CHAPTER-I INTRODUCTION Heat resistant composites are essential for the successful launch and operation of all space

vehicles. The selection of a composite material depends upon the mission of the space craft. While often the temperature capability is a major concern, the goal remains to protect the internal components at a minimal weight. This means extra insulation if the exterior material has a high heat capacity. In order to meet the mission objectives and the criteria the heat resistant material essential properties are it should have high heat of ablation, specific heat and low thermal conductivity, expansion coefficient, erosion rate. Fiber reinforced polymer matrix composite materials has

constituted a major breakthrough in the construction of lightweight structures. In particular significant benefits have been realized in the aerospace sector to meet the severe performance requirements with stringent demands of reliability. Almost all aerospace structural components airframes of fighter aircraft, helicopters, control surface and fins of civil aircraft, various planes in satellites, antennas, rocket motor casings and some complete airframes of small aircraft are witnessing an increasing use of the advanced composites. An important technological development that has contributed significantly to this growth of composites is the development of strong and stiff fibers such as Glass, Carbon and Aramid along with concurrent developments in the polymer chemistry resulting in a various polymeric materials to serve as matrix materials. In particular the versatility of the technology of the carbon fibers having various properties has played a key role in this growth. With complimentary developments in computer hardware and software technology, and in computational methods of analysis rendering help to the analyze and understand the material behavior and to provide
1

predictive as well as design tools, the complexity of the polymer matrix composites has been overcome to facilitate the extensive applications. Composites have the applications in many fields some of them are given in the following, since we are interested in aerospace applications it illustrated briefly. The creation of reliable heat resistant laminate composites for space applications requires precision design and proper tests. Because composite materials are necessary to meet heat resistant requirements for the aerospace applications such as nose cones, flame deflectors, airframes etc., some of aerospace applications where different types of materials are being used are shown below. AEROSPACE APPLICATIONS: Use of composites in LCA Tejas:

Fig 1.1 Composites in Light Combat Aeroplane (Tejas)

2

 Use of composites in LCH

Fig 1.2 Light Combat Helicopter

Helicopter Blade

Fig 1.3 Helicopter Blade

3

CHAPTER-II COMPOSITE MATERIALS A composite material can be defined as a macroscopic combination of two or more distinct materials, having a recognizable interface between them. However, because composites are usually used for their structural properties, the definition can be restricted to include only those materials that contain reinforcement (such as fibres or particles) supported by a binder (matrix) material. Composite materials generally consist of a bulk material, called matrix, and a filler of some type, viz., fibres, whiskers, or particles. Composite materials are usually divided into three broad groups identified by the matrix material: viz., polymer matrix composite (PMC), metal matrix composite (MMC) and ceramic matrix composite (CMC). These composite can have fibres, whiskers, or particulates in a matrix forming a single thin lamina, or a laminated composite consisting of layers of various laminae. The fibres, whiskers, or particulates are usually the material that carries the major stresses and loads, while the matrix holds them together to facilitate the transfer of stresses to the fibres/whiskers/particulates. It can be defined as a heterogeneous solid structural material consisting of two or more distinct components that are mechanically or metallurgically bonded together such as wire or filament of high melting substance embedded in a metal or non metal matrix.

2.1 CLASSIFICATION OF COMPOSITES: Composite materials are classified based on the matrix materials as well as the reinforcements as follows. A) Based on the Matrix material B) Based on the Reinforcement

Fig 2.1 Classification Of Composites Fibre - a filament with L/D very high (of the order 1000) A composite with fibre-reinforcement is called Fibrous Composite Particle non fibrous with no long dimension A composite with particles as reinforcement is called Particulate Composite Whiskers nearly perfect single crystal fibre Short, discontinuous, polygonal cross-section

Fig 2.2 Types Of Fibres

2.2 FIBRE AS REINFORCEMENT: a). As the diameter decreases the inherent flaws in the material also decreases and the strength increases.

Fig 2.3 Strength vs Fibre diameter graph b). For better load transfer from matrix to fibre composites require larger surface area of the fibre matrix interface. Fibre matrix interface area: A=NDL (N No. of fibres, D fibre diameter, L length of fibres) Replace D by d (smaller diameter fibres) For same Fibre Volume Fraction*: n = N(D/d)2 New fibre matrix interface area: A= N D2 L/d = 4 * Volume of fibres / d Thus, for a given fibre volume fraction, the area of the fibre-matrix interface is inversely proportional to the diameter of the fibre. * Fibre Volume Fraction (Vf) = Volume of fibres/Volume of Composite

Matrix Volume Fraction (Vm) = Volume of matrix/Volume of composite Vf + Vm = 1 c). The fibres should be flexible/pliant so that they can be bend easily without breaking. For example, woven fibre composites needs flexible fibres. Flexibility is defined as inverse of bending stiffness. Consider a fibre as beam under pure bending, then EI Bending stiffness or Flexural rigidity Flexibility 1/EI Where, I = d4/64 Flexibility 1/Ed4 Thus, flexibility of a fibre is inversely proportional to 4th power of the fibre diameter. 2.3 TYPES OF FIBRES: Advanced Fibres: Fibres possessing high specific stiffness [E/] and specific strength [/]) a) Glass b) Carbon c) Organic d) Ceramic Natural Fibres: a) Animal fibres i) Silk iv) Sinew i) Cotton iv) Sisal b) Vegetable fibres ii) Jute v) Maze
7

ii)Wool

iii) Spider silk

v) Camel hair iii) Bamboo vi) Hemp

vii) Sugarcane x) Kapok xii) Kenaf c) Mineral fibres i) Asbestos iii) Mineral wool

viii) Banana ix) Ramie xii) Abaca xv) Raffia palm..

xi) Coir xiv) Flax

ii) Basalt iv) Glass wool

In the figure 2.4 given below the elements with which the fibres are made is shown by the rounded up oval. They are used for advanced fibre reinforcements for the composites.

Fig 2.4 Periodic Table 2.4 ADVANCED FIBRES: 2.4.1GLASS FIBRES: Ancient Egyptians made containers from coarse fibres drawn from heat softened glass produced by extruding molten glass at 1200C passed through spinnerets of 1-2 mm diameter

 then drawing the filaments to produce fibres of diameter between 1-5 m individual filament is small in diameter, isotropic in behavior and very flexible VARIETY OF FORMS: E glass: high strength and high resistivity S2 glass: high strength, modulus and stability under extreme temperature, corrosive environment R glass: enhanced mechanical properties C glass: resists corrosion in an acid environment D glass: dielectric properties In general, glass fibres are isotropic in nature

Fig 2.5 E-Glass(V-9)

2.5 CARBON FIBRES: carbon- carbon covalent bond is the strongest in nature Thomas Edison made carbon fibre from bamboo when experimenting for light bulb ! Carbon fibre contains 80-95 % of carbon and graphite fibre contains more than 99% carbon carbon fibre is produced at 1300C while graphite fibre is produced in excess of 1900C In general term carbon fibre is used for both fibres Made from two types of precursor materials: 1) Polyacrylonitrile (PAN) (PAN Based) 2) Rayon Pitch - residue of petroleum refining (Pitch Based)

Fig 2.6 Carbon Fibre Precursor fiber is carbonized rather then melting Filaments are made by controlled pyrolysis (chemical deposition by heat) of a precursor material in fiber form by heat treatment at temperature 1000-3000 C Different fibers have different morphology, origin, size and shape. The morphology is very dependent on the manufacturing process. The size of individual filament ranges from 3 to 14 m. Hence, very flexible.

10

 Maximum temperature of use of the fibers ranges from 250 C to 2000 C. Properties changes with temperature at higher temperature. The maximum temperature of use of a composite is controlled by the use temperature of the matrix Modulus and strength is controlled by the process-thermal decomposition of the organic precursor under well controlled conditions of temperature and stress Heterogeneous microstructure consisting of numerous lamellar ribbons Thus, carbon fibers are anisotropic in nature 2.6 ARAMID FIBRES: Aromatic polyamide family of nylons. Polyamide 6 = nylon 6, Polyamide 6.6 = nylon 6.6 Melt-spun from a liquid solution Morphology radially arranged crystalline sheets resulting into anisotropic properties Filament diameter about 12 m and partially flexible High tensile strength Intermediate modulus Very low elongation up to breaking point Significantly lower strength in compression Du Pont developed these fibers under the trade name Kevlar. From poly (p- Phenylene terephthalamide (PPTA) polymer 5 grades of Kevlar with varying engineering properties are available kevlar-29, Kevlar-49, Kevlar-100, Kevlar-119, Kevlar-129

11

Fig 2.7 Aramid Fibres 2.7 TYPES OF MATRIX MATERIALS: 2.7.1 POLYMERS: Thermoplastic: Soften upon heating and can be reshaped with heat & pressure Thermosetting: become cross linked during fabrication & do not soften upon reheating Metals: Ceramics: Carbon and Graphite: 2.7.2 THERMOPLASTICS: polypropylene, polyvinyl chloride (PVC), nylon, polyurethane, poly-ether-ether ketone (PEEK), polyphenylene sulfide (PPS), polysulpone higher toughness high volume low- cost processing Temperature range 225C
12

THERMOPLASTICS: Thermoplastics are increasingly used over thermosets becuase of the following reasons: Processing is faster than thermoset composites since no curing reaction is required. Thermoplastic composites require only heating, shaping and cooling. Better properties: high toughness (delamination resistance) and damage tolerance, low moisture absorption chemical resistance They have low toxity. Cost is high! 2.7.3 THERMOSETS: polyesters, epoxies, polyimides Other resins 2.7.4 POLYESTERS: Low cost Good mechanical strength Low viscosity and versatility Good electrical properties Good heat resistance Cold and hot molding Curing temperature is 120C 2.7.5 EPOXY: Epoxy resins are widely used for most advanced composites.

13

Advantages: Low shrinkage during curing High strength and flexibility Adjustable curing range Better adhesion between fibre and matrix Better electrical properties Resistance to chemicals and solvents Disadvantages: somewhat toxic in nature limited temperature application range upto 175C moisture absorption affecting dimensional properties

high thermal coefficient of expansion slow curing 2.7.6 POLYIMIDES: Excellent mechanical strength 600F) range and short term in 370C (700F) range Excellent electrical properties Good fire resistance and low smoke emission Hot molding under pressure and Curing temperature is 175C (350F) and 315C Excellent strength retention for long term in 260-315C (500-

Problems with using polymer matrix materials: Limited temperature range Susceptibility to environmental degradation due to moisture, radiation, atomic oxygen (in space) Low transverse strength

14

 High residual stress due to large mismatch in coefficients of thermal expansion both fiber and matrix Polymer matrix cannot be used near or above the glass transition temperature 2.7.7 METALS: Aluminum Titanium Copper Higher use temperature range Aluminum matrix composite use temperature range above 300C and titanium at 800 C Higher transfer strength, toughness( in contrast with brittle behavior of polymers and ceramics) The absence of moisture & high thermal conductivity (copper) Disadvantages: Heavier More susceptible to interface degradation at the fiber/matrix interface and to corrosion 2.7.8 CERAMICS: Carbon, Silicon carbide and Silicon nitride Ceramic have use very high temperature range > 2000 C High elastic modulus Low density Disadvantages: brittleness Susceptible to flows

15

2.7.9 CARBON: Carbon fibres in carbon matrix carbon/carbon composites used under extreme mechanical and thermal loads (space applications) Advantages: Low specific weight High heat absorption capacity Resistance to thermal shock High resistance to damage Exceptional frictional properties at high energy levels Resistance to high temperatures Chemical inertness low coefficient of thermal expansion (excellent dimensional stability) Disadvantages: low resistance to oxidation above 500C high cost of materials and manufacturing

16

2.7.10 PROPERTIES OF FIBRE AND MATRIX MATERIALS: Properties of fibre and matrix materials are given in below table 2.1 Material Densi Modu Poisso ty g/cm lus Gpa ns Ratio Streng Specifi th Mpa c Stiffne ss METALS Steel Titanium AS4 T300 P100S IM8 Boron Kevlar 49 SCS-6 Nicalon Alumina S-2 Glass E-Glass Sapphire Epoxy Polyimide Copper Si-Carbide 7.8 4.5 1.80 1.76 2.15 1.8 2.6 1.44 3.3 2.55 3.95 2.46 2.58 3.97 1.38 1.46 8.9 3.2 200 69 91 235 231 724 310 385 124 400 180 379 86.8 69 435 4.6 3.5 117 400 0.32 0.33 0.36 0.20 0.20 0.20 0.20 0.21 0.34 0.25 0.25 0.25 0.23 0.22 0.28 0.36 0.35 0.33 0.25 1724 483 758 3599 3655 2199 5171 3799 3620 3496 2000 1585 4585 3450 3600 58.6 103 400 310 1.0 1.0 0.95 5.1 5.1 13.2 6.7 5.8 3.6 5.1 2.8 3.7 1.4 1.05 4.3 0.08 0.03 0.5 4.9 1.2 1.0 1.2 11.1 11.5 5.5 16.1 8.3 13.9 6.1 4.4 1.9 10.4 7.5 5.1 0.4 0.4 0.3 0.5 12.8 23.4 8.8 -0.8 -0.5 -1.4 --8.3 -2.0 5.0 4.0 7.5 1.6 5.4 8.8 63 36 17 4.8 Aluminium 2.7 Specific Thermal Strengt h Expansi on Coefficie nt

FIBERS

MATRIX MATERIALS

17

CHAPTER-III SELECTION OF MATERIALS Since E-Glass V-9 is a conventional fibre for structural

applications at high temperatures, it is also the insulating and since it is cheap in cost and easily available which is being used for many aerospace applications, hence it is selected. Though the rayon carbon is very expensive, it is amorphous material for ablative purpose and is having vast applications in aerospace industry, hence it is selected. Phenolic resin is the conventional matrix material which is used for aerospace applications to with stand high temperatures. The properties and specifications of these materials are as follows. 3.1 E-Glass V-9:

3.1.1TECHNICAL SPECIFICATIONS a) Nomenclature : E-GLASS FABRIC V-9 (FULLY PROCESSED) b) Thickness, mm c) Width, mm d) Weave e) Count Warp, ends/inch : 442 : 0.78-0.82 : 1000 (nominal) : 8 Harness Satin

18

Weft ends/inch f) Tex Warp, g/km Weft, g/km g) Areal Density, gm/sqm. h) Breaking strengh Warp, kg/inch Weft, Kg/inch i) Compatibility

: 332

: 2136 (approx.) : 2136 (approx.) : 840-930

: 148 minimum : 119 minimum : Should be compatible with Phenolic resin(ILSS of Phenolic laminate should be 15 Mpa minimum)

j) Shelf life

: One year from the date of Manufacture.

3.1.2 ACCEPTANCE TEST PROCEDURE 3.1.2.1 VISUAL INSPECTION: (i) APPEARANCE: The fabric shall be reasonably free from yarn defects and defects of weaving. holes, smashes, abrasions, stains, oil and grease spots or other contaminations, torn selvedges, excessive ends out, missing picks and other permanent distortions. (ii) HOLES AND TEARS: Fabric shall be inspected (100%) and shall not have more than one hole and one torn selvedge per one metre of fabric length. Holes 25mm in maximum dimension or less shall not be cause for rejection unless the holes are of a greater frequency of 10 per roll.
19

The distance between a hole and a tear should not be less than 50 mm. Tears larger than 75 mm in any dimension shall be removed. Abrasions are defined visually as local areas of gross broken filaments. Abrasions marks less than 25 mm in any dimension shall not be cause for rejection unless there are more than 3 in any one meter. (iii) LENGTH AND WIDTH: The length and width of the fabric shall be inspected during visual inspection and the roll length shall not be less than 40 meters nor more than 200 meters. (iv) ANTECEDENTS: Antecedents of each roll of material shall be identified with an unambiguous number and relevant information like Roll No., Date of manufacturing and Date of expiry in indelible ink or with non-removable stickers. It must be ensured that test reports from the supply agency has been provided. 3.1.2.2 SAMPLING: (i) ROLL AND LOT SAMPLING: A roll is defined as a continuous fabric mentioned in 1.3 above. Rolls shall be selected randomly 1:5 minimum for each lot. A lot will be considered as 5 rolls. A sample of 0.5 meter length and of full width of the fabric shall be cut from inner and outer end of a roll for testing. (ii) CONTROL SAMPLING: A sample will be drawn at any point of time by the authorized inspection agency, the sample will be sealed and will be subjected to all conformity tests in order to ensure the consistency in quality of the fabric during production.
20

3.1.2.3 CONFORMITY TESTS: The sample fabric selected shall be tested for all requirements mentioned below. There shall be no failure in respect of any of the requirements, if lot is to be accepted. 3.1.2.4 THICKNESS: Thickness of the fabric shall be inspected by dial thickness gauge. The acceptance value shall be 0.78-0.82 mm. 3.1.2.5 COUNT: Fabric count shall be inspected as per IS 3442 (ASTM D3775) using a Magnifying and counting eye piece to confirm the thread count. The acceptance value shall be Warp 442 and Weft 332 ends/inch. 3.1.2.6 TEX & AREAL DENSITY: Mass per Unit length (Tex) and Mass per Unit area (Areal Density) of the fabric shall be inspected as per IS 1964 (ASTM D578 and ASTM D3776)The acceptance value shall be Tex 272 g/km and Areal Density 840-930 gm/sqm 3.1.2.7 BREAKING STRENGTH: The breaking strength of the fabric shall be inspected as per ASTM D1682.5 specimens of Warp and 5 specimens of Weft shall be tested The acceptance value shall be Warp 148 Kg/inch and Kg/inch minimum. Weft 119

21

3.1.2.8 ILSS: Compatibility of fabric with Phenolic resin shall be determined by ILSS test as per ASTM D2344. 10 specimens minimum shall be tested for whole lots of same batch. The acceptance value shall be 15 MPa minimum. 3.1.2.9 PACKING: The fabric shall be rolled evenly on tubes of sufficient length and strength to produce firm packages so as to prevent collapsing or telescoping during transit, storage or handling. Both ends of the roll and edges shall be suitably protected to prevent damage to the edges and surface of the cloth and the whole shall be packed in moisture proof containers. The fabric shall be packed in the form of rolls weighing not more than 200 Kg. No pack shall contain more than 3 pieces of fabric. 3.1.2.10 STORAGE: To ensure stable quality of fabric during storage, it shall be stored in dry, if possible, air-conditioned room in original unopened packing. Direct sunlight shall be avoided. The rolls shall be stored horizontally avoiding external pressure to the glass fabric. Under these conditions, the storage life of the finished fabric is normally one year. 3.1.2.11 EXTENSION OF SHELF LIFE: The shelf life of the glass fabric can be extended for one more year at any given time. The properties to be tested for extension of life are Breaking Strength & ILSS (Ref 7.0 & 8.0). Three extensions, one year each, can be permitted for a specific batch.

22

3.2 RAYON BASED CARBON: 3.2.1 TECHNICAL SPECIFICATIONS Carbon cloth shall be derived from woven continuous Rayon Filament yarn. Chemical Properties Minimum Carbon Content, Wt% Ash Content , Wt% pH Value Sodium Content, ppm Physical Properties Specific Gravity, Breaking Strength Warp Weft Weight , Gms/M2 Thread Count Warp (Ends/Inch) Weft (Picks/Inch) Thickness, mm By Federal gauge By Dial thickness gauge Width, mm Moisture Content, Wt% Type of Weave Structure 0.3 0.4 990 ----8Harness satin Amorphous 0.4 0.5 1100 5 48 45 58 55 9.1 Kg/Inch 6.8 Kg/Inch 255 --------325 1.7 1.9 94 ----7 ----Maximum ----1 11 800

23

3.2.2 ACCEPTANCE TEST PROCEDURE 3.2.2.1 ANTECEDENTS Each roll of fabric shall be identified with an unambiguous number and relevant information like roll no, date of manufacturing in indelible ink or with stickers. Once the roll of fabric is manufactured it must be stored in a room where proper humid conditions are being maintained. It must be ensured that in-house test reports from the supplying agency have been obtained. 3.2.2.2 VISUAL INSPECTION Visual inspection shall be carried out as per ASTM D4029 on every roll of fabric in order to find-out defects such as discolored patches, tears, any holes and stains etc., if such defects present overall length of fabric the roll should be rejected. 3.2.2.3 THICKNESS Thickness (t) of the fabric shall be inspected as per ASTM D1777 The acceptance value shall be 0.3-0.4 mm by federal gauge (Average of any three values meeting the specification out of five values at different places is acceptable) The acceptance value shall be 0.4-0.5 mm by dial gauge 3.2.2.4 WIDTH Width (b) of the fabric shall be inspected as per ASTM D3774 The acceptance value shall be 990 1100 mm 3.2.2.5 AREAL DENSITY Areal density of the fabric shall be inspected as per ASTM D3776 The acceptance value shall be 255- 325 GSM

24

3.2.2.6 SPECIFIC GRAVITY Specific gravity shall be inspected as per ASTM D792. The acceptance value shall be 1.7 - 1.9 3.2.2.7 THREAD COUNT The fabric shall be inspected using a Magnifying and Counting Eye piece to confirm the thread count. The acceptance value shall be Warp: 48 58 Ends /Inch & Weft: 4555 Picks / Inch 3.2.2.8 BREAKING STRENGTH Breaking strength of the fabric shall be inspected as per ASTM D1682 The acceptance value shall be Warp : 9.1 Kg/Inch (Minimum) Weft : 6.8 3.2.2.9 PH VALUE pH Value shall be determined as per ASTM D2165.The acceptance value shall be 7-11 3.2.2.10 CARBON CONTENT Carbon content shall be measured by instrumental method of analysis using CHNS analyser. The acceptance value shall be 94% (minimum) 3.2.2.11 SODIUM CONTENT Sodium content shall be determined by instrumental method of analysis using Flame Photometer. The acceptance value shall be 800 ppm (Maximum) Kg/Inch (Minimum)

25

3.2.2.12 ASH CONTENT Ash content of the cloth shall be determined as per ASTM C561The acceptance value shall be 1 %( Maximum) 3.2.2.13MOISTURE CONTENT Moisture content of the cloth shall be determined as per ASTM D2654 The acceptance value shall be 5%(Maximum) since cloth undergoes pre-heating during impregnation. 3.3 PHENOLIC RESIN: INTRODUCTION Phenolics are thermosetting resins produced by the reaction of Phenol with formaldehyde in the presence of a catalyst. Phenolic resins are available commercially in wide variety of types. The two main types are a single-stage resole and a two-stage novolac. The resole phenolic is the most widely used, because of its handling characteristics in the impregnated form. It cures by means of a condensation type reaction in which water is formed as a by-product. The water is removed by vacuum or distillation and resin redissoved in alcohol for most uses. Phenolics have high heat and chemical resistance, good dielectric properties, dimensional and thermal stability, and surface hardness. They yield low smoke and toxicity properties after combustion. However,

Moisture content deviation from specification up to 10% can be accepted,

26

Table-3.1 Technical specifications (at the time of procurement) S. No. 1. 2 3. 4. 5. Parameter Grade Colour Viscosity at 30c Specific gravity at 30 C Point of trouble at specific gravity o.860 6. 7. 8. 9. 10. Volatile content Solid resin content Free Formaldehyde Free Phenol Shelf life 32 38 % by weight 60 65% by weight 3.0 % Maximum 6.0 % Maximum One month at 25 C from the date of manufacture Specified value ABRON PR100(WS)/IVAREZ ISRO Honey red colour liquid 100 to 150cps 1.12 to 1.16 8 to 12 C.C

Table-3.2 Technical specification (at the time of prepregging) The Phenolic Resin will be tested for following properties not more than 24 hours prior to Pre-pregging and should meet following values Sl.N0. 1 2 3 4 PARAMETER Specific gravity Viscosity at 30c, CPS Point of trouble, CC Volatile content,% SPECIFIED VALUE 1.12-1.16 150-500 6-8 32-38

27

3.3.1 STORAGE CONDITIONS Phenolic resin must be stored at 4c in their original containers. The products shall remain in good conditions for three months from the date of manufacturing. Opened containers must be closed immediately after use. 3.3.2 SOURCE OF SUPPLY (a) M/S ABR ORGANICS LIMITED, A3, Sri Madhava Apartments, Bank colony, Bagh Amberpet, Hyderabad 500 013 (b) M/S IVP LIMITED, 604, Karan Centre, Sarojini Devi Road, Secunderabad 500 003 3.3.3 ACCEPTANCE TEST PROCEDURE The antecedents of the Phenolic resin shall be verified as regards to the date of manufacture, adherence to storage conditions and shelf life of the material. It must also be ensured that the test reports from the supplying agency are obtained. The following tests out of properties specified are to be carried-out as per standards specified and the test values should be within the specified limits. 3.3.3.1SPECIFIC GRAVITY The specific gravity of resin should be measured at 30c as per ASTM D891.The acceptance value shall lie between 1.12 to 1.16. 3.3.3.2VISCOSITY The viscosity of the resin shall be measured at 30c using Viscometer as per ASTM D 2393.The acceptance value shall lie between 150 to 350 CPS.
28

3.3.3.3POINT OF TROUBLE Point of trouble is a measure of the degree of the advancement of polymerization of the resin. The resin shall be diluted with ethyl alcohol 99.98 % purity to get the specific gravity of 0.860 of solution. 10 ml. of this solution shall be titrated against distilled water to the turbidity point and the volume of water consumed in the process is the point of trouble. The acceptance value shall lie between 8 to 12 cc Phenolic resin should be conditioned before impregnation for making prepregs. Point of trouble of conditioned Phenolic resin before impregnation shall be 6 to 8 cc, and all other specified parameters shall be same. If the point trouble falls below 6 cc, which occurs with the passage of time, it is an indication the resin has a more advanced stage of polymerization and therefore shall be unsuitable for use. 3.3.3.4VOLATILE CONTENT Take a 1-2 gms of a resin sample from a well mixed lot in a silica crucible weighed to an accuracy of 0.1 milligrams. The resin sample shall be heated at 160C for 20 minutes in an oven. Crucible is then cooled to room temperature and weighed. Net weight of the empty crucible be Weight of crucible + resin sample = W1 gms = W2 gms

Weight of crucible (with resin) after heating for 20 minutes at 160C % Volatile Content = W3 gms =(w2-w3/w2-w1)*100

The acceptance value shall lie between 32 to 38%

29

CHAPTER-IV FABRICATION TECHNIQUES Manufacturing techniques for composites are not dependent on the type of matrix material. In fact, some metal forming techniques have been adapted to composites fabrication (e.g., matched-metal die molding). However, processing conditions are entirely dependent on the type of matrix material used. For instance, thermosets require long processing times, whereas thermoplastics require relatively high pressures and temperatures. 4.1 FABRICATION OF FIBROUS COMPOSITES: There are more than 50 processes depending upon fibre and matrix material type and nature. Some of them are illustrated below. Wet/Hand Lay-Up Spray Lay-Up Vacuum Bagging Filament Winding Pultrusion Resin Transfer Molding (RTM) Pre-pregg Resin Film Infussion 4.1.1 WET/HAND LAY-UP DESCRIPTION Resins are impregnated by hand into fibres which are in the form of woven, knitted, stitched or bonded fabrics. This is usually accomplished by rollers or brushes, with an increasing use of nip-roller type impregnators for forcing resin into the fabrics by means of rotating rollers and a bath of resin. Laminates are left to cure under standard atmospheric conditions.
30

Main Advantages: Widely used for many years. Simple principles to teach. Low cost tooling, if room-temperature cure resins are used. Wide choice of suppliers and material types. Higher fibre contents, and longer fibres than with spray lay-up Main Disadvantages: Resin mixing, laminate resin contents, and laminate quality are very dependent on the skills of laminators. Low resin content laminates cannot usually be achieved without the incorporation of excessive quantities of voids. Health and safety considerations of resins. The lower molecular weights of hand lay-up resins generally means that they have the potential to be more harmful than higher molecular weight products. The lower viscosity of the resins also means that they have an increased tendency to penetrate clothing etc. Limiting airborne styrene concentrations to legislated levels from polyesters and vinylesters is becoming increasingly hard without expensive extraction systems. Resins need to be low in viscosity to be workable by hand. This generally compromises their mechanical/thermal properties due to the need for high diluent/styrene levels. Typical Applications: Standard wind-turbine blades, production boats, architectural mouldings

31

Fig 4.1 Wet/Hand lay-up 4.1.2 SPRAY LAY-UP: DESCRIPTION Fibre is chopped in a hand-held gun and fed into a spray of catalysed resin directed at the mould. The deposited materials are left to cure under standard atmospheric conditions. Main Advantages: Widely used for many years. Low cost way of quickly depositing fibre and resin. Low cost tooling. Main Disadvantages: Laminates tend to be very resin-rich and therefore excessively heavy. Only short fibres are incorporated which severely limits the mechanical properties of the laminate. Resins need to be low in viscosity to be sprayable. This generally compromises their mechanical/thermal properties. The high styrene contents of spray lay-up resins generally means that they have the potential to be more harmful and their lower viscosity means that they have an increased tendency to penetrate clothing etc. Limiting airborne styrene concentrations to legislated levels is becoming increasingly difficult.
32

Typical Applications: Simple enclosures, lightly loaded structural panels, e.g. caravan bodies, truck fairings, bathtubs, shower trays, some small dinghies.

Fig 4.2 Spray lay-up 4.1.3 VACUUM BAGGING: DESCRIPTION This is basically an extension of the wet lay-up process described above where pressure is applied to the laminate once laid-up in order to improve its consolidation. This is achieved by sealing a plastic film over the wet laid-up laminate and onto the tool. The air under the bag is extracted by a vacuum pump and thus up to one atmosphere of pressure can be applied to the laminate to consolidate it . Main Advantages: Higher fibre content laminates can usually be achieved than with standard wet lay-up techniques. Lower void contents are achieved than with wet lay-up. Better fibre wet-out due to pressure and resin flow throughout structural fibres, with excess into bagging materials. Health and safety: The vacuum bag reduces the amount of volatiles emitted during cure.

33

Main Disadvantages: The extra process adds cost both in labour and in disposable bagging materials A higher level of skill is required by the operators Mixing and control of resin content still largely determined by operator skill Typical Applications: Large one-off cruising boats, racecar components, core-bonding in production boats.

Fig 4.3 Vacuum bagging 4.1.4 FILAMENT WINDING: DESCRIPTION This process is primarily used for hollow, generally circular or oval sectioned components, such as pipes and tanks. Fibre tows are passed through a resin bath before being wound onto a mandrel in a variety of orientations, controlled by the fibre feeding mechanism, and rate of rotation of the mandrel.

34

Main Advantages: This can be a very fast and therefore economic method of laying material down. Resin content can be controlled by metering the resin onto each fibre tow through nips or dies. Fibre cost is minimised since there is no secondary process to convert fibre into fabric prior to use. Structural properties of laminates can be very good since straight fibres can be laid in a complex pattern to match the applied loads. Main Disadvantages: The process is limited to convex shaped components. Fibre cannot easily be laid exactly along the length of a component. Mandrel costs for large components can be high. The external surface of the component is unmoulded, and therefore cosmetically unattractive. Low viscosity resins usually need to be used with their attendant lower mechanical and health and safety properties.

Fig 4.4 Filament winding

35

4.1.5 PULTRUSION: DESCRIPTION Fibres are pulled from a creel through a resin bath and then on through a heated die. The die completes the impregnation of the fibre, controls the resin content and cures the material into its final shape as it passes through the die. This cured profile is then automatically cut to length. Fabrics may also be introduced into the die to provide fibre direction other than at 0. Although pultrusion is a continuous process, producing a profile of constant cross-section, a variant known as pulforming allows for some variation to be introduced into the crosssection. The process pulls the materials through the die for impregnation, and then clamps them in a mould for curing. This makes the process non-continuous, but accommodating of small changes in cross-section. Main Advantages: This can be a very fast, and therefore economic, way of impregnating and curing materials. Resin content can be accurately controlled. Fibre cost is minimised since the majority is taken from a creel. Structural properties of laminates can be very good since the profiles have very straight fibres and high fibre volume fractions can be obtained. Resin impregnation area can be enclosed thus limiting volatile emissions. Main Disadvantages: Limited to constant or near constant cross-section components Heated die costs can be high.

36

Typical Applications: Beams and girders used in roof structures, bridges, ladders, frameworks.

Fig 4.5 Pultrusion

4.1.6 RESIN TRANSFER MOLDING (RTM): DESCRIPTION Fabrics are laid up as a dry stack of materials. These fabrics are sometimes pre-pressed to the mould shape, and held together by a binder. These preforms are then more easily laid into the mould tool. A second mould tool is then clamped over the first, and resin is injected into the cavity. Vacuum can also be applied to the mould cavity to assist resin in being drawn into the fabrics. This is known as Vacuum Assisted Resin Injection (VARI). Once all the fabric is wet out, the resin inlets are closed, and the laminate is allowed to cure. Both injection and cure can take place at either ambient or elevated temperature. Main Advantages: High fibre volume laminates can be obtained with very low void contents. Good health and safety, and environmental control due to enclosure of resin. Possible labor reductions. Both sides of the component have a molded surface.

37

Main Disadvantages: Matched tooling is expensive and heavy in order to withstand pressures. Generally limited to smaller components. Un impregnated areas can occur resulting in very expensive scrap parts. Typical Applications: Small complex aircraft and automotive components, train seats.

Fig 4.6 RTM 4.1.7 PRE-PREGG: DESCRIPTION Fabrics and fibres are pre-impregnated by the materials manufacturer, under heat and pressure or with solvent, with a precatalysed resin. The catalyst is largely latent at ambient temperatures giving the materials several weeks, or sometimes months, of useful life when defrosted. However to prolong storage life the materials are stored frozen. The resin is usually a near-solid at ambient temperatures, and so the pre-impregnated materials (prepregs) have a light sticky feel to them, such as that of adhesive tape. Unidirectional materials take fibre direct
38

from a creel, and are held together by the resin alone. The prepregs are laid up by hand or machine onto a mould surface, vacuum bagged and then heated to typically 120-180C. This allows the resin to initially reflow and eventually to cure. Additional pressure for the moulding is usually provided by an autoclave (effectively a pressurised oven) which can apply up to 5 atmospheres to the laminate. Main Advantages: Resin/catalyst levels and the resin content in the fibre are accurately set by the materials manufacturer. High fibre contents can be safely achieved. The materials have excellent health and safety characteristics and are clean to work with. Fibre cost is minimised in unidirectional tapes since there is no secondary process to convert fibre into fabric prior to use. Resin chemistry can be optimised for mechanical and thermal performance, with the high viscosity resins being impregnable due to the manufacturing process. The extended working times (of up to several months at room temperatures) means that structurally optimised, complex lay-ups can be readily achieved. Potential for automation and labour saving. Main Disadvantages: Materials cost is higher for preimpregnated fabrics. Autoclaves are usually required to cure the component. These are expensive, slow to operate and limited in size. Tooling needs to be able to withstand the process temperatures involved Core materials need to be able to withstand the process temperatures and pressures.
39

Typical Applications: Aircraft structural components (e.g. wings and tail sections), F1 racing cars, sporting goods such as tennis racquets and skis.

Fig 4.7 Pre-Pregg

4.1.8 RESIN FILM INFUSION: DESCRIPTION Dry fabrics are laid up interleaved with layers of semi-solid resin film supplied on a release paper. The lay-up is vacuum bagged to remove air through the dry fabrics, and then heated to allow the resin to first melt and flow into the air-free fabrics, and then after a certain time, to cure. Main Advantages: High fibre volumes can be accurately achieved with low void contents. Good health and safety and a clean lay-up, like prepreg.
40

 High resin mechanical properties due to solid state of initial polymer material and elevated temperature cure. Potentially lower cost than prepreg, with most of the advantages. Less likelihood of dry areas than SCRIMP process due to resin travelling through fabric thickness only. Main Disadvantages: Not widely proven outside the aerospace industry. An oven and vacuum bagging system is required to cure the component as for prepreg, although the autoclave systems used by the aerospace industry are not always required. Tooling needs to be able to withstand the process temperatures of the resin film ( which if using similar resin to those in lowtemperature curing prepregs, is typically 60-100C). Core materials need to be able to withstand the process temperatures and pressures. Typical Applications: Aircraft radomes and submarine sonar domes.

Fig 4.8 Resin film infusion

41

4.2 SELECTION OF THE FABRICATION PROCESS: Several factors should be considered before selecting the

manufacturing process for a particular part; User requirements Performance requirements Total production volume Production rate Cost of production Size of the production Surface finish of the final product Geometry of the product Material These are important for all manufacturing processes, and even more so for composite materials Ideally, structural design of the product, and design of the required manufacturing process should be completed using a concurrent approach. Table-4.1 Selection of manufacturing process. PROCESS Filament winding Pultrusion Fast PRODUCTION COST SPEED Slow to fast Low high Low to High medium Wet lay up Slow to High Small to large No restricion on length Medium Medium to Medium high to large STRENGTH SIZE

42

Spray up Rtm Srim

Medium fast Medium Fast

to Low Low Low

Low to Medium Medium

Small to medium Small to medium Small to medium Small to medium Medium to Small Small to medium

medium

Compression Fast molding Stamping Injection moulding Roll wrapping Medium fast Fast Fast

Medium Medium Low Low to Low Medium Low medium to High medium

43

CHAPTER-V EXPERIMENTAL WORK In this project the matrix is conventional phenolic resin and it is modified with Di-amine and ether. By this modification it is observed that when phenolic resin is modified with Di- amine the gel time is increased. And point of trouble is decreased considerably. Similar changes are observed in the properties of the resin by modifying with ether. In this experimental work the following types of laminates were made: a) E-Glass (V-9)/Phenolic composite b) E-Glass (V-9)/Di-amine modified phenolic composite c) E-Glass (V-9)/ether modified phenolic composite d) Rayon carbon/ether modified Phenolic composite e) Rayon carbon/Di-amine modified Phenolic composite

5.1 PREPARATION OF LAMINATE BY HAND LAY-UP PROCESS: Even though the method has been replaced with automated techniques, the lay-up of pre impregnated material by hand is the oldest and most common fabrication method for advanced composite structures. Furthermore, the basic features of the method remain unchanged. A pictorial essay showing each step in the hand lay-up of a flat composite laminate is shown in Figures 5.1-5.14. Each step must follow in successive fashion in order to obtain a high-quality composite laminate after final processing. A description of these steps follows. Step 1: The surface of the tool is cleaned and a release agent is applied. If the surface is not clean, then the release agent will not function properly. The release agent can be in liquid form, or it may be a
44

solid film. (In the photo-essay, to provide an indication of scale, a handheld pointer or knife is included in the photographs.)

Fig 5.1 The mold is covered with a release film Step 2: An optional sacrificial layer is laid up on the tool surface. This layer is usually a fiberglass fabric made with the same resin system as the composite laminate. The sacrificial layer protects the laminate from surface abrasion and surface irregularities during manufacturing. Step 3: A peel ply is placed on top of the sacrificial layer. The peel ply will be removed after processing.

Fig 5.2 A peel ply is laid on the top of film Step 4:The preimpregnated plies are cut according to design specifications. They can be cut by hand using shears or a steel blade knife. However, automated cutting machines have largely replaced hand cutting. The Gerber knife is a reciprocating-knife system originally
45

developed for the textile industry. It is extremely fast and can cut up to 20 plies at one time. Lasers have been used for cutting, but they are expensive and have limitations on the number of plies that can be cut at one time. Water-jet cutters are also used extensively, and they can cut a large number of plies (> 40) at one time, but some moisture absorption occurs during the cutting operation. Ultrasonic cutters have been used as well.

Fig 5.3 Prepreg plies are cut to design Step 5: The first prepreg ply is oriented and placed upon the tool or mold. Subsequent plies are placed one upon another; a roller or other small hand tool is used to compact the plies and remove entrapped air that could later lead to voids or layer separations. It is important that the preimpregnated material have sufficient tack so that it sticks slightly to the peel ply and to the adjacent plies. Tackiness, a characteristic of pre impregnated material, quantifies the relative stickiness of the plies at room temperature. As the pre impregnated material ages, its tackiness is reduced. Eventually, the plies no longer stick together and they may have to be heated slightly to soften them during lay-up. Oils and dirt on the surface of the pre impregnated plies will contribute to reducing composite strength after processing. Technicians should wear gloves
46

during lay-up so that oils and dirt from the hands do not contaminate the pre-preg plies during lay-up. In some cases the hand lay-up procedure may be carried out in a clean room to reduce the risk of contamination of the pre-preg plies.

Fig 5.4 prepreg plies are oriented and laid on tool Step 6: A flexible resin dam is anchored to the sacrificial layer approximately 3 mm from the edge of the laminate. The dam prevents resin flow out of the laminate, in the plane of the laminate. Flexible dams can be made from silicon rubber, cork, or release coated metal. (As no sacrificial layer is being used in the procedure here, the flexible dam is anchored to the peel ply.)

47

Fig 5.5 A Flexible reisn dam is anchored Step 7: Another peel ply is placed on top of the laminate to protect the laminate surface.

Fig 5.6 A peel ply is placed on the laminate Step 8: A sheet of porous release film is laid over the dam and the laminate. The porous release film will serve as a barrier to prevent bonding of the composite laminate to the secondary materials to follow. Step 9: Next, bleeder plies are laid up over the release film, in this case the peel ply. The bleeder plies extend to the edge of the laminate. The number of bleeder plies to be used for a given laminate can be determined by using a resin flow process model or through empirical observation. As the number of bleeder plies increases, the final fiber volume fraction of the composite laminate increases. Eventually, a
48

maximum number of bleeder plies is reached and no further increase in fiber volume fraction occurs.

Fig 5.7 Bleeder plies are laid up Step 10: Another porous release ply is next laid up over the bleeder plies extending past the flexible dam. This prevents excessive resin flow into the breather material while maintaining a vacuum pathway into the composite laminate. Step 11: Breather plies are placed over the entire lay-up. The breather plies will conduct the vacuum path into the laminate. It is critically important that sufficient breather material is used throughout the entire laminate. Creases and areas with shallow curvature are sometimes reinforced with additional layers of breather material to ensure that the breather plies do not collapse in these areas. Usually, two or three breather plies are sufficient. Step 12: An edge bleeder is used to connect to the vacuum ports. An edge bleeder is nothing more than a strip of breather material folded along its length several times. It is placed so that it overlays the breather material surrounding the laminate and extends out to a convenient location for the placement of the vacuum port. Step 13: Caul plates are sometimes placed on top of the lay-up. The caul plate is steel or aluminum plate that protects the surface from

49

sharp temperature increases (it acts as a heat sink) and it gives a smooth non-wavy surface texture.

Fig 5.8 Caul plates are placed on the lay up Step 14: If a caul plate is used, then additional breather or bleeder plies are placed over the plate to protect the vacuum bag from puncture.

Fig 5.9 Additional bleeder plies are placed Step 15: Sealant tape is placed around the entire periphery of the lay-up.

Fig 5.10 Sealant tape is placed

50

Step 16: The vacuum bag is cut to size and placed over the lay-up. Step 17: The bag is sealed by pressing the bag over the sealant tape. It is critically important to ensure that the bag is adequately sealed before proceeding to the processing cycle. Many parts are scrapped because the vacuum fails during processing, causing excessive voids, inadequate resin flow, or incomplete consolidation.

Fig 5.11 Bag is Sealed Step 18: The vacuum port is installed through the bag and the contents are evacuated. The bag is now checked for leaks. If any are detected, they are repaired before processing. Usually a leak test calls for application of a vacuum to some specified level (cm of Hg), followed by a 30-60 minute hold. During the hold the bag is disconnected from the vacuum source and the pressure level within the bag is monitored. If the bag is sealed well and there are no leaks, then the vacuum level should not change for the 30-60 minutes. Some leaking generally occurs, so it is a question of having sufficient vacuum pump capacity to maintain the specified vacuum level. When the vacuum is satisfactory, the composite part is ready for processing. The specific processing steps depend on the particular composite material being used, and the operation of the autoclave depends on the specific make and model. General discussions

51

of processing and autoclave features are presented in the sections to follow.

Fig 5.12 Vaccum port is installed and keeping in auto clave Obviously, there is a significant amount of skilled labor necessary for the hand lay-up of composite parts. Each step has a specific purpose and function. This type of fabrication is the most time-consuming, but it is also the most flexible and when combined with autoclave processing, it results in high-quality parts. Automated equipment can be used to cut and place the preimpregnated material onto the tool surface. The economics of manufacturing dictate that a relatively large volume of parts must be made to make automated equipment cost-effective. 5.2 AUTOCLAVE CURING: The best quality parts are cured using an autoclave. Autoclaves have been used extensively for processing high-performance composite materials in the civilian and military aerospace industries. An autoclave
52

consists of a large cylindrical metal pressure vessel with end enclosures that is thermally insulated and heated. Most autoclaves have a forcedhot-gas circulation system as well. An autoclave is pressurized using air or an inert gas such as nitrogen. What distinguishes the autoclave from the curing oven and hot press, to be discussed later, is the ability to cure parts using large, hydrostatic like pressure. A typical autoclave can pressurize up to 20 atm. The large majority of composite structures can be processed using autoclaves with 2-4 m internal diameter, although some extremely large aerospace structures require autoclaves over 20 m in diameter. The capital equipment costs and operating costs for large autoclaves make this type of processing very costly. However, the high quality and high performance of autoclaved parts makes them attractive for certain applications. A typical autoclave is shown in schematic form in Figure 5.15. The primary component is the pressure vessel itself, which is cylindrical and contains embedded heaters and cooling coils. A door at one end allows access to the interior to load parts and perform periodic maintenance. Also, several ports may be installed through the autoclave wall for access to the interior. Some of these ports are dedicated to vacuum lines connected to the parts to be cured. Others are used for control functions such as thermocouples, dielectric sensors, and pressure sensors, all of which help monitor the curing of the material. The interior of the autoclave is heated by radiation from the vessel walls and convection of hot gases as they circulate through the vessel. A circulating fan forces the hot gases through a series of baffles within the autoclave in a circulation loop that runs the length of the autoclave. Typically, this fan is housed at one end of the autoclave and the interior gases are drawn from the central portion of the cylinder, through the baffles, and they return to the other end through a jacket that covers the interior wall. The autoclave applies a pressure to the outer surface of the composite part through pressurization of the interior gases. This pressure is then transferred through the tool plate(s), breather plies,
53

bleeder plies, and other secondary materials to the laminate surface. From there the pressure is shared between the fiber and matrix during curing. The most important aspect is the matrix resin pressure during cure. If it is too low, then voids can grow in the resin or inadequate resin bleeding may occur. In general, composite structures which have been processed in an autoclave exhibit uniform thicknesses, good consolidation, and very low void content.

Fig 5.13 Auto clave

Fig 5.14 Typical Cure cycle

54

5.3 LAMINATE MACHINING & CUTTING: Machining of laminate is an art. Because if it is cut by an ill skilled person it could no more seem like a good one. And to cut the laminates made by fiber reinforcements polymer matrixes normal cutter will not be useful. Hence it should be cut by the machine shown in the figure 5.15 since it is having the diamond edge to cut so that it can appear like smooth surface after cutting by which. A laminate which is cut by the diamond edge cutter is as shown in the figure 5.16.

Fig 5.15 Cutting of Laminate

Fig 5.16 Specimens cut from laminate

55

CHAPTER-VI NON DESTRUCTIVE TESTS NDT is used to detect defects and as a check either in new items or in items already in service, as maintenance checks. In both cases the items is not damaged in any way by the test procedure. The main aim is to detect poor compaction leading to resin-rich areas or low fibre loading, bad surface appearance or internal defect such as: a) Lack of reinforcement: b) Porosity: c) Poor fibre- matrix bonding (delamination) d) Cracks of all sizes: e) Failure of the adhesive bond between components f) Inclusions Note that the notion of defect or discontinuity in a composite material is enhanced since these materials are characterized by their heterogeneous nature. Any defect that is detected must be determined: a) In area or volume b) By its location within the structure in relation to the laryers of reinforcement c) By its relation to the mechanical stresses to which the material may be subjected. A defect of a constant type and size may be unimportant in any case, but serious in another. Thus a series of air bubbles between two layers may be harmful if the material is subjected to a shear or flexural stress but the same defect occurring in a different item subjected to tension or compression would be of no consequence.
56

Tremendous advances have been made in the field of NDT in the last few years. Formerly the philosophy was to check for the absence of detects. Currently the trend is towards differentiating between those that are harmful to the structure and those that are not. Considerable effort is being made to automate error. Universal criteria for assessing the seriousness or otherwise of defects cannot be defined in the absence of a complete knowledge of the artifact and the way it will be employed. Owing to the fact that the aerospace industry requires fail-proof parts, non-destructive test methods were first introduced by companies working in this field. Individual companies have their own acceptance/ rejection criteria but do not publicize these. The techniques used are complementary. In principle the methods used are very often similar to those recommended for homogeneous and metal objects. However, their application to heterogeneous laminates and commercial committees are trying to establish standards in this area. 6.1 Non Destructive Tests on Laminates: a) Ultrasonics b) X-ray, radiography; 6.1.1 Ultrasonic tests (US): Low- frequency ultrasonic (0.2 to 15MHz) can propagate through composites. The anisotropic, heterogeneous nature of the material causes alteration and dispersion of the beam. From a theoretical point of view, propagation is a complex phenomenon because of the two- phase nature of the system (fibre and resin). Structural defect interfere with the propagation of US and partially reflect the sound waves. Hence two methods have been develop based on reflection and transmission of the
57

signal. At best lamination defects measuring 0.2mm can be detected. The presence of voids reduces the transmission of US, and the method used can be used to quantify void content. The transmission speed of US increases with increasing fibre loading and the method can be used to determine the fibre loading of a unidirectional composite. The US method is complementary to X-ray or IR thermography, and is suitable for the detection of internal delamination.

Fig 6.1 Illustration of ultrasonic flaw detection Different types of ultrasonic methods: There are three principal methods of ultrasonic testing of aerospace materials. (a) The pulse-echo method (b) The through transmission method and (c) The pitch-catch method.

58

These three ultrasonic method use pulses of energy during testing operations. 6.1.1.1 THE PULSE-ECHO METHOD In the pulse-echo method, a piezoelectric transducer with its longitudinal axis located perpendicular to and mounted on or near the surface of the test material is used to transmit and receive ultrasonic energy. The ultrasonic waves are reflected by opposite face of material or by discontinuities. Layer, voids, or inclusions in the material, and received by the same transducer where the reflected energy is converted into an electrical signal. The electrical signal is computer processed for display on a video monitor or tv screen. The display can show the relative thickness of the material, depth into the material where the flaws are located, and (with proper scanning hardware and software), where the flaws are located in the X-Y plane. In aerospace application, the pulseecho method is used primarily for the detection of flaws in metals but has been used for first and second bond line interrogation in solid rocket motors (each transmitted/received wave in figure represent a pulse of energy).

Fig 6.2 pulse-echo method of ultrasonic testing

59

6.1.1.2THE THROUGH-TRANSMISSION METHOD In the through-transmission method, an ultrasonic transmitter is used on one used on one side of the material while a detector is placed on the opposite side. Scanning of the material using this method will result in the location of defects, flaws, and inclusions in the X-Y plane. These methods is used for nondestructive testing of multilayered and multicomponents materials as encountered in solid rocket motor case/insulation/liner/propellants, in composite material, and on highly attenuative materials.(Each transmitted/received wave in Fig5.19 represents a pulse of energy).

Fig 6.3Through-transmission method of ultrasonic testing The following figure 6.4 shows the amplitude of the defect of our laminate made by E-glassV-9 with phenolic resin.

60

Fig 6.4Amplitude of the defect of the laminate 6.1.1.3THE PITCH-CATCH METHOD The pitch-catch method, in which the ultrasonic energy is transmitted at any angle to the surface of the material and received as reflected energy returning at the reflected angle, is used primarily for cylindrical tubes and other nonlinear parallel sided surfaces. The pitchcatch method can determine depth of the flaw in the material as well as detect the location in the X-Y plane through scanning.(Each transmitted/received wave in fig6.5 represents a pulse of energy).

Fig 6.5 pitch-catch method of ultrasonic testing

61

6.1.2 Radiography-X and Gamma ray tests: This technique is suitable for the detection of internal defects in ferrous and non ferrous metals and other materials. X-rays, generated electrical, and gamma rays emitted from radioactive isotopes, are penetrating radiation which is differentially observed by the material through which it passes the greater the thickness, the greater the absorption. Furthermore, the denser the material has the greater the absorption. X and gamma rays also have the property, like light, of partially converting silver halide crystals in a photographic film to metallic silver, in proportion to the intensity of the radiation reaching the film, and therefore forming a latent image. This can be developed and fixed in a similar way to normal photographic film. Material with internal voids is tested by placing the subject between the sources of radiation and the film. The principles are the same for both X and Gamma radiography. In X-radiography the penetrating power is determine by the number of volts applied to the X-ray tube in steel approximately 1000 volts per inch thickness is necessary. The time of exposure must be increased as the isotopes decays when the exposure period becomes uneconomical the isotopes must be renewed. As the isotopes is continuously emitting radiation it must be housed in a container of deleted uranium or similar dense shielding materials, which not exposed to protect the environment and personnel. To produce an X OR Gamma radiograph, the film package (comprising film and intensifying screensthe latter being required to reduce the exposure time-enclosed in a light tight cassette) is placed close to the surface of the subject. Various radiography and photographic accessories are necessary, including such items as radiation monitors, film makers, image quality indicators, darkroom equipment etc. These accessories are the same for both X and
62

Gamma radiography system. Also required are such consumable items as radiographic film and processing chemicals.

Fig 6.6 An illustration of radiography test Recent developments in radiography permits real time diagnosis. Such techniques computerized tomography yield much important information, through these methods maybe suitable for only investigative purposes and not generally employed in production quality control. The defect of the laminate is observed as shown in the figure 6.7 below.

Fig 6.7 Defect observed in radiography film

63

CHAPTER-VII DESTRUCTIVE TESTS The destructive tests are to determine the physical properties of the material. For the laminates that we made with fibre reinforcements and matrix the destructive tests are done according to the ASTM standards. The test procedures are as follows. 7.1 DENSITY TEST ( ASTM-D-792): Theory: Density of composite is determined by Archimedes principle according to it, any object, completely or partially immersed in a fluid, is buoyed by a force equal to the weight of the fluid displaced by the object. i.e., apparent immersed weight = actual weight weight of displaced fluid Then it is inserted into the quotient of weights, which has been expanded by the mutual volume. (Density/density of fluid )=(weight/weight of displaced fluid) Thus the density of the immersed object relative to the density of the fluid can easily be calculated without measuring any volumes as follows. (Desity of object/density of fluid)=(weight/weight-apparent immersed weight) Procedure: Take the test specimen dimensions as per the ASTM D- standard denotes. i.e., 20x10x5. Measure the weights of the specimens in the air by pykinometer.
64

Fig 7.1 pykinometer Now measure the weights of specimens by immersing them in distilled water. Calculate the difference of the weights. Now the density of the specimen is obtained by the following formula (Densityof specimen)=(Weight in air/weight in air-weight in distilled water) gm/cc Repeat this for three test specimens and get the average value. 7.2 RESIN CONTENT TEST: This test is done by burn off method because the fabric in laminate is E-Glass V-9. For Rayon fibre we use nitric acid digestion method. BURN-OFF METHOD (ASTM D-2584): The test is done in the furnace. Wait till the temperature of the furnace up to 600C After temperature reaches to 600C, the test piece kept in furnace for one hour as shown in the figure 7.2. The resin gets evaporated at this temperature and fabric plys are remained in the furnace. The weight of the fabric plys should be measured.
65

 The difference between total weight of the test piece and fabric plys will give the percentage of resin content in the laminate.

Fig 7.2Oven NITRIC ACID DIGESTION METHOD (ASTM D-3171): This test is done using nitric acid Measure the temperature of the Rayon carbon using pykinometer Keep the rayon carbon in the nitric acid until they are digested as shown in the figure7.3 Then separate the acid and fibre Now the fibre is free of resin, hence measure the weight of that fibre Calculate the difference between the total test specimen and the fibre is resin content value.

66

Calculation of Density and Resin content tests: Table:7.1 Density & Resin content test results Density & Resin content test Density S.NO. Material E-GlassV1 9/Ph(DA) E-GlassV2 9/Ph(E) 3 Rayon/Ph(DA) 4 Rayon/Ph(E) 1.767 1.3 1.29 19.1 28.49 29.13 80.9 71.51 70.87 56.27 53.12 52.24 1.92 19.16 80.84 61.1 (gm/cc) Resin (% of wt) Fiber (% of wt) Vf (% of Vol.)

Fig 7.3 Nitric acid digestion

7.3 OXYACETYLENE EROSION TEST (ASTM Designation E-285): Theory: This test method is intended to screen the most obvious poor materials from further consideration. Since the most combustion gases more closely resemble the environment generated in rocket motors, this
67

test method is more applicable to screening materials for nozzles and motor liners than for aerodynamic heating. In this test we could not calculate the heat flux and could not measure the velocity the flame though it is a neutral flame. Hence it can give information about the comparison of erosion rates of the different materials. Procedure: Place the specimen in the holder and secure it firmly. Set the distance between the specimen face and torch tip to 19.0 0.3mm and angle between torch and specimen to 90 3. Ignite the torch and adjust the gas flow rates to the conditions. After flow conditions are stabilized, terminate the test at the instance that burn-through is detected. Record the burn - through time. And calculate the erosion rate. Erosion rate=(thickness of specimen/burn through time)m/s

Fig 7.4 Settings of erosion test

68

Calculations of Erosion rate: Table:7.2 erosion rate test results Thickness S.NO. Material E-GlassV1 9/Ph E-GlassV2 9/Ph(DA) E-GlassV3 9/Ph(E) 4 Rayon/Ph(DA) 5 Rayon/Ph(E) 7.4 ILSS (ASTM D 2344): Theory The INTER LAMINAR SHEAR STRENGTH (ILSS) is done using a 3-point test of flexure. The specimen is as per the standard dimensions. The material direction under investigation must be oriented along the length of the specimen. The test pieces require a span/depth ratio low enough to minimize the influence of bending deformation and achieve failure shear rather than bending. The ILSS is calculated as follows ILSS=(3*load/4*width*thickness)N/mm2 4.9 4.32 5 11.22 0.00043672 34.4 0.000125581 37.71 0.000132591 4.01 10.72 0.000374067 3.61 12.25 0.000294694 (mm) Burn through time (sec) Erosion rate (m/S)

69

Fig 7.5 Testing of ILSS Procedure: As per the standard the specimen dimensions should be 40mm x 10mm x 5mm. Keep the specimen in the UTM as shown in the figure 7.5 with the span length of four times of the thickness of specimen. Now gradually apply the load on mid span of the specimen. Note down at which load the shear is occurred. Using that load calculate the ILSS of the specimen. Repeat this for ten specimens and consider the average value of which. Calculations of ILSS: Table 7.3 ILSS test results E-Glass V-9/Phenolic (E) S.NO. Dimensions(mm) Max.Load(KN) 0.9 0.91 0.94 0.92
70

Max.Displ.(mm) ILSS(Mpa) 0.292 0.276 0.341 0.351 14.76 15.11 14.93 14.65

1 9.98x4.58 2 9.90x4.56 3 9.96x4.74 4 9.98x4.72

5 9.92x4.70 6 10.0x4.64 7 10.08x4.64 8 9.84x4.64 9 10.0x4.66 10 10.12x4.72

0.86 0.84 0.95 0.9 0.82 0.92 Average E-Glass V-9/Phenolic (DA)

0.316 0.364 0.268 0.339 0.342 0.254

13.83 13.57 15.23 14.78 13.19 14.44 14.449

S.NO.

Dimensions(mm) 1 10.18x3.98 2 9.9x4.0 3 10.4x3.96 4 10.2x3.98 5 10.0x4.0 6 10.0x3.98 7 10.3x4.0 8 10.0x4.0 9 10.1x3.96

Max.Load(KN) 1.63 1.44 1.68 1.56 1.45 1.62 1.62 1.58 1.67 1.62

Max.Displ.(mm) 0.585 0.356 0.463 0.421 0.43 0.502 0.388 0.324 0.533 0.438

ILSS(Mpa) 30.17 27.27 30.59 28.82 27.18 30.52 29.49 29.62 31.31 30.375 29.5345

10 10.0x4.0

Average

Rayon/Phenolic (DA) S.NO. Dimensions(mm) 1 9.62x4.08 2 9.70x4.10 3 9.76x4.2 4 9.68x4.04 5 10.2x4.32 Max.Load(KN) 0.71 0.92 0.82 0.91 0.89 Max.Displ.(mm) 0.345 0.574 0.362 0.509 0.282 ILSS(Mpa) 13.56 17.34 15 17.45 15.14

71

6 9.82x4.2 7 10.06x4.36 8 10.0x4.12 9 9.86x4.18 10 9.74x4.1

1.13 0.67 1.02 0.92 0.93 Average Rayon/Phenolic (E)

0.419 0.52 0.549 0.935 0.378

20.54 11.45 18.56 16.74 17.46 16.324

S.NO.

Dimensions(mm) 1 9.52x4.82 2 9.7x5.0 3 9.7x5.0 4 9.6x4.98 5 9.9x5.0 6 10.0x5.0 7 10.0x5.0 8 10.0x5.0 9 9.8x5.0

Max.Load(KN) 0.97 0.65 0.99 0.75 1.14 0.66 0.93 0.8 0.81 0.83

Max.Displ.(mm) 0.356 0.317 0.432 0.437 0.478 0.517 0.432 0.33 0.315 0.425

ILSS(Mpa) 15.85 10.05 15.3 11.76 17.27 9.9 13.95 12 12.39 12.83 13.13

10 9.7x5.0

Average E-Glass V-9/Phenolic S.NO. Dimensions(mm) 1 10.32x3.56 2 10.24x3.54 3 10.08x3.64 4 10.00x3.56 5 10.00x3.64 Max.Load(KN) 1.65 1.71 1.54 1.52 1.78 Max.Displ.(mm) 0.418 0.321 0.565 0.508 0.32

ILSS(Mpa) 33.68 34.55 31.47 32.02 36.67

72

6 10.34x3.54 7 10.28x3.56 8 10.28x3.64 9 10.36x3.54 10 10.34x3.6

1.53 1.53 1.59 1.68 1.52 Average

0.393 0.337 0.38 0.363 0.355

31.34 31.35 31.86 34.35 30.62 32.791

7.5 FLEXURAL STRENGTH (ASTM D-790): Theory: The FLEXURAL STRENGTH (FS) is done using a 3-point test of flexure The specimen is as per the standard dimensions. The material direction under investigation must be oriented along the length of the specimen. The FS is calculated as follows FS=(3*load*span length/2*width*thickness) Procedure: As per the standard the specimen dimensions should be 100mm x 10mm x 5mm. Keep the specimen in the UTM with the span length of sixteen times of the thickness of specimen. Now gradually apply the load on the mid span of the specimen. Note down at which load the bending is occurred. Using that load calculate the FS of the specimen. Repeat this for five specimens and consider the average value of which. The Flexure of the specimen will be as shown in the figure 7.6

73

Fig 7.6 Flexural test

74

Calculations of the Flexural test: Table 7.4 Flexural strength results E-Glass V-9/Phenolic (DA) F.S S.NO. Dimensions(mm) 1 10.34x3.91 2 9.86x3.94 3 10.21x3.94 4 10.0x3.98 5 9.96x3.95 Max.Load(KN) 0.82 0.73 0.75 0.78 0.7 Average E-Glass V-9/Phenolic (E) F.S S.NO. Dimensions(mm) 1 10.2x4.9 2 9.74x4.77 3 9.99x4.78 4 10.05x4.87 5 10.03x4.83 Max.Load(KN) 0.4 0.44 0.46 0.44 0.41 Average Rayon/Phenolic (DA) F.S S.NO. Dimensions(mm) 1 9.78x4.45 2 9.79x4.24 3 10.6x4.32 Max.Load(KN) 0.43 0.35 0.31 Max.Displ.(mm) 4.085 3.454 2.924 (Mpa) 228.2 205.5 157.4 E (Gpa) 18.35 21.46 42.48 Max.Displ.(mm) 3.019 2.691 2.662 2.687 2.66 (Mpa) 195.8 237 243.1 219.2 209.5 220.92 E (Gpa) 27.05 30.78 14.66 26.43 34.79 26.742 Max.Displ.(mm) 3.11 2.99 2.761 2.997 2.682 (Mpa) 497.6 457.5 454.1 473.4 431.3 462.78 E (Gpa) 44.97 46.15 40.87 42.49 45.58 44.012

75

4 9.93x4.25 5 9.78x4.3

0.38 0.39

3.935 3.501

217.04 220.3

22.36 12.49

Average Rayon/Phenolic (E)

205.688 F.S

23.428

S.NO.

Dimensions(mm) 1 9.79x4.95 2 9.37x4.98 3 9.75x4.97 4 9.80x4.99 5 9.63x4.98

Max.Load(KN) 0.27 0.35 6.28 0.39 0.25

Max.Displ.(mm) 2.68 2.6 2.416 3.795 2.564

(Mpa) 133.6 126.3 89

E (Gpa) 21.52 19.31 23.73 15.05

104 _ 80.3

Average E-Glass V-9/Phenolic

106.64 19.9025

F.S S.NO. Dimensions(mm) 1 9.96x3.52 2 9.88x3.53 3 9.84x3.56 4 9.95x3.55 5 9.91x3.56 Max.Load(KN) 0.53 0.52 0.57 0.53 0.56 Average Max.Displ.(mm) 3.526 2.305 2.352 2.272 2.334 (Mpa) 363 356.8 381 351 376.8 365.72 E (Gpa) 26.97 18.17 36.16 35.59 35.81 30.54

76

7.6 IMPACT STRENGTH (ASTM D 5941): Theory: The angle of tip of hammer = 751 The angle between normal to the specimen and underside face of the hammer at striking point = 101 Speed of hammer at impact =3.99 m/s Striking energy = 168 N-m or J Angle of drop of pendulum = 90 Effective weight of pendulum = 21.79 kg Permissible total friction loss of corresponding energy = 0.50% Length of the pendulum = 0.796m Time period of the pendulum = 1.79 sec

Procedure:

Fig 7.7 Izod impact test Conduct the test in the same atmosphere as that used for conditioning, unless otherwise agreed upon by the interested parties, for example, for testing at high or low temperatures.
77

 Measure the thickness and the width of each test specimen, in the centre, to the nearest 0.02mm. Check that the pendulum machine has the specified velocity of impact and that it is in the correct range of absorbed energy, which shall be between 10 and 80% of the pendulum energy. Conduct a blank test and record the measured values of the total frictional loss. Ensure that this energy loss does not exceed the appropriate value as per the standard. If frictional losses are equal to or less than the standard values, they may be used in the calculation of corrected energy absorbed. If they exceed, care should be taken to evaluate the cause of any excess frictional losses and corrections made, as necessary, to the equipment. Lift and support the pendulum. Place the specimen in the vice, and clamp it as shown in the figure 7.7 Release the pendulum. Record the impact energy absorbed by the specimen, and apply any necessary corrections for frictional losses. Calculations of Impact strength: Table 7.5 Impact energy test results E-Glass V-9/Phenolic (DA) C/S Area S.NO. (sq.mm) 1 40.198 2 40.198 3 40.198 Average Absorbed Energy (J) 10 11 11 Impact Energy (KJ/sq.m) 248.76 273.65 273.65 265.3533333

E-Glass V-9/Phenolic (E)

78

C/S Area S.NO. 1 2 3 (sq.mm) 46.51 46.51 46.51

Absorbed Energy (J) 5 6 6

Impact Energy (KJ/sq.m) 107.5 129 129 121.8333333

Average

Rayon/Phenolic (DA) C/S Area S.NO. 1 2 3 (sq.mm) 41.03 41.03 41.03 Average Rayon/Phenolic (E) C/S Area S.NO. 1 2 3 (sq.mm) 48.75 48.75 48.75 Average E-Glass V-9/Phenolic C/S Area S.NO. 1 2 3 (sq.mm) 35.046 35.046 35.046 Average Absorbed Energy (J) 8 8 7.5 Impact Energy (KJ/sq.m) 228.27 228.27 214 223.5133333 Absorbed Energy (J) 3 3 3 Impact Energy (KJ/sq.m) 61.54 61.54 61.54 61.54 Absorbed Energy (J) 2 2 2 Impact Energy (KJ/sq.m) 48.74 48.74 48.74 48.74

79

CHAPTER-VIII RESULTS AND DISCUSSION The following are the test results of composite laminates made for this project work. These test results are obtained by destructive testing process, the test results are given in below tables for comparision. Flexural load and inter laminar shear strength graphs are given in below figures. Table 8.1 Test results comparison Resin Density S.NO. Material E-GlassV1 9/Ph(DA) 2 E-GlassV-9/Ph(E) 3 Rayon/Ph(DA) 4 Rayon/Ph(E) 1.92 1.767 1.3 1.29 19.16 19.1 28.49 29.13 80.84 80.9 71.51 70.87 61.1 56.27 53.12 52.24 (gm/cc) content (% of wt) Fiber content (% of wt) Vf (% of Vol.)

Table 8.2 Test results comparison Youngs ILSS S.NO. Material E-GlassV1 9/Ph(DA) E-GlassV2 9/Ph(E) 3 Rayon/Ph(DA) 4 Rayon/Ph(E) 14.45 220.92 16.32 205.69 13.13 106.64 26.74 23.43 19.9 30.54 121.83 0.000436 48.74 0.000126 61.54 0.000133 223.51 0.000294 29.53 462.78 44.01 265.35 0.000374 F.S Modulus E (Gpa) (Mpa) (Mpa) Impact Energy I (KJ/sq.m) Erosion rate (m/s)

5 E-GlassV-9/Ph 32.79 365.72

80

FS Comparison
0.9 0.8 0.7 Load(KN) 0.6 0.5 0.4 0.3 0.2 0.1 0 0 1 2 3 4 5 Position(m) E-Glass V9/Ph(DA) E-Glass V9/Ph(E) E-Glass V9/Ph Rayon/Ph(DA) Rayon/Ph(E)

Fig 8.1 Flexural load comparison graph

ILSS Comparison
1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 0 0.2 Positin(m) 0.4 0.6

Load(KN)

Rayon/Ph(DA) Rayon/Ph(E) E-glass V9/Ph(DA) E-Glass V9/Ph(E)

Fig 8.2 ILSS comparison graph

81

DISCUSSION: It is observed from the tested data E-glass V-9/phenolic

conventional composite compared with modified phenolic E-glass V-9 composite, the Flexural strength and Impact strength of the Di-amine modified phenolic composite gave higher values. Whereas ether modified phenolic composite with E-glass V-9 gave poor values indicates the compatibility problem of the matrix to reinforcements. Where ever Impact application is more one can go for Di-amine modified phenolic composite. The density variation in the composite is because of the compatibility of the matrix to reinforcements. Consolidation of composite during fabrication plays a major role on properties of the material. It is obvious from the test data better compaction has high density and will have low porosity. Composite density is calculated theoretically may not always be same with the experimentally determined value. This is due to poor compaction and voids present in the composite. A good composite for better properties should have higher density. Composite with modified Di-amine is having is having good compatibility so is its density. Even though E-glass V-9 is having high density its composites are used as insulating applications particularly where large amounts of heat to be absorbed or deflected. Rayon carbon/phenolic composite erosion rate is low due to amorphous nature of the material. Aerospace applications such as heat shields, nose cones and nozzles where ablative property is important these rayon/phenolics are used because they absorb large quantity of heat with the sacrificial loss of minimum material. A Known defect which was identified with NDT tests such as Ultrasonic test and Radiography test. Ultra sonic through transmission loss observed at particular zone gave the resemblance of introduced defect. This is studied by Radiography which shown the defect by the difference of the material densities. Both these NDT tests are complimentary to each other. Defect
82

in the composite leads to bad performance so composite products for aerospace applications should meet all quality control checks before being inducted into the machine.

83

CONCLUSION Applications of fibre reinforced polymer matrix composites for aerospace structures have been studied. Different fibre reinforced polymer matrix composite laminates were fabricated by Autoclave vacuum bagging process. Specimens were cut by diamond edge cutter as per ASTM standards and their physical, mechanical and thermal properties were evaluated by destructive and non destructive techniques. Conventional phenolic resin and modified phenolic resin were studied with E-glass V-9 and Rayon carbon fabrics. Phenolic resin is used as a matrix material because of its excellent thermal properties. Phenolic resin modified by Diamine exhibited high flexural and impact strength. Composites made of E-glass V-9 and Rayon carbon replaced many metallic components because of their low density and high heat capacity. For high temperature applications in aerospace carbon phenolics are used as ablative materials because of their low erosion. E-glass composites because of their insulating character utilized for heat resistant composite. Quality control checks play crucial role in the fabrication of aerospace components. Defect free components ensure better performance of the mission. In this project work we dealt with fabrication and testing of aerospace composite materials. Composite laminate properties were evaluated both by destructive and non destructive techniques. Fibre volume fraction, density, non destructive evaluations are essential for the acceptance of any composite product for its intended end use.

84

REFERENCES 1) Carbon-Carbon Materials and Composites By John D. Buckley

Published: December 1993. 2) Composite Structures Safety Management By Dr. Bjorn

Backman, Structure and Materials Structured Research, Camano Island, WA, USA Published: December 1997. 3) Carbon Fiber Composites By Deborah Chung, Niagara Mohawk

endowed Chair Professor, Professor of Mechanical and Aerospace Engineering @ State Univ. of New York Published: December 1994. 4) Carbon/Phenolic Nanocomposites as Advanced Thermal Protection

Material in Aerospace Applications By J.S.Tate. 5) 6) Composite materials for aerospace structures By Dr Douglas. Composite materials for Aerospace application By S.J Dastin

Published: December 2007. 7) Manufacturing Processes for Advanced Composites By Flake

Campbell Jr, Senior Technical Fellow at the Boeing Phantom Works in Missouri, USA. Published: July 2001. 8) Analysis of Composite Structures By Christian Decolon,

Associate Professor of Mechanics at the Conservatoire National des Arts et Mtiers (CNAM), France Published: July 2003. 9) Application of Fracture Mechanics to Composite Materials By

K. Friedrich Published: November 1989. 10) Fatigue of Composite Materials By K.L. Reifsnider, Virginia

Polytechnic Institute and State University, Blacksburg, VA, USA Published: July 1991.

85

11)

Fracture Mechanics Testing Methods for Polymers, Adhesives and

Composites By D.R. Moore, Business Research Associate, ICI plc, UK Published: July 2012. 12) NDT Data Fusion By Xavier Gros, BSc(Hon), MSc, PhD,,

Independent NDT Centre, France Published: November 1996. 13) 14) 15) Damage Detection in Composite materials By S.Mark. Non Destructive testing of composite materials By Ajay Kapadia. ASTM-hand book.

86