go for advanced
ceramics you have electronic ceramic, and you have advanced structural ceramic.
Predominantly our focus will be on structural ceramics. So, in structural ceramics you
have nuclear ceramics, bio ceramic, tribological ceramics and automotive ceramics.
So, bio ceramics, which is used as bio implants into the body, when you look at electro
ceramics, we will have electronic substrate for package ceramics; we will have capacitor
dielectric of piezo electric ceramic, magnetic ceramics, optical ceramics and conductive
ceramics. So, all these things are electro ceramics. This is a new area, which is there
from the last 50 60 years and today we are finding lot of applications in this areas. For
example, magnetic ceramics which is not thought of, is now there, and we also have
capacitor dielectric ceramics, which is for very small applications. We also have Piezo
crystal ceramics, where and with very small displacement are to be measured, are to be
given. We go for piezo crystal ceramics. So, when you talk about matrices.

So, since ceramic is, the form of existence of ceramic, is always in powder form. So, the
reinforcement whatever we mix, has to also be somewhere close to powder form. So, we
always used particulate. So, we always use particulate whisker, we use nano, nano
powder or nano whatever. So, these are the three reinforcement, which are predominantly
used. The form can be particulate, where in which we talk about aspect ratio, then
whisker then you can also have nano.
So, these are some of the reinforcements which are added to the matrix ceramics, to get a
ceramic matrix composite. So, matrix can be of two types; it can be oxide and it can be
non oxide. When I talk about oxide, it is TiO 2, Al2O3, SiO2. All these things can be there.
When I talk about non oxides it can be SiC SiN TiC TiN TiCN, these are some of the non
oxide ceramics which are there. So, you can choose, depending upon your requirements,
choose any one of these ceramics as a matrix.

And then this matrix is blended or mixed with this reinforcement, and finally, you get the
output ceramic matrix composite. So, we can see that. So, these are the matrices you
have SiC Si3N4 silicon nitride molybdenum silicid boron carbide boron nitride
aluminium nitride TiB2 TiN TiCN and alumina, which is very commonly used. So, if you
see the particulates we can see, TiC can be there, SiC can be there, TiN can be there, TiB
2 can be there, you can have zirconium oxide, you can have niobium and you can have
silicon nitride B4C we have seen. So, I can be in platelet form it can be in whisker form,
and today we have also started using fiber form. So, fiber is, you will have fiber which is
made out of metal, and this metal will be coated with ceramic material. So, this a coating
which is done on top of ceramic. So, now, the fiber is called as ceramic fiber.
So, predominantly this is done by CVD process. This is done by, see chemical vapor
deposition process, what we give; say for example, you can have a tungsten wire, and
then which is coated with boron. You can have a carbon fiber also. So, you can also have
alumina fiber, where in which it is coated, ductile wire, tungsten or something which is
coated, because tungsten is very high temperature. So, when alumina is coated, it can
withstand very high temperature applications.

So, ceramics are sub group of composites, as well as sub group of technical ceramics. By
definition ceramic matrix composites are materials, in which one or more district ceramic
phase are intentionally added in order to enhance some properties; that is not possessed
in the monolithic ceramic. So, the biggest thing what we are looking forward is, we
would like to enhance the toughness property.
So, the toughness property can be enhanced by adding particulates. What happened when
you have particulate? When you have a ceramics, and when you add particulates in it,
and when a crack grows, the crack is getting diverted or distributed, or the crack energy
is reduced, and it goes around the ceramics and then it goes. When it goes around the
ceramics, the energy is dissipated and, because of this dissipation the crack does not go
further. So, the toughness property increase. So, this is the particulate or particle
whatever it is.
So, what I have done. I have intentionally added this, particulates; such that I can
enhance the toughness property; that is what we are talking here. In ceramic matrix
composite, a given ceramic matrix is reinforced either with discontinuous reinforcement,
or it can be with a continuous reinforcement. Predominantly what we look forward is,
discontinues. So, it can be in particulate form, whisker form, or it can be chopped fiber,
the continuous fiber is also possible. So, the basic reinforcement which are included in a
ceramic matrix are; carbon, glass, glass ceramics, oxide and non oxide ceramics are
added to the basic ceramic matrix.
So, if you look at the A CM figure of a ceramic matrix composite, you can very well see,
this is a matrix, and you can see this is the alumina fiber which is reinforced, and this is
what I was trying to say, if at all there is a crack here. This crack grow goes around and
the energy is dissipated. So, you can see this is 5 microns. So, this reinforcement, maybe
somewhere around about 10 to 15 microns. This is an alumina fiber, this is one cross
section. So, you can see how it is done. So, reinforced by 2 D woven fabric, they have
done it with using it 2 D woven fabric.

So, the fracture toughness of the ceramic is improved, by introducing a secondary phase
which we were discussing. So, I was saying that the secondary phase are chosen, to act
as a barrier for crack propagation. So, is it clear whatever we have seen here in the
previous CM, we have just put it inwards predominately in ceramic matrix composite,
we would try to enhance the toughness property; that is one property, but if you want to
make it conducting ceramics. So, we try to add ingredients; such that it makes the
ceramic conducting.
So, there we choose conducting particulates to be added, and then people are started
using it today people have started using CMT in a big way, so that they would like get
advantages over the toughness property. The whisker, whisker and particulate the
different is aspect ratio, is introduce into the ceramic matrix for retard the crack
propagation, because the stresses in the whisker, spanning the crack plane, will tend to
pull the crack shut.
This phenomena called as crack bridging, crack bridging is one very important
phenomena, very important phenomena. What is this phenomena. Here the crack
propagation can. So, what happens whisker, when it is introduced into the ceramic
matrix, it can retard the ceramic propagation, because the stresses in the whiskers
spanning, the crack plane will tend to pull the crack shut, and this is called as crack
bridging, which leads to very high fracture toughness. When we are using continuous
fiber composite, it exhibits quasi ductile fracture behavior, which resulting in extensive
fiber bridging, but please understand, using or reinforcing a ceramic fiber into the matrix,
is really a challenge while manufacturing.
It is very easy to manufacture particulate type or whisker type ceramic matrix composite.
Simple example is your cutting tool, where in which use tungsten carbide and cobalt.
Then you can try to say, you can try to say add tungsten carbide, today we had cobalt and
we also call add zirconium oxide. This is also a cutting tool which people have started
using right, and then you can also use alumina, which is reinforced with S i C, which is
in the whisker form. All these things are done only to enhance the fracture toughness
behavior.

So, there are two categories of ceramic matrix composite; one is a group of toughened
ceramic reinforced with the particulate. The second one is a continuous fiber composite
which exhibits quasi ductile fracture behavior, accompanied by a expensive fiber pull
out. So, basically what happens is, when the crack tries to grow, around the particulate
either this particulate tries to distribute and do something, or the fiber or the particulate
pulls out of the existing location. So, that all the energy gets dissipated in pulling it out.
So, that crack does not go further.
So, the fracture toughness of this class of material, can be higher than 20 mega Pascal
route meter, when produced with a weaken interface between the fiber and the matrix.
For example, what are we trying say, let us go back to the cm which we are discussing.
So, one way we are doing it to the crack which is growing here, one way is you distribute
the crack energy. The other way is the crack is growing, you try to pull this particulate
out or you try to pull this fiber out, when you try to pull the fiber out, the energy gets into
pulling it out, because you have a very weak interface, weak interface means, it quickly
goes around and tries to remove the particle very easily, and the energy is dissipated in to
the fiber, in that location where we pull out has happened.

So, different types of ceramics alumina, zirconium oxide ceramics are there, SiC
particulate reinforced in s silicon nitride. Again cutting usage, then alumina and SiC then
we have a, this is whisker, first one was particulate, this was whisker, then you have
continuous fiber, then carbon carbon composite is there SiC SiC. These are all very high
temperature application high temperature, which is used in missile rocket all those
things, oxide oxide composites are also there available. So, for example, alumina
reinforced with an alumina particulate, or alumina reinforced with zirconium oxide. So,
alumina reinforced to SiO2.

So, this are some of the examples. So, what are the different types of composites,
ceramics matrix composite. It can be short fiber, it can be long fiber, it can be layer, it
can be particulate, it can be functionally graded ceramics. Look at the functionally
graded ceramics, the reinforcement if you see layer by layer by layer, there is the volume
fraction keeps changing layer by layer by layer. So, what happened, on the periphery you
have a large amount of particulates, as and when it goes down you it is less what,
because of this, what happens the tribological properties and fracture toughness property
enhances. This is functionally graded material today; there is a huge demand for
functionally graded materials.
Then you can have polycrystalline with different fracture properties of grain boundaries
you can have. Then particulate with small interface you, these are interface and then
particulate with very thick interface. So, these are the different types of classification of
ceramic matrix composite. I repeat it and can be shot fiber or if you want you can go one
step ahead ok.
Shot fiber, then you can have long fiber, then you can have layer. Layered are basically at
something like a tip type, you try to cut it down, or you try to make a preform or
something like that, so you get that. Today you get, you have ceramic steps which are
available. So, you put those steps as and when you want to reinforce, then you have
particulates right. The difference between this and this is aspect ratio.
So, here particulates can be whiskers it can be particulates. The distribution of

particulates between layer to layer to layer there is a variation, which leads to
functionally graded materials. So, functionally graded materials, if you see, the function
you try to reinforce the function, grades along the material. So, if you see after you
remove the first three layers then the tribological property will be less, then you have a
polycrystalline with a different fracture properties of grain boundaries, these are grain
boundaries.
Then you will have with weak interface with strong interface. So; that means, to say this
interface the crack can grow break it will yield out and then you get the required output.
So, what are the properties of a ceramic matrix composite? Generally when you make a
product, first thing what you have to look you have to right down the objectives, or you
have write down on the specification, what is the specification this product has to
execute when put on service condition.
So; that means, to say we will always tried the list down all the properties, what you
want from this material, plus you will also try to put a quantifying value for each of the
specification whatever you say. So, with this what did you get, you get the properties
moment you have these properties then you start working on which matrix to choose,
which interface to choose, what is a processing route and how do I meet out to the
requirements. So, if you want to make a ceramic matrix composite. So, first thing is, you
have to understand what are the properties of ceramic matrix composite.
So, ceramic matrix composite the property which is common for all, composites is, it has
very high strength to weight ratio. Ceramics of its own has very good wear resistance.
So, ceramic matrix composite matrix will have wear resistance properties, ceramic
matrix will have corrosion resistance.
Now, since it is ceramic matrix composite, it fatigue strength is enhanced. Suppose for
ceramics you want to enhance the fatigue strength. So, then basically what we do is, we
convert it into ceramic composites. Then we have low electrical conductivity, you can
add particulates to change this property, it has an anisotropic property, it is low cost, it is
easy for processing, the matrix is harder and brittle. The reinforcement must have high
tensile strength to arrest the crack growth. This is very important. The reinforcement
must have high tensile strength, then the reinforcement must be free to pull out as the
track extends. So, basically what you doing energy which is getting dissipated into the
product. So, the energy when it propagates, it should spend enough of energy.
So, that it pulls out the fiber, or it pulls out the particulates. So, once its pull out the
energy it dissipated that point crack does not grow; the material retains for a longer time.
So, the fatigue life enhances the toughness value goes high. This is a typically, I have just
put different ceramic matrix composite, and I have put the ceramic matrix.
What is there properties, when you talk about porosity density, you see alumina 3.8,
when you make alumina alumina, it goes to 2.1, you have tensile properties, you have
elongation, you have young’s modulus, and then you have flexural strength. Young’s
modulus means, higher young’s modulus means it is becoming harder it is brittle; like
there is no, there is no elongation at all. So, you can do with carbon reinforced with SiC
then C with SiC, these are different process which we will see later.

So, the other properties which people are now trying to enhance on a ceramics matrix is,
they wanted to enhance the thermal conductivity, they want to enhance the linear
expansion and the electrical resistance. So, these are the values by of different processes.
So, the property of ceramic matrix composite, if you see in the, it is exhaustively used in
aerospace industry, and turbine engine. If you in aerospace engineer, the temperature
what we talked about is about 1500 degree Celsius. Here it is about 1000 degree Celsius,
and in turbo engine components are heat exchanges, it is expected to work for 10000
hours, and when you have a sliding and sleeve or in a pump components, it is expected
the temperature will up to 500 degree Celsius. The temperatures are the working hours is
going to be from 1000 to 10000 hours. So, here what we are looking at it, we are looking
at properties which can enhance the temperature, which can be withstand for a longer
temperature, which is light in weight. The fracture toughness is high, and the tribological
properties, tribological ok.
So, long life time under extreme temperatures; that is oxidation and wear, we also a
taking about oxidation resistance, and corrosion, oxidation and corrosion resistance are
some of the properties, which we always expect from ceramic matrix composites.
I already discuss this interface interphase, I will re, I tread the same thing, interface is
very important, because if you want to enhance the crack propagation. So, basically what
you have to do is, you have to enhance the interface property. So, it is the boundary
demarketing, the distinct phase of the reinforcement and the matrix. This is a zone across
which the matrix and the reinforcement phase interact. The interaction can be chemical,
it can be physical, it can be through mechanical. Mechanical means, it can be through
locking, mechanical locking right. For the composite to operate effectively, the phase
must bond, where they join at the interface. In some cases the third ingredient must be
added to achieve bonding of primary and secondary phase called an interphase. Is it
clear? This third ingredient can be through an additive or a coating.
So, basically it is same reaction happens between these two, between the matrix and the
ceramic, which is reinforced. So, now, what happens is, there is a reaction happening and
it can format interphase. So, this interphase is between matrix and the ceramic, and this
interface is between these two, we try to functional.
So, that you get a proper this thing. So, this we have already discussed I just wanted to
put it for the reiteration. So, interface, what is interface. Right. Is it clear now?

We studied in metal matrix composite also. I have just wanted to reiterate the same thing.
So, interfaces, little bit when you look mechanical strength and other things. So, here we
see a brittle fracture, here we see a non-brittle fracture. So, these are the mechanism of
the crack deflection, which happens in a ceramic matrix composite. You can see here, if
it is a brittle fracture. So, the crack just keeps propagating in this direction, fiber break
this. These are the fiber, these are ceramic it breaks. So, no interface of the fiber, on the
fiber surfaces are there. So, it is just breaks like this right. The next one is, if it is a non
brittle fracture, there is debonding at the interphase of the fiber and surface.
So, what happens is crack gets distributed. So, this interphase tries to distribute the crack.
So, it is going to withstand higher amount of toughness. So, here additional interphase
layer for example, a film of sic of thickness 0.5 to 5 micron provides protection of the
fiber, from either the environmental attack, or the aggrieve action of the of the infiltrator
material. So, this is very important. So, this happens, this is the importance of interphase
between a fiber and the ceramic matrix. The mechanism of failure can be brittle, or it can
be non-brittle. So, the debonding at the interface happened here, it just crack propagates
and then it breaks all the fiber and do, because it has no interface.

So, the interface can in influencing the composite strength, modes of failure, young’s
modulus, inter laminar shear stress, compressive strength, environmental resistance,
sustainable at higher temperature, and fracture and fatigue behavior. These are all
important properties for interface, very important, important for interface in ceramic
matrix composites.
So, the cracks at interface, you can see here. This is alumina, this zirconium oxide. So,
this is the diameter of the, there are saying 2.5 microns, and this is the small
reinforcement which is there.
So, we can have, these are at the interface, this are the crack, and then you can see, a unit
cell a with a meso cell level you have and we can make this. So, you look at it.
So, these are nothing, but wing cracks at micron level between the interface.
So, these are mesocrack, these are wing crack, micro level crack which happens and the
crack keeps growing. So, you see beautifully that crack keeps going from here to the next
crack. And the other thing is the micro level crack, between the grains it can have, and
the last one is the second king initiative of the wink crack.
So, you can see here. So, here it again it bifurcates, and it starts growing, and this, this
are the loads when they are applied, tensile load which is applied. So, you can see what
happens to the crack and how does it grow. So, in all the three cases you see the
important thing is, tensile is loaded, it is loaded tensile, and because of that the crack
keeps growing. So, this is wing level, micro level crack, this is mesocrack, then this is
secondary kink initiative for wing cracks.
So, the most important property between the ceramic, which is used as a particulate, and
the ceramic which is used as a matrix, between these two fellows, to have a very good
attachment or something, we need to look at their wettability property.

Wettability property becomes very important. So, wettability property, the liquid which
spreads over the solid is wettability, good wettability means, that liquid matrix will flow
over the reinforcement. Here it is already ceramic, so you cannot take it to the liquid
face. So, you have to say how do you make this wettability property very good. The
wetting will also occur, if the viscosity of the matrix is too high, the interfacial bound
exits due to adhesion between the reinforcement at the matrix, which means to say, the
wetting is good between the reinforcement and the ceramic matrix.
So, we have already seen it in the metal matrix. So, the same figure we have repeating
here for ceramic matrix also. You have a vapour state, you have a liquid state, you have a
solid state. This is a line which talks about the interface between the solid liquid,
between an interface which talks about liquid vapour, and this is an angle which is made.
So, and this angle is called as the contact angle. We are more interested to find out the
contact angle, and here I have forgotten to say this is a interface between the vapour
phase and the solid face. So, if there if this theta is 180 degrees, then it as no wetting
angle if it is 0, it is perfect wetting angle, so this goes 0. So, it goes down, it is perfectly
wetting and if it is anything between 0 and 180, 0 and 180. The wetting, the degree of the
wetting angle increases or as theta decreases.
So, when you go lower and lower and lower, wetting is good. When you go higher and
higher and higher, it is not good, or it is it is having a poor wettability property. So, this
can be found out by the formula cost theta equal to gamma SG minus gamma SL by
gamma LG. So, SG is solid and the gas, solid and liquid, liquid and gas. So, if you want
to look at it, solid and liquid. So, this is solid and gas, solid and vapour and. So, we can
make it as G, and this we can make it as, this we are making it as SL, this is (Refer
Time:32:40) and this is SG, vapor is SG right.
So, this is what is the formula, we try to find out the cos theta. This is wetting and the
poor wettability lotus leaf effect. So, majority we have the insects, insects leaf and all,
they have a nano fiber; nano fiber, or they call it as nano texturing, nano slash micro
texture. On the surface of the leaf we have this nano or micro textures. So, this makes it
have poor wettability property.
So, that the water droplet rolls out of the thing, of the leaf and falls down. The same is
with respective of lot of animals on their skin. For example, sharp which is always in
water never as a skin disease, why, because of the micro nano texting. So, here it is all
more focus towards wettability.
Globally, ceramic matrix composite in the last couple of years. What is happened is,
slowly it has been started getting increased in different areas, where mechanical and
chemical applications. So, it is there, it is used for example, it is used in heat exchangers,
it is used in extraction unit, oil refineries. Now when they are looking forward for
chemical aerospace and defense, if they wanted to make it lightweight material, they are
looking for energy and environment, they are also looking for ceramic matrix composite
and others are there, you can see slowly the manifold from 2005 to from 250 million
dollars, it has gone too far, close to 450 million dollars.
So, this from 100 million dollars, it has gone down to 220 million dollar. So, the other
industries are also there is lot amount of the usage of ceramic matrix composites.

So, what is the next generation of ceramic matrix composite? So, the next generation of
ceramic matrix composite are going to be. So, these are TBC, this is thermal barrier
coating. Thermal barrier coating can be used for aerospace cutting tool, so many
applications. First it was uncooled, now it is film cooled, then with thermal barrier
coating, then with EBG. We are also now getting materials which are silicon based,
ceramic matrix composites are there. We are, then this will go into eutectic oxide based
ceramic matrix composite, with heat pipe cooling we will try to make. So, you can see
these are the ceramic materials which can go up to 3000 to 3500 degrees. It can go up to
3500 degrees Fahrenheit.
So, this is what we are looking at it. We are looking at high temperatures, and very high
temperature we are looking at. And now we are also looking at very good mechanical
properties such that it can be used for that. So, this is electronic barrier coating, thermal
barrier coating. So, electronic barrier coating silicon based. So, here we are looking at,
these are the first generation, these are the second generation, and now it goes. We will
move towards the application of ceramic matrix composite. It is today exhaustively used
in automobile brake learning, what happens.

Now, a days we talk about very high speed. So, the very high speeds, if you apply brake,
there will be lot of heat which is getting generated. So, there will thermal expansion, and
softening of the material which we do not want to happen. So, we are nowadays going
for C SIC rotors, and we also have cooling channel. These are the bells which are used,
and these are tungsten pads which are used. So, when these to come in contact, we will
try to get very high temperatures, and there will be very high frictions; that is reduced
when we start using ceramic matrix composites.
So, carbon with SIC. So, high braking performance, the weight goes down, the wear
resistance goes down, the temperature of which it is operating goes very high up to 1400
degree Celsius, and nothing happens. The first study has started in 1990, and it is
available from 2000, it has been introduced in Mercedes and Porsche cars it has been
introduced. There are 50000 to 70000 ceramic matrix composite brake disc, which are
manufactured in 2006 by these two companies.

So, if you look at it, these are ceramic matrix composite rotor on a BST carbon fiber
wheels. So, carbon fiber wheel is very light weight. So, paired with Brembo Monobloc
Capillary, custom anodized spacer and bottom of this superhike bike forks, you can see
this. So, these are the forks, and these, and this is completely now made of ceramic
matrix composite. This is what the monobloc caliper, which is monobloc caliper which is
used. So, this is best for are breaking. This is the carbon ceramic composite disc brakes
which are used. So, this are the disc brakes, which are used in automobile today.
So, the Porsche ceramic composite clutches are made out of it, which is called as PCCC
Porsche ceramic composite clutches, designed, designed and these siliconized carbon
fiber is used here. The diameter is a round about 170 millimeter, weight is round about
3.5 kgs already it is made out of cast iron, which was like 7 10 kgs, now it has come to
3.5 one tenth of the mass moment of inertia comes, because of this ceramic matrix
composite, which is a huge reduction in energy consumption and all those things, lower
transmission and engine mounting, lower center gravity, and it is very high since the
technology is not become popular, and intellectual property technology. So, still it is
expensive. So, you can see that, in transmission systems also, the ceramic clutches, here
are ceramic clutches which are there, and this as engine, and you have transmission. So,
now, in transmission and in ceramic clutches, there are using ceramic matrix composites.
So, in the nozzle; the aerospace nozzles, which we use F 16 fighter planes right. So, the
engine exhaust nozzles with five A 500 ceramic matrix composites divergent seals,
which are. These are the divergent seals which are, you made out of ceramic matrix
composites.
So, they are, and ceramic matrix composite are an excellent replacement for nickel based
super alloys. Already these nickel base super alloys are very light in weight, fab
manufacturing is big challenge of this, but where a ceramic matrix composite, the
manufacturing to large extent is, as compare to this, it is very easy. So, currently used as
exhaust nozzle parts and primarily due to the high capacity of withstanding very high
temperature, and severe environmental conditions; very high temperature, severe it can
be tribological it can be low and high temperature. So, for example, all these fighter
plane go at minus 35 degree c. It can go up to, maybe somewhere and about 900 degrees
c, or it can be also up to 1500 degree c. So, this is the ambient temperature, when it goes
at very high altitude, this is the working temperature, when it is burning. So, that has to
be minimum structural changes, there as to be minimum distortion which is happening,
and it has to retain its shape. So, an oxide ceramic matrix composite exhaust ground
demonstrates which is round about 1.6 meter diameter nozzles. This is 1.6 meter
diameter nozzles, and it is one, which is also a, which is the conical shape. Fabrication is
the big challenge. Now it is made out of ceramic matrix composite, with a titanium cap
on top of it.
So, a complete turbine is made out of ceramic matrix composite, or the parts, which are,
there are made out of ceramic matrix composite. So, invasion. So, what they are trying to
do is, first there are trying to attack at lower pressure compressor side, then there are
looking at higher point pressure composite side. So, here they would make ceramic
matrix composite, either as insert or as a whole body, whole part body right. So, do not
think completely the turbine would be made.
So, the either it they can make small inserts. For example, they can make a small insert
here of very high temperature withstanding, and then they can also make the whole body
is, what I am trying to say is a small portion where and which it gets attached to a
another big portion of the entire system. So, combustor is there. So, here you will have
high pressure turbine, and you will have a low pressure turbine. So, high pressure, here it
is a compressor. So, high pressure compressor and high pressure turbine low pressure
turbine. Today they are made of ceramic matrix composite material, because they have
this CMC has toughness very high, and making small inserts is very easy as compared to
make a complete body.
So, there is lot of aero engine which is made out of composite. Now CMC is getting
(Refer Rime: 42:32) in all these things. So, that it can be made lighter and lighter. So,
SIC nuclear application is other thing. Today we talk about SiC silicon carbide silicon
carbide reinforced composites, which are used for advanced structural materials in fusion
and fission energy systems, where in which the heat resistance and integrated safety is
also there. So, this is now thought of SiC in nuclear application is the next place where
ceramic matrix composites are talk top in a very big way. So, when you talk about fusion
the temperatures are very high. So, the blanket structure, the blanket channels liners are
made out of ceramic matrix composites.
So, jet engines, turbine blade which we are already discussed. See if you look at it these
are some inserts, this is a path, here is a joining adaptor and this is a slot. So, they are
now made out of ceramics then you can also see hot fluid channels are there. So, these
are all made out of ceramics or this all. So, that it can withstand very high temperature
and corrosion resistance.
What are the advantage of ceramic matrix composite excellent where, excellent
corrosion resistance strengths to weight ratio, elevated temperature retraining the
structural properties, chemically stable, catastrophic failures, because of the
reinforcement the cracks can go high hardness and light in weight, are some of the major
advantages of ceramic matrix composites.

So, the advantage, the processing route of ceramic matrix composite involves very high
temperature, and can be deployed only with high temperature reinforcements. So,
whenever you need a very high temperature application, there we will use this. The
ceramic matrix composites improved toughness. The high processing of temperature
results in the complexity and manufacturing, in manufacturing and hence the process
becomes costly. Then the difference and coefficient of thermal expansion between the
matrix and reinforcement of thermal stresses on cooling for the processing temperature is
very high.
So, the disadvantages of what is processing difficulty and other things, the biggest
disadvantages, it since it is, it has to be process at very high temperature. We have to
have furnaces which can withstand very high temperature, and the reinforcement also
should be of very high temperature withstanding. So, that is one of the disadvantages of
ceramic matrix composite to it is used to enhance the toughness property.
So, because of the toughness property, you also have to see the match in the grain size,
the match in their properties between these two. So, the next things is, since it is higher
processing temperatures are there, all these, there are lot of complexity and the process is
pretty expensive. The difference in the coefficient of thermal expansion between the
matrix and reinforcement leads to thermal stress on cooling, while the processes made.
This has to be taken care, while choosing the ceramic and the reinforcement for making
ceramic matrix composite. So, this is expensive, this is challenging, and this is also.
These three properties are very. These three are the biggest disadvantages of ceramic
matrix composite.
For this lecture assignment what I would request you is, I would request you to pick
some ceramics, ceramic parts or products right, and try to replace or add some particulate
to the ceramic product, and see its performance. For example, take clay, clay is a ceramic
material, ordinary clay try to add abrasive to it. Try to add abrasive, abrasive means sand
ordinary sand, which is nothing, but SiO2 try to add to it.
Now, you try to try to make a something like a cup, cup or pot or a part whatever you
want, a very simple trivial part. So, what you do is, first take clay, and then what you do
is you try to fire the clay. The firing of the clay can be done on a microwave oven, or if
you have, if you have a furnace you can put it in a furnace, maintain at slightly higher
temperature.
So, around about 800, we are not looking for a very sound quality, but just for your
understanding and experimentation sake. So, 800 degree Celsius, if you have a furnace
you can put, or you can just put it in a microwave oven, and keep it for some time,
maybe 2 minutes or 3 minutes, and see before it forms any cracks, you have to pull it out
of the microwave. So, you can put in a microwave, and then try to make one again. So,
cup slash pot slash part whatever it is. Next you take clay, mix with some volume
fraction of SiO2, and then first see what happens in the formability while making a shape
what happens, and then when you try to put it inside microwave what happens. Just
qualitatively make a comparison and then just for your (refer time: 48:38) study
comparison, comparison and study for yourself. So, you will make up a clay.
So, the steps involved if you want, I can. You take clay give a shape to it, and then put it
inside microwave oven, and make sure it does not crack, and allow it to dry. The next
thing is, a clay mixed with abrasive. Again you will try to shape, put in microwave and
then allow it to dry right, and then you will try to compare.
So, here sic is a reinforcement agent. Compare what, compare strength, compare
formability, compare the crack if it is growing, and finally, you can also compare it with
respect to sound. So, just heat it with another surface, and then try to note down the
sound, how shrieking it is coming and other things. So, this is an assignment which will
try to give you an understanding of ceramic matrix, and ceramic matrix reinforced
ceramics. So, that you compare the processing difficulty and the other properties with
respect to these two.
Thank you.

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Manufacturing of Composites

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These will be the content.

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If you look at it this is a composite carbon-carbon composite, this is a carbon matrix.

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So, the pitch impregnated preform is subjected to 2 pyrolysis carbonisation; in an inert

So, the densification process is carried out at atmospheres at atmospheric or at reduced

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Look at carbon-carbon composite, it can go up to 1500 degree Celsius service condition

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Thank you much.

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