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Surface & Coatings Technology 201 (2007) 4653 – 4658 www.elsevier.com/locate/surfcoat

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Metallurgy Division, GPO Box No. 502, Rawalpinidi, Pakistan LASMIS, BP 2060, 12 Rue de Marie Curie, Université de Technologie de Troyes, 10000 Troyes, France Received 27 May 2006; accepted in revised form 2 October 2006 Available online 28 November 2006

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Abstract

Keywords: Air Plasma Spraying; Thermal barrier coatings; Thermal shock test; Residual stresses

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Thermal barrier coatings (TBCs) were deposited by an Air Plasma Spraying (APS) technique. The coating comprised of 93 wt.% ZrO2 and 7 wt.% Y2O3 (YSZ); CoNiCrAlY bond coat; and AISI 316L stainless steels substrate. Thermal cyclic lives of the TBC were determined as a function of bond coat surface roughness, thickness of the coating and the final deposition temperature. Two types of thermal shock tests were performed over the specimens, firstly holding of specimens at 1020 °C for 5 min and then water quenching. The other test consisted of holding of specimens at the same temperature for 4 min and then forced air quenching. In both of the cases the samples were directly pushed into the furnace at 1020 °C. It was observed that the final deposition temperature has great impact over the thermal shock life. The results were more prominent in forced air quenching tests, where the lives of the TBCs were observed more than 500 cycles (at 10% spalling). It was noticed that with increase of TBC's thickness the thermal shock life of the specimens significantly decreased. Further, the bond coat surface roughness varied by employing intermediate grit blasting just after the bond coat spray. It was observed that with decrease in bond coat roughness, the thermal shock life decreased slightly. The results are discussed in terms of residual stresses, determined by hole drill method. © 2006 Elsevier B.V. All rights reserved.

1. Introduction

Thermal barrier coatings (TBCs) can be considered as a three layer material system, consisting of (1) a substrate, (2) an oxidation-resistant metallic bond coat, usually MCrAlY or a platinum aluminide coating, and (3) the ceramic top coating, usually 6 to 8 wt.% yttria-stabilized zirconia deposited either by plasma spray or electron beam physical vapor deposition process. The zirconia topcoat has excellent thermal shock resistance, low thermal conductivity and relatively high coefficient of thermal expansion (CTE) [1]. The MCrAlY bond coats provide a rough surface for mechanical bonding of the ceramic top coat, protect the underlying alloy substrate against the high temperature oxidation corrosion, and reduce the CTE mismatch between the substrate and ceramic top coat materials [2].
⁎ Corresponding author. E-mail address: nusairy@yahoo.com (A.N. Khan). 0257-8972/$ - see front matter © 2006 Elsevier B.V. All rights reserved. doi:10.1016/j.surfcoat.2006.10.022

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Thermal barrier coatings, however, have a tendency to spall, or debond, under cyclic high temperature conditions. It is believed that spallation of the ceramic component in TBC's is a result of the stresses generated in service [3]. The performance of TBC's is also affected by thermal expansion mismatch between the ceramic and the metal, thermal stresses generated by the temperature gradients in the TBC, ceramic sintering, phase transformation, corrosive and erosive attack, and the residual stresses arising from the deposition process. Thermal barrier coatings offer the potential of increasing turbine operating temperature up to 150 °C, which permits a reduction in the mass of cooling air required while maintaining the turbine operating temperature giving improved specific fuel consumption [4,5]. Increasing the thickness of the coating can increase the temperature resistance property. However, the thickness of the coating is limited by mechanical and thermal stresses and the thermal cyclic life of the coating. Moreover, increased resistance of plasma sprayed coatings to cyclic thermal exposure can be achieved by increasing the strain

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A. Nusair Khan a,⁎, J. Lu b

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Thermal cyclic behavior of air plasma sprayed thermal barrier coatings sprayed on stainless steel substrates

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2.1. Materials

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The thermal barrier coatings, composed of a bond coat and a top coating, were air plasma sprayed onto a stainless steel AISI 316L samples. The powder used for the bond coating was CoNiCrAlY (AMDRY® 995(4)), had spherical free flowing gas atomized powder with grain size, 20 ± 10 μm. The top coating material (NORTON HW 1193) was consisted of spherical particles with grain size 25 ± 15 μm, and the powder was porous in nature with chemical composition 93ZrO2–7Y2O3, wt.%. 2.2. Deposition process

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Circular substrates with a diameter of 25 mm and a thickness of 10 mm were grit blasted on the flat surface to be coated. Just after the grit blasting the samples were subjected to Air Plasma Spraying. Fig. 1 shows the schematic view of the experimental arrangement. A DC, PT-2000 Plasma Tenhnik AG Switzerland, gun was utilized for the deposition of both the bond and top

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Fig. 1. Schematic view of the experimental arrangement.

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2. Experimental

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tolerance of the ceramic and by controlling harmful residual stresses. These residual stresses can be controlled by the substrate roughness [6], and final deposition temperature. Residual stresses, originate from the large temperature differences, and are divided into two main groups: quenching and thermal stresses [7]. Quenching stresses develop while the semi-molten particles strike to the relative colder substrate surface where the temperature drops drastically. Consequently, these semi-molten particles try to contract over the underlying metal, where the substrate restricts them as a result tensile stresses develops within the coating material. The thermal stresses generate while the whole system, i.e. deposit and substrate cool down to room temperature. A thermal mismatch stress develops due to the difference in thermal expansions of each material. Since these stresses are associated with temperature differences thus by controlling the temperature history one can control the residual stresses. The deposition temperature can be controlled by varying the substrate to torch distance, gas cooling during spraying, and pre-heat treatment of the substrates. In our study we controlled the residual stress profile by changing the torch distance vs substrate. In this paper we will study the effects of bond coat surface roughness, coating thickness effects and the final deposition temperature over the thermal cyclic life of TBC.

2.3. Thermal shock test

Two different types of thermal shock tests were performed. In both cases the samples were heated in the muffle furnace. When the temperature of the furnace reached up to 1020 °C, the samples were pushed into the furnace. In water quenching thermal shock tests, the samples were held about 300 s into the furnace and then directly quenched into the water. The temperature of the water throughout the cycling was between 20 and 35 °C. whereas, in compressed air quenching test the samples were held about 240 s into the furnace at 1020 °C and then quenched by compressed air. The cooling time for air quenching was about 90 s. After 90 s, the samples were on room temperature. More than 50% of the spalled region of the surface of the top coating was adopted as criteria for the failure of the coating in both water and air quenched samples. At least three samples were tested for each condition. This type of thermal shock testing was also performed by other investigators [8–11]. 2.4. Residual stress and Roughness measurements The residual stresses were measured by hole drill method. In this method a blind hole is brought step by step into the surface of the component. The residual stresses are relieved by material removal (blind hole), deform the surface around the hole and are measured as relaxed strains at the surface by means of strain gauges. Together with calibration curves, Young's Modulus and Poisson's ratio the measured relaxed strains at the surface are transformed into true strains at the bottom of the drilled hole. Out of the strains at the bottom, plane stresses are incrementally determined by Hook's law [12]. The Young's Modulus and Poisson's ratio were taken from the published literature i.e. 30 GPa and 0.2 respectively [13]. The roughness was measured by Taylor Hobson roughness meter. For this purpose Ra values were considered. 3. Results and discussion The observations and possible discussion during the water and forced air quenching for different parameter are presented below.

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coating. The plasma gun moved up and down in the vertical direction, in each passage depositing a thin layer of molten material on the rotating substrates. The bond coating was sprayed to a total thickness of 45 ± 10 μm whereas 300 to 500 μm thick top coatings were produced by the same technique. During the spraying of both bond and top coatings the substrate temperature was controlled by air jets. Pressurized air jets were blown from two directions, one directed parallel to the plasma torch, and the other behind the rotating fixture of substrates. The spraying distance between the torch and the substrates was 125 mm. The temperature measurements were made by an optical pyrometer, fixed close to the rotating assembly of the samples.

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A.N. Khan, J. Lu / Surface & Coatings Technology 201 (2007) 4653–4658 Table 1 Number of sustained cycles with top coating thickness Sample No. Top coat thickness, μm 300 400 500 Number of sustained cycles, water quenched 40 to 44 15 to 18 3 to 4 Number of sustained cycles, force air quenched 171 29 13 Final deposition temperature, °C 55 70 70

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3.1. Top coat thickness Three different topcoats with the same thickness of bond coats were produced by the same deposition parameters. The thickness of topcoat, number of sustained thermal cycles and the final deposition temperature for the coatings are given in Table 1. On comparing sample No. 3 and sample No. 1, in Table 1, where the top coatings are 500 and 300 μm in thickness, respectively, the number of sustained cycles for sample No. 3 are only 3 to 4 for water quenching and about 13 for forced air quenching. For sample No. 1 these number of cycles in water quenching tests are 40 to 44 and for force air quenching, these are about 171 cycles. In all the samples (water quenched and forced air quenched) the spalling mode was same i.e. all spalled completely at the interface of bond and topcoat, Fig. 2(b). Similarly, in case of sample No. 2 (Table 1), where the thickness of the top coat was 400 μm the trend was similar i.e. with increase of coating thickness the number of sustained cycles were decreased to 15–18 cycles in water quenching and to 29 in forced air quenching. The delamination mode remained the same as in the other two samples. The whole picture is summarized in Fig. 3. These results are consistent with those of the other investigators [14]. P.G. Tsantrizs et al. [14] suggest that partially stabilized zirconia layers thicker than 300 μm are more susceptible to cracking and delamination. The possible explanation might be the large temperature differences, at quenching and heating times, between the substrate and surface of the topcoat. In case of thick TBCs, this temperature difference increased and as a result more thermal stresses developed at the interface of the bond and topcoats. The miss-match in coefficient of thermal expansion

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Sample No.

Fig. 3. Number of sustained cycles with top coat thickness for water and air quenched samples.

(CTE) between the ceramic and the bond coat or oxidation of bond coat (in case of sample No. 1 and 2) leads to failure. The other possible explanation might be that for thicker coatings there is more stored elastic strain energy than for thin coatings, which is the driving force for debonding. 3.2. Topcoat deposition temperature

Two sets of samples were prepared to observe the effect of deposition temperature. The final deposition temperature, topcoat thickness and number of sustained cycles for both water quenched and forced air quenched samples are in Table 2. The final deposition temperature was controlled by external cooling, shown in Fig. 1 and by changing the spraying distance between the torch and the substrate. It was observed that the final deposition temperature played an important role on the course of spalling. The samples having more deposition temperature showed more resistance towards the spalling as compared to those with low final deposition temperature. On comparing sample No. 1 and sample No. 2 in Table 2 it is noted that even the thickness of the top coat in the case of sample No. 2 is 50 μm more even then it sustained more number of cycles as compared to sample No. 1. The spalling mode for sample No. 2 was gradual and started from the extreme edges in
Table 2 Number of sustained cycles with top coat deposition temperature Final deposition temperature, °C 70 350 Top coat thickness, μm 320 ± 10 377 ± 15 Number of sustained cycles, water quenched 35 90 Number of sustained cycles, air quenched 113 N500

Fig. 2. (a) After 90 cycles, still coating ∼ 40% coating attached with substrate; (b) after 3 cycles, complete delamination of top coat.

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rquench ¼ ac d Ec ðTexit −Tdep: Þ

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171 113

of intrinsic residual stresses within the as-deposited TBC is the thermal residual stresses of plasma-sprayed zirconia coating which arises from the nature of the plasma-spraying process associated with the rapid cooling of molten droplets, impacting on the cold substrate. The deposition temperature of the coating can control these stresses. The arising stresses while solidification and quenching can be approximately estimated with Eq. (1) [15]: ð1Þ

Fig. 4. Number of sustained cycles for different final deposition temperature, for air and water quenching.

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both water and forced air quenched samples. In water quenched samples, the spalling was up to ∼ 50% in 90 cycles and for water quenched samples ∼ 10% spalled in 500 cycles, we stopped cycling after 500 cycles. The results are summarized in Fig. 4. Further, on comparing the thickness of sample No. 2 (in Table 2) with sample No. 2 (in Table 1) is almost same but the number of sustained cycles for high deposition temperature (sample No. 2, Table 2) are much more than that with low deposition temperature for both water and forced air quenching. Residual stresses are believed to affect the TBC integrity in high temperature applications. Qain et al. [15] showed in his experiments that the thermal fatigue lifetime of some TBCs is directly related to the magnitude of the residual stresses. The residual stresses in the case of sample No. 2 (Table 2, Fig. 5) were found to be more compressive in bond coat (up to 160 MPa) as compared to sample No. 1. These compressive inplane stresses can cause cracking parallel to, or at, the coating substrate interface, leading to spalling or delamination failures [16]. Residual stresses within the coating system are generated by both the coating deposition process and service. One source

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where, Ec and αc are the Young's modulus and CTE (coefficient of thermal expansion) of the coating and Texit and Tdep are the temperatures of the splat at the exit of the torch and at the deposition respectively. Further, the high thermo-mechanical stability of plasma sprayed zirconia topcoats is associated with its low macroscopic stiffness [17] so that the residual stress level remains low and the material has high strain tolerance. This apparently, arises due to the presence of microcracks, pores and lack of splat bonding. Although it is expected to rise in stiffness values under compressive stresses large enough to cause closure of microcracks etc. Thus the rise in compressive stresses, in sample No. 1, and the associated strain energy release rate also increase, making spallation more likely. It was observed that in sample No. 1 the topcoat was totally delaminated, Fig. 2 (a), from the substrate whereas in sample No. 2, the topcoat remained in contact to substrate even after 90 cycles, Fig. 2(b). Thus the deposition temperature plays an important role over the thermal cyclic life of the TBCs; according to T. Haublod et al. [18] the main influence working on the thermal cycling life during spraying is temperature. 3.3. Effect of bond coat roughness Recently researchers have begun to emphasize the influence of bond coat surface roughness on TBC performance. Y.C. Tsui and E.Y. Lee et al. [19,20] suggested that bond coat surface roughness affects the thermal fatigue life of TBC's. A. Frebory et al. [21] also analyzed the effects of bond coat surface roughness on TBC stress and life time. Hence, some samples were prepared for this purpose. The as-sprayed samples surface roughness was measured and was about 7.2 ± 2 μm. The bond coat surface roughness was altered by intermediate grit blasting immediately after spraying the bond coat and the surface roughness decreased to 4.0 ± 0.5 μm. The surface roughness of the bond-coat, number of sustained thermal cycles, and the thickness of the coating are given in Table 3. During water quench tests the effect of bond coat surface roughness was not

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Ra, μm

Table 3 Number of sustained cycles with bond coat surface roughness Number of sustained cycles, water quenched 40 35 Number of sustained cycles, air quenched Top coat thickness, μm 320 320

Fig. 5. Residual stress variation with depth for two samples, No. 1 and 2. Final deposition temperature for sample No. 1 and sample No. 2 is 70 °C and 350 °C respectively.

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7.2 ± 1.5 4.0 ± 1.0

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Fig. 8. Stainless steel based TBC spalled after sustaining 53 cycles with schematic showing hanging TBC.

Fig. 6. Residual stresses profile with different bond coat surface roughness.

3.4. Long thermal cycling

Fig. 7. Influence of bondcoat surface roughness on number of sustained cycles.

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The coatings that sustained the maximum number of cycles were also tested for long thermal cycle. This cycle is comprised of heating at 1100 °C for 50 min and then still air-cooling for 10 min. It was observed that in the early stages of cycling the bare surface of the substrate starts to oxidize. And after a few

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prominent while it became significant during forced air quenching, i.e. up to 60 cycles difference. Residual stresses for both samples were determined by hole drill method and profile as shown in Fig. 6. These stresses were about 140 MPa and 160 MPa in sample No. 1 and sample No. 2 respectively. It seems that due to more stresses in sample No. 2, it spalled earlier than sample No. 1, this difference is especially clear in forced air quenched samples, as shown in Fig. 7.

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4. Conclusions The final deposition temperature strongly affects the TBCs thermal shock life; the probable reason was the relaxation of residual stresses. The life of TBC deposited at 70 °C was only 113 cycles for (50% spalling) whereas for 350 °C the life increased to more than 500 cycles (for only 10% spalling) in forced air quenching tests. It was observed that thick coatings were more prone to thermal cyclic failures as compare to thin coatings. The top coatings, which were 500 μm in thickness, were spalled just after 13 cycles in forced air quenching tests whereas those having 300 μm thickness sustained up to 171 cycles. Further, by increasing the deposition temperature the coating thickness may be increased, as what was observed in the high deposition temperature's case, where the samples having ∼ 400 μm thick TBCs spalled only 10% after 500 cycles as compared to only 29 cycles with 50% spalling (in case of forced air quenching). The effect of bond coat surface roughness was more prominent in the case of forced air quenched samples.

Fig. 9. Weight loss during the cycling of stainless steel based TBC system.

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cycles it was observed that the TBC at the edges was hanged freely, Fig. 8 and then spalled in the next few cycles. The average cycles sustained by these coatings were up to 53 cycles. The weight loss during the thermal cycling is shown in Fig. 9. This demonstrates the excellent thermal cycling properties of the TBC on stainless steel substrates.

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A.N. Khan, J. Lu / Surface & Coatings Technology 201 (2007) 4653–4658 [12] K. Berreth, M. Buchmann, R. Gadow, J. Tabellion, United thermal spray conference, Dusseldort, 17 bis 19 Marz (1999), ASM Thermal spray society, 1999, p. 670. [13] Per Bengtsson, Mirostrural Studies and Residual Stress Evolution in Zirconia-Based thermal barrier coatings, Thesis No. 524; Linköping University, Sweden, 1995. [14] P.G. Tsantrizs, G.E. Kim, T.A. Braezinski TBCs on free standing multilayer components; AGARD meeting on thermal barrier coatings, Aalberg, Denmark, 15–16 Oct. 1997, 7-1 to 7-8. [15] G. Qain, T. Nakamura, C.C. Berndt, Mech. Mater. 27 (1998) 91. [16] S. Kuroda, T.W. Clyne, Thin solid films 200 (1991) 49. [17] J.A. Thompson, T.W. Clyne, Acta Mater. 49 (2001) 1565. [18] T. Haublod, H. Gans, D. Schwingle, R. Taylor, AGARD SMP meeting on thermal barrier coatings, Aalberg, Denmark, Oct 15–16 1997, p. 5. [19] Y.C. Tsui, T.W. Clyne, Proc. 9th National Thermal Spray Conference, (NTSC 96), ASM International, Cincinnati, OH. USA, Oct. 7–11 1996, p. 275. [20] E.Y. Lee, et al., Proc. 7th National Thermal Spray Conference, (NTSC 94), ASM Internatinal, Bost, MA, June 20–24 1994, p. 55. [21] A. Frebory, et al., Proc.1997 TBC Workshop, Cincinnati, OH. USA, May 19–21 1997, p. 53.

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