CIDETEC FOUNDATION-LOCALIZATION

- RTD Foundation created in 1997

- Member of IK4 Technological Alliance
1405 researchers
2011: 103 M Turnover
- CIDETEC:
9 Laboratories in 5000 m
2

115 Researchers, with 40% PhD and 90% Degree
2011 Turnover: 9,5 M
3 Technical Departments
Energy
Surface Finishing
New Materials
CIDETEC FOUNDATION
CIDETEC FOUNDATION Kera-coat
Batteries Unit
Fuel Cells Unit
Coatings Unit
LIGHT ALLOYS ANODISATION (Al, Mg & Ti)
SOL-GEL COATINGS
ELECTRODEPOSITION COATINGS
Processes Unit
ELECTROPHORETIC DEPOSITION (EPD)
AESTHETIC SURFACE COLOURING
PHYSICAL TREATMENTS (Laser, PVD)
ELECTROCHEMICAL MACHINING (ECM)
ENVIRONMENTAL ELECTROCHEMISTRY
Nanotechnology Unit
Biomaterials Unit
Sensors & Fotonics Unit
Surface Finishing
New Materials
Energy
SCALING-UP EPD PROCESSES
SPIN OFF
KERACOAT
FACILITIES
PROCESS &
PROTECTION
CERAMIC COATING
Properties of ceramics
CERAMIC
COATING
CERAMIC COATINGS PROCESS
Corrosion/oxidation resistance
Thermal
Electrical
Optical
Magnetic
Wear-resistant
Sol-gel
Vapour phase: PVD and CVD
Thermal Spray Process: LVOF, HVOF, VPS and APS
Laser
Electrophoretic deposition (EPD)
Electrophoretic deposition is a colloidal processing
technique to deposit thin films and coatings on substrates.
After EPD, the obtained coating, which is in fact still a
powder compact, has to be densified by a heat treatment.
CERAMIC COATING
Technique Thickness
Coatings
Materials
Temperature
of work
Geometry of
the pieces
Substrate Investment
Process
Cost
PVD 2- 4 m
Ceramic
and metal
200 500 C
Metal,
glass and
ceramic
4 3
CVD 6 9 m
Ceramic
and metal
1000 C
Metal and
ceramic
4 4
Plasma
Thermal
spraying
1- 5 m
Refractory
materials
600 C
Metal and
ceramic
4 3
HVOF >700m Ceramic 800 1000 C
Metal and
ceramic
4 3
EPD 1900 m
Ceramic,
composite
and cermet
25 C
Metal,
ceramic
and
others
2 2
CERAMIC COATING PROCESS
CERAMIC COATING BY EPD R+D
CERAMIC
COATING BY EPD
ACCESIBILITY TO INTRINCATE
SHAPES AND FLEXIBILITY
HIGH HARDNESS
(> 700Hv)
HIGH CORROSION RESISTANCE
FeCl
3
> 72h at 50 C
Salt spray test > 1000 h
VARIABLE SINTERING
TEMPERATURE .
(600 - 950 C)
LOW ROUGHNESS (< 0.04 m)
VITREOUS FINISH
CONDENSING HEATING BOILERS
Ceramic coating for acid environment
corrosion protection in copper alloys
AERONAUTICAL AND
AUTOMOTIVE
COMPONENTS
Cermets coatings for high-precision
special alloy mechanical components
Technical ceramic coating with
improvement of mechanical and
tribological properties for tool steels
TOOL
MACHINE
MEDICAL APPLICATIONS
Bioceramic coatings for dental
implants
CERAMIC COATING BY EPD R+D

CERAMIC
COATING BY EPD
APPLICATIONS

PIPE AND EQUIPMENT TO
PETROCHEMICAL
AND CHEMICAL INDUSTRY
Inert barrier coating with advanced anticorrosive
properties for austenitic stainless steels
AESTHETIC APPLICATIONS
Aesthetic and functional ceramic
coating
ALUMINIUM

CERAMIC
COATING BY EPD
METAL
SUBSTRATES

TECHNOLOGICAL IMPROVEMENT OF DIFFERENT METAL SUBSTRATES SURFACE
COPPER
STAINLESS STEEL
CARBON STEEL
CAST IRON
R+D
IN DIFFERENT METAL
SUBSRATES (BRASS,
TITANIUM)
CERAMIC COATING BY EPD R+D
ELECTROPHORETIC DEPOSITION
Cold rolled
austenitic
stainless steel
tube

EPD Cell:
Aqueous suspensions
of non- commercial
ceramic enamels (SiO
2
,
Na
2
O, K
2
O, TiO
2,
etc.)
EPD PROCESS
Ceramic coating
deposited over
metal substrate
Thermal
treatment
Outside coating
Inner coating
CERAMIC COATING
PROPERTIES
Thickness: Optical microscopy
Continuous and homogeneous coating.
Thickness can be adjust modifying EPD
parameters based on final coating properties


COATING CHARACTERIZATION
MORPHOLOGYCAL
CERAMIC COATING PROPERTIES (R+D)
Joining metal and ceramic : SEM
- Low density of cracks and bubbles
- High joining between substrate and ceramic coating
- The adhesion between coating and substrate is strong
COATING CHARACTERIZATION
Ceramic
Coating
Substrate
Ceramic
Coating
Substrate
MORPHOLOGYCAL
CERAMIC COATING PROPERTIES (R+D)
Substrate Ceramic coating
Important decrease of
roughness, avoiding corrosive
particles adhesion
COATING CHARACTERIZATION
MORPHOLOGYCAL
Roughness: Profilometry and AFM
CERAMIC COATING PROPERTIES (R+D)
F = 300.000mN/20s
C = ---
R = Same as load increase
C = ---
0.2 0.4 0.6 0.8 1.0 1.2 1.4
h [m]
50
150
250
F [mN]
CERAMIC COATING
IS HARDER THAN
THE SUBSTRATE
COATING CHARACTERIZATION
MECHANICAL
Hardness test
HARDNESS (HV)
84010
ELASTIC MODULUS EIT
(GPa)
87
CERAMIC COATING PROPERTIES (R+D)
THE IMPROVEMENT OF HARDENESS AND ELASTICITY IS POSSIBLE MODIFYING
THE STRUCTURE AND COMPOSITION OF CERAMIC COMPOUNDS IN ORDER
TO CERAMIC COATING FINAL PROPERTIES REQUIRED
MECHANICAL
COATING CHARACTERIZATION
Abrasion resistance
0 cycles 10000 cycles
Mass loss for 10000 cycles:
w
n
= < w
0
> - < w
n
>
Substrate
w
10000
= 94.783 94.725
w
10000
= 58 mg

Ceramic coating
w
10000
= 119.377 119.374
w
10000
= 3 mg
CERAMIC COATING PROPERTIES (R+D)
High Stainless Steel Ceramic coating
5 cm
10 cm
15 cm
MECHANICAL
COATING CHARACTERIZATION
Impact resistance
NO CERAMIC COATING
DETACHMENTS AT MEDIUM
LOADS: GOOD ADHERENCE
Before After
CERAMIC COATING PROPERTIES (R+D)
MECHANICAL
COATING CHARACTERIZATION
Thermal cycling (450C)
0 cycles 1 cycle 2 cycles 3 cycles 4 cycles 5 cycles 6 cycles
Air
cooled
CERAMIC COATING PROPERTIES (R+D)
MODIFYING CERAMICS
COMPOUNDS IS POSSIBLE TO
OBTAIN CERAMIC COATING WITH
DIFFERENTS TEMPERATURE
RESISTANCE
CORROSION RESISTANCE
-Pitting potential measurement:
- JIS G-0577:2005
- Conditions:
o Solution: 5% NaCl, 25 C
o Counter electrode: Platinum
o Reference electrode: Ag/AgCl
o The tested surface was fully immersed in test
solution for 2 h
o The test was conducted by potentiokinetic
method from natural electrode potential to 1
mA/cm
2
of anodic current density
o Potential sweeping velocity: 1mV/s
COATING CHARACTERIZATION
CERAMIC COATING PROPERTIES (R+D)
-9 -8 -7 -6 -5 -4 -3 -2 -1 0 1 2
-0,4
-0,2
0,0
0,2
0,4
0,6
0,8
1,0
AISI 316L
Ceramic coating T153
E

(
V
)

v
s
.

A
g
/
A
g
C
l
/
K
C
l

(
3
,
5
M
)
log J (mA/cm
2
)
Ecorr Log Jcorr
(mV vs Ag/AgCl) (mA/cm
2
)
Stainless Steel -106 -2.54
Ceramic coating UNALTERED
CORROSION
- Pitting Corrosion Resistance:
ASTM G48A
Method A-Ferric Chloride Pitting test:
o Conditions:
Solution: 10% FeCl
3

Steps:
1. 24 hours in 10% FeCl
3
at room temperature
2. 72 hours in 10% FeCl
3
at 50 C
o Determination of weight loss:
Maximum 4g/m
2
(Norsok)
COATING CHARACTERIZATION
CORROSION RESISTANCE
10%
FeCl
3

Stainless steel
Ceramic
coating
0 h
(25 C)

72 h
(50 C)


Weight
Loss
(g/m2)
>700 0
CERAMIC COATING PROPERTIES (R+D)
- Crevice Corrosion Resistance:
ASTM G48A
Method B-Ferric Chloride Crevice Corrosion Test:
o Conditions:
Solution: 10% FeCl
3
at 22 C
Steps:
1. Fasten TFE-fluorocarbon block and crevice to the
test specimen with rubber band
2. 72 hours in 10% FeCl
3
at 22 C
3. Visual inspection
COATING CHARACTERIZATION
CORROSION RESISTANCE
block crevice
CERAMIC COATING PROPERTIES (R+D)
Stainless Steel Ceramic coating
COATING CHARACTERIZATION
CORROSION RESISTANCE
CERAMIC COATING PROPERTIES (R+D)
- Seawater Corrosion Resistance (Offshore):
Conditions:
Solution: 3,5% NaCl at 22 C
Visual inspection after test

Seawater Corrosion Test
0 h

1000 h

2000 h

HIGH CORROSION
RESISTANCE FOR
OFFSHORE
APPLICATIONS
CORROSION RESISTANCE
- Acid Corrosion Resistance :
Conditions:
Solution: 10% HCl at 22 C
Visual inspection after test

Acid Corrosion Test
0 h

1000 h

2000 h

LOST OF BRIGHTNESS
DURING THE TIMING
TEST, BUT THE CERAMIC
COATING CONTINUES TO
PROTECT THE METAL
SUBSTRATE
COATING CHARACTERIZATION
CERAMIC COATING PROPERTIES (R+D)
CORROSION RESISTANCE
COATING CHARACTERIZATION
CERAMIC COATING PROPERTIES (R+D)
- Molten salt Corrosion Resistance :
Conditions:
Molten salt composition: NaNO
3
+ KNO
3
(60/40)
Blocks of molten salts positioned over the ceramic
coating
46 cycles HEATING (8 hours at 400C)/COOLING
(air cooled)
Visual and optical microscopy inspection

Initial test
After 46 cycles /Before cleaning
After 46 cycles / Surface clean
SURFACE
UNALTERED
R+D SOLUTIONS
R+D SOLUTIONS FOR NEW DEMANDING
MATERIALS
R+D SOLUTIONS FOR NEW DEMANDING
MATERIALS