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2012, Brno, Czech Republic, EU

ADHESION PROPERTIES OF THE PLASMA SPRAY COATINGS

1-2

Ekrem ALTUNCU, 2Fatih USTEL

Kocaeli University, School of Asim Kocabiyik, Dept. Machine-Metal Tech. Hereke Borusan Campus, altuncu@kocaeli.edu.tr

Sakarya University, Metallurgical and Materials Eng. , Thermal Spray R&D Center, Esentepe Campus, ustel@sakarya.edu.tr

Abstract Plasma sprayed thermal barrier coatings (TBCs) are widely used in gas turbines to reduce thermal effect and increase turbine efficiency. Depending on the application of plasma spray coating, different characteristics are important but there are some characteristics that are the same for all plasma spray applications: thickness, porosity, microstructure, presence of unmelted particles, cracks and oxides, microhardness and bond strength. The poor bonding between splats and the imperfections in the form of pores or thermal cracks cause the thermo-mechanical property values of plasma spray coatings. Bond strengths of TBCs were tested with the standard test method ASTM C 633. Porosity and unmelted particles ratio generally decreases adhesion tensile test values since a pore of critical size can induce a macroscopic failure with tensile stress applied. It was observed that the spray parameters: plasma gas flow rates, plasma current , powder feed rate and spray distance are important effective parameters on the microstructure as well as bond strength of the coatings. Keywords: Plasma Spray, TBC, Bond Strength, ASTM C633 1. INTRODUCTION

Plasma spray deposition method is the most flexible or versatile thermal spray process. Plasma spray have been used to improve thermal protection, wear and erosion resistance, chemical stability and biocompatibility [1]. Plasma spray coating characteristics are very dependent on feedstock powder properties, substrate surface condition and spray parameters. Mechanical properties of the coatings are related with microstructural features [2,3]. There are more than 50 macroscopic parameters that influence the quality of the plasma spray coating. Depending on the application of plasma spray coating, different characteristics are important but there are some characteristics that are the same for all applications: thickness, porosity, microstructure, presence of unmelted particles, cracks and oxides, microhardness and bond strength [4]. The poor bonding between splats and the imperfections in the form of pores or cracks cause the mechanical property values of plasma spray coatings to be considerably lower than those of the corresponding bulk materials [2-4]. Adhesion bond strength primarily determines the quality of a coating while the cohesion bond strength indicates coating lifetime. Yttria or/and Ceria Stabilized Zirconia coatings which are used for production of the thermal barrier coatings (TBC) have been widely developed due to their low thermal conductivity, relative high coefficient of thermal expansion and high durability. The long term performance of thermal barrier coated components such as gas turbine blades, vanes, combustion chambers, heat sinks can be affected by the adhesion coatings to superalloy substrate [5-9]. In this study spray parameters and substrate factors effect on bond strength of coatings were investigated by ASTM C633 test standard. 2. EXPERIMENTAL

The ceramic top coats used were ZrO28wt.%Y2O3 (204NS Sulzer Metco) and ZrO22.5wt.% Y2O3 -25wt.% CeO2 (205NS Sulzer Metco). A deposition of all coatings was done by atmospheric plasma spraying (APS) process. Coatings were deposited with a Sulzer Metco F4 MB plasma spray gun, Before the spraying process, the surface of the substrate was activated and preheated. Surface roughening was done with an

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appropriate abrasive (Al2O3). The target coating thickness for all specimens was 250750 m (100-250 m bond coat thickness). The selected spray parameters are given in Table 1. Table 1 Spray Parameters
Plasma Current 550-600A Ar/H2 gas flow rates nlpm Ar: 40-44, H2: 8-12 Feed Rate gr/ min. 35-45 Spray Distances mm 120-180 TC Thickness m 200-1050 BC Thickness m 100-250 Total Thickness m 300-1300

Cross-sectional Vickers microhardness measurements were performed on polished samples at 300gr. Both microhardness and roughness values quoted are an average of 18 measurements for each coating.The most commonly applied standard tensile test method for adhesion or cohesion strength of thermal spray coatings (ASTM C 633). ASTM Standard C633-79, is widely used in industry and research for evaluating bond strengths of thermal spray coatings. Tests are conducted by applying the coating to the end of a cylindrical test specimen 25.4 mm (1 in.) in diameter by 25.4 mm (1 in.) long. The coating surface is bonded to an uncoated cylinder of the same material and geometry. The force required to pull the cylinders apart is recorded. The bond strength is calculated by dividing the maximum force by the area of the 1 -in. diameter cylinder assuming that the stress is uniform over the area where the debonding occurs[10]. A constant cross head displacement rate of 0.32 cm thick disk that was bond coated on all surfaces 0.101 cm/min (0.040 in/min) was employed. The adhesive used in the adhesion test was the FM1000 cured for 1,5 h at 185 C and 30N of pressure. 3. 3.1. RESULTS AND DISCUSSION Microstructure

All coatings show a typical lamellar microstructure containing solidified splats, inter-splat imperfections, crack network and macro/ micro porosity. Fig 2. shows pores morphology, unmelted particles and splat boundaries in the coatings. The higher magnification of SEM micrograph (Fig2.) shows inter-splat boundaries/cracks. Such splat flaws are present in the all of the air plasma-sprayed coatings and they may have up to 0.1 mm length. The microstructure of plasma-sprayed coatings may be altered with change powder feed rate/ spray distance, plasma power. It can be explained by changes in total porosity, shape/size of the inter-splat pores and unmelted particles. The total porosity of coatings decreases as powder feed rate and plasma power increases. Higher plasma energy improves the melting ratio of powders. With the increase of intersplat contact areas leads the less porosity. Unmelted particle ratio affect the porosity. When the powder feed rate is high more unmelted particles may be preserved. This means that some of the powder particles either have not melted completely or have melted and cooled before impact. Such particles do not flatten as splat and therefore possess a very small area of intimate contact with other particles, so large pores can be created between them. The velocity and temperature of particles are dependent on spray distance and arc current. Powder is melted in high temperature plasma flame and accelerated toward the substrate, where it rapidly solidifies. The spray distance determines the velocity of melted powder when it impacts to the substrate. At low spray distance, many micro/ macro-cracks are found in the coating.

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Cross Section Micrographs YSZ Optical microscophy, OM CSZ

Scanning electron Microscophy SEM

Macro porosity Micro porosity Micro cracks

Fig. 2 Cross section and microstructure of the coatings 3.2. Bond Strength

The mechanical properties of plasma-sprayed coatings, such as adhesion to substrate, can be affected by the process parameters. Adherence of the coatings is determined by the volume fraction of porosity and unmelted regions. It may be concluded that the improvement in the adhesive properties of the coatings can mainly be achieved by decreasing the volume fraction of porosity and reducing unmelted areas. Bond strength results and surfaces of the pull out test samples at Fig 3. The residual stress is believed to be an important effective factor on the adhesion properties of coatings. The residual stress may be affected by substrate temperature, coating thickness and process parameters. The coatings with lower thickness show higher adhesion due to lesser internal stress. When YSZ and CSZ based coatings were compared, Bond strength of CSZ higher than YSZ and also were achieved higher thicknesses due to the lower internal stresses (Fig.4). Generally bond strength values were changed between 10MPa and 38MPa. Higher coating thickness (>500m) showed low adhesion. Highest strength of adhesion obtained with 400m thickness. Higher than 750 m thickness of the coating exhibited lowest bonding.

Fig. 3 Bond strength results and surfaces of the pull out test samples

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Fig. 4 Bond strength of stabilized ZrO2 based coatings deposited at different thicknesses. Experimental results obtained from tensile tests. In Fig.5 shows that the different spray parameters effect on bond strength of the coatings. Ar/H2 ratio and plasma current influenced the particle melting ratio and acceleration. However the optimum gas flow rate and plasma current have to be determined. Ar/H2 ratio: 44/10 gas flow ratio showed highest bond strength at 600A plasma current spray conditions. When the hydrogene gas flow rate increased particle temperature increased and then hot particles crashed the cold substrate surface with highly scattered. This leads to the high porosity levels of the coatings and decreases the bond strength.

Fig. 5 Bond strength of stabilized YSZ based coatings deposited at different spray parameters (Variables: plasma current, Ar/H2 gas flow rates, constant: 120mm spray distance, 35 gr/ min. feed rate). When the spray distance and feed rate were changed, bond strength were siginificantly influenced (Fig 6.). Lower feed rate as 35 gr/ min at 150mm spray distance for 600A showed high bond strength. However at higher spray distances adhesion properties is not clarified. But we can say that the higher melting ratio and acceleration of the particles improved the bonding. With the higher spray distances occurs better melting ratio. Spray distance effect is higher than the plasma current on bond strength.Because it control the porosity of the coating and intersplat adhesion.

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Fig. 6 Bond strength of stabilized YSZ based coatings deposited at different spray distances and feed rates. (Variables: spray distance, feed rate). In Fig.7. shows the surface roughness and substrate temperature effect on bond strength. These results imply that the adhesive strength between the coating and the substrate roughened by grit blasting was partly due to the anchor effect caused by surface roughness. The bond strength of the sprayed coating was affected by the surface roughness of the substrate. Higher roughness have negative effect on bond strength. However substrate temperature have improved the bond strength.

Fig. 7 Surface roughness and substrate temperature effect on bond strength

4.

CONCLUSION

In conclusion, the sprayed coatings would bond to the substrate by a combination of mechanical anchoring and metallurgical bonding. Table 2. summarizes the effective factors for bond strength/ adhesion test results. It was observed that the plasma gas flow rates, plasma current , powder feed rate and spray distance are important effective parameters on the microstructure as well as adhesion behavior of the coatings. Microstructure analysis showed that powder feed rate and spray distance have great effect on the pores morphology. Coating failures are mainly located in the bond coat/substrate interface at highest adhesion strength. Highest bond strength was obtained with optimum parameters: 44/10 gas flow ratio at 150mm for 600A and 35gr/min feed rate.The Ra 4.8 m surface roughness show the highest adhesion values at 300 C.

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Table 2 Summary of Effective Factors for Bond Strength/ Adhesion Test Results
Factors As Sprayed Primer and seconder gas flow rates Plasma current, Plasma power Spray distance Powder Feed rate Roughness Temperature Chemical composition The coefficient of thermal expansion Thickness Surface rougness Oxide content Chemical composition Thickness, pass number, pass thickness Porosity ratio Unmelted particle ratio Macro/micro cracks Vertical or horizontal cracks Chemical composition Glue type Curing time Curing temperature Test condition- pull out rate

Process

Substrate

Bond coat

Top coat

Glue

LITERATURE
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