ceramic and cermet coating with advanced

CIDETEC FOUNDATION-LOCALIZATION

- RTD Foundation created in 1997

- Member of IK4 Technological Alliance

1405 researchers 2011: 103 M Turnover

- CIDETEC:

9 Laboratories in 5000 m2

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 FeCl3 > 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 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)


ELECTROPHORETIC DEPOSITION

Cold rolled austenitic

stainless steel tube

EPD Cell: Aqueous suspensions of non- commercial ceramic enamels (SiO2, Na2O, K2O, TiO2, 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


Ceramic Coating

Substrate

Ceramic Coating

Substrate

MORPHOLOGYCAL


Substrate Ceramic coating

Important decrease of roughness, avoiding corrosive

particles adhesion


MORPHOLOGYCAL Roughness: Profilometry and AFM


F = 300.000mN/20s

C = ---

R = Same as load increase

C = ---

0.2 0.4 0.6 0.8 1.0 1.2 1.4h [m]

50

150

250

F [mN]

CERAMIC COATING IS HARDER THAN THE SUBSTRATE


MECHANICAL Hardness test

HARDNESS (HV)

84010 ELASTIC MODULUS EIT

(GPa)

87


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


Abrasion resistance

0 cycles 10000 cycles Mass loss for 10000 cycles:

wn = < w0 > - < wn >

Substrate

w10000 = 94.783 94.725

w10000 = 58 mg

Ceramic coating

w10000 = 119.377 119.374

w10000 = 3 mg


High Stainless Steel Ceramic coating

5 cm

10 cm

15 cm

MECHANICAL


Impact resistance

NO CERAMIC COATING DETACHMENTS AT MEDIUM LOADS: GOOD ADHERENCE

Before After


MECHANICAL


Thermal cycling (450C)

0 cycles 1 cycle 2 cycles 3 cycles 4 cycles 5 cycles 6 cycles

Air cooled


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/cm2 of anodic current density

o Potential sweeping velocity: 1mV/s



-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)

vs. A

g/A

gC

l/K

Cl (3

,5M

)

log J (mA/cm2)

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% FeCl3

Steps:

1. 24 hours in 10% FeCl3 at room temperature

2. 72 hours in 10% FeCl3 at 50 C

o Determination of weight loss:

Maximum 4g/m2 (Norsok)



10% FeCl3

Stainless steel Ceramic coating

0 h (25 C)

72 h (50 C)

Weight Loss

(g/m2) >700 0


- Crevice Corrosion Resistance:

ASTM G48A

Method B-Ferric Chloride Crevice Corrosion Test:

o Conditions:

Solution: 10% FeCl3 at 22 C

Steps:

1. Fasten TFE-fluorocarbon block and crevice to the

test specimen with rubber band

2. 72 hours in 10% FeCl3 at 22 C

3. Visual inspection



block crevice


Stainless Steel Ceramic coating




- 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


- 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






- Molten salt Corrosion Resistance :

Conditions:

Molten salt composition: NaNO3 + KNO3 (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

ceramic and cermet coating with advanced

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