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Degradation of TiAlN coatings by the accelerated life test using pulsed laser ablation
Seol Jeona, Chester J. Van Tyneb, Heesoo Leea,n
b a Department of Materials Science and Engineering, Pusan National University, Busan 609-735, Korea Department of Metallurgical and Materials Engineering, Colorado School of Mines, Golden, CO 80401, USA

Received 27 November 2013; received in revised form 16 January 2014; accepted 16 January 2014

Abstract The degradation behaviors of TiAlN coatings were evaluated by an accelerated life test under thermo-mechanical loading using a Nd:YAG pulsed laser ablation system. Pulse laser levels were chosen based on nite element analysis, and failure was determined when the specimen hardness decreased below 50% from its initial value. The accelerated life test was conducted on both TiAlN and TiN coatings deposited on an Inconel 617 substrate. The predicted lifetimes were obtained through statistical analysis of the failure time data. Surface and cross-sectional microstructural observations of the ablated spots were made to identify the cause for the difference in lifetimes since the TiAlN coating lasted longer than the TiN coatings by a factor of  1.7. Pores formed on the TiAlN coating surface by the repeated laser ablation, and surface cracking and delamination of the coating layers were observed on the ablated spots in the failed specimens. The TiN coating also showed surface cracks with fewer surface pores than the TiAlN coating, but spalling of the coating layer occurred due to bursting of the substrate. Secondary ion mass spectrometry (SIMS) depth proling revealed that surface oxidation increased in the TiN coating as the number of laser pulses increased, while the TiAlN coating showed less surface oxidation. The surface oxidation and spalling of the coating layer is considered to be the dominant inuence on the decrease in hardness of the TiN coating. The TiAlN coating retains its hardness longer due to its lower thermal conductivity and higher oxidation resistance, as compared to the TiN coating. & 2014 Elsevier Ltd All rights reserved.
Keywords: C. Lifetime; C. Thermal shock resistance; E. Cutting tools

1. Introduction Titanium nitride (TiN) coatings have become increasingly important for use in cutting tools, forming dies, and many other mechanical parts, because of the increase in lifetime and performance due to several benecial properties, such as high hardness, good wear, and chemical stability [13]. Recently, titanium aluminum nitride (TiAlN) coatings have been developed into another excellent candidate for hard coating applications, because they show excellent durability, especially at high temperatures [46]. In production use of cutting tools, thermo-mechanical loads are repeatedly applied to the coatingsubstrate system. These loads can result in cracking, delamination, or spalling of the protective layer, which limits the lifetime of the tools [7,8]. As a result, it is crucial to understand the
n

Corresponding author. Tel.: 82 51 510 2388; fax: 82 51 510 0528. E-mail address: heesoo@pusan.ac.kr (H. Lee).

degradation behavior of coatings under thermo-mechanical conditions that are close to actual production conditions, so a reliable evaluation of the hard coating material can be made. Accelerated test, which can cause failure and deterioration, is often used as a method for reliability assessment because of time restrictions and cost aspects. The results of an accelerated test can provide a lifetime prediction through the use of an adequate statistical analysis of the shortened times to failure [9]. Thermal shock test using laser ablation can apply local thermo-mechanical loads during a short period of time. Hence, the laser thermal shock test is a close simulation of the industrial conditions of a cutting tool, whereas conventional furnace heating is further removed from the actual working environment of hard coatings. Furnace heating causes the entire area of the coating to be thermally loaded, as well as overexposing the specimen to heat [10,11]. Several investigations have been conducted on the degradation of nitride hard coatings by thermal loading in order to identify their fracture

0272-8842/$ - see front matter & 2014 Elsevier Ltd All rights reserved. http://dx.doi.org/10.1016/j.ceramint.2014.01.085 Please cite this article as: S. Jeon, et al., Degradation of TiAlN coatings by the accelerated life test using pulsed laser ablation, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.01.085

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and oxidation behavior at high temperatures [1215]. Deformation modes and mechanisms of hard coatings during mechanical loading have also been studied to observe the degradation of coating-substrate systems by normal loads and shear loads from indentation [1619]. However, the degradation behavior of hard coatings with the application of thermomechanical loads has not been investigated. Finite element analysis (FEA) has become a useful tool for studying the changes in coating specimens tested with thermal and mechanical loads. FEA is an alternative to experimental methods to determine temperature and pressure distributions in the specimen, since it is difcult to accurately measure the temperature and load in the cutting zone [2022]. FEA can also be used to determine the expected stress and temperature distributions in ablated spots during laser ablation [2325]. In the current study, an accelerated testing using a Nd:YAG pulsed laser ablation system was designed based on FEA results and was conducted on TiAlN and TiN coated specimens. Statistical analysis of the failure time data was performed in conjunction with morphological observation of the failed specimens. Focused ion beam milling and depth proling by secondary ion mass spectrometry (SIMS) were also conducted to identify the degradation behavior of these coatings.

2. Experimental procedures The TiAlN and TiN coatings were deposited on Inconel 617 substrates (25 30 10 mm3) with the coating thickness of  2.0 m by an arc discharge technique. Table 1 shows detailed deposition conditions. FEA using ABAQUS/CAE
Table 1 Deposition conditions for the TiAlN and TiN coated specimens. Coating material Base pressure (Torr) Working pressure (Torr) Arc material (at%) Arc current (A) Sputter current (A) Deposition temperature (K) Deposition time (min) Rotational velocity of substrate (rpm) N2 gas ratio TiAlN 1.0 10 5 3.0 10 3 Ti (99.99), Al (99.99) 50 1.0 823 25 25 0.25 TiN 1.0 10 5 3.0 10 3 Ti (99.99) 50 1.0 723 20 25 0.3

simulated the pulsed laser ablation as a uniform heat ux to the coated specimen based on laser energy ux (W/cm2). For the simulations, the coating specimens were quarter cylinders and matched the size of the experimental specimens [26,27]. The maximum temperature and principal stress were calculated during the short ablation times (5 ns). Table 2 shows the properties of the coating specimens used in the FEA model [2835]. The 1st order 8-noded thermally coupled brick element (tri-linear displacement and temperature system, C3D8T) was used in the modeling, and total nodes were 26,578 (total elements: 23,564, thermal gap conductance: 50,000 W/m K for 0.1 mm). Contact property of the coating and the substrate was chosen by cohesive behavior, and geometric boundaries were riveted as the X and Y axes with zero in displacement for each other. A high power Nd:YAG laser ablation system (LSX-213, CETAC Technologies) was used for the laser thermal shock testing of the coating specimens. The laser was operated in the Q-switched mode at a basic wavelength of 213 nm, The laser uency was  13 J/cm2 for the 200 m spot at 100% energy output and the laser irradiance was  2 GW/cm2 with a pulse width of o 6 ns [10,11]. The number of laser ablation pulses was increased in 1 Hz frequency. The specimens were repeatedly ablated with an ablation diameter of 200 m with 10%, 20%, and 30% energy output, at acceleration levels determined by the FEA method, and with the number of laser pulses varying from 1 up to 50. The ablation interval was held constant at 1 s. Fig. 1 shows a schematic of the laser ablation system and its energy output. A decrease in hardness of the ablated spots to below 50% of the initial value was chosen as the failure criterion. Hardness of the ablated spots was measured using a Knoop microhardness tester (MMT-7, Matsuzawa) under a load of 50 gf. The hardness value of each ablated spot was calculated by taking the average of 10 measurements. Statistical analysis of the accelerated life testing was done with the MINITAB statistical software, assuming a Weibull distribution for the failure time. The acceleration model was based on the generalized Erying model for prediction of life cycles of the coating specimens under two accelerating factors: temperature (Arrhenius model) and stress (Inverse Power model). The surface morphologies of the ablated spots were investigated by scanning electron microscopy (S-4800, Hitachi). Cross-sections of the coating-substrate system were prepared and imaged using a dual-focused ion beam (Nova 200

Table 2 Material properties used in the FEA simulation of the coated specimens. Material Dimension (m2) Density (g/cm3) Elastic modulus (GPa) Specic heat (J/kg-K) Linear thermal expansion coefcient (1/K) Thermal conductivity (W/m-K) Poission's ratio TiAlN (500 500) 2 4.70 380 779 7.5 10 6 4.63 0.23 TiN (500 500) 2 5.22 251 601.71 9.35 10 6 19.2 0.25 Inconel 617 (500 500) 500 8.36 211 419 11.6 10 6 13.4 0.30

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Fig. 1. LSX-213 pulsed laser ablation system: (a) schematic of operating process and (b) linear output of laser energy.

NanoLab, FEI). To identify atomic changes in the ablated spots, secondary ion mass spectrometry analysis was conducted (Adept1010 Dynamic SIMS System, Physical Electronics) with a 30 nA Cs beam at 3 kV. The primary ions were rastered within a square of 150 150 m2 and the secondary ions were collected from the central 10% of the rastered region in an area of about 47 47 m2. 3. Results and discussion Fig. 2 shows the results of the FEA simulation of the laser ablation for the coated specimens with a uniform heat ux. At 100% energy level for the laser, the maximum temperature and principal stress of the specimens were about  14000 K and 7000 MPa, respectively. Both the TiAlN and TiN coated specimens had similar results when a high pulsed energy was applied to the coated surface during a short ablation time (5 ns). Table 3 gives the maximum temperature and principal stress at each energy level, based on the linear relationship between the laser output and energy. The acceleration levels

were chosen as 10%, 20%, and 30% levels for the accelerated testing because the loads, which were generated at 10%, are close to the actual conditions of cutting tools [21,36,37]. A ratio of 1:2:4 is a good rule of thumb for the number of samples at the high, mid, and low loads, according to the MeekerHahn theory [38], so that the number of samples tested are 3:6:12 at each acceleration level, respectively. Fig. 3 shows an example of the decreasing hardness of the ablated spots. The hardness decreases as the number of laser pulses increases for both coatings. The decrease in the hardness was  1000 HK after seven pulses for the TiN coating. It is expected that the coating layer would be dramatically deteriorated after seven pulses so that the hardness is inuenced by the substrate material during the hardness measurement [39]. The number of laser pulses indicated with black arrows is selected as the failure time, since the failure criterion is met. Based on the generalized Erying model, the factors of temperature and principal stress were designated as an Arrhenius model and inverse-power relationship model, respectively. Fig. 4

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Fig. 2. Simulation of the pulsed laser ablation of the coated specimen: (a) assembled model of the coated specimen, (b) model of the laser ablation as a uniform heat ux to the coating surface and (c) change in temperature during laser ablation.

Table 3 Maximum temperature and principal stress at the coating surface. Laser energy level (%) Max. temperature (K) TiAlN 10 20 30 40 50 60 70 80 90 100 1458 2665 3954 5287 6475 7863 9114 10368 11568 13888 TiN 1507 2741 3976 5374 6554 7980 9214 10448 11627 14025 Max. principal stress (MPa) TiAlN 662 1248 1899 2649 3294 4104 4765 5265 6084 7030 TiN 665 1329 1994 2747 3382 4150 4814 5479 6114 7087

shows the Weibull probability plots and predicted lifetimes (cycles or pulses) of the coating based on the failure data from the accelerated life testing function in MINITAB 6.10. Table 4 shows the predicted Weibull characteristic time, which is a failure point for 63.2% of all specimens [40,41]. The predicted lifetimes of the TiAlN coating is higher than the TiN coating by a factor of  1.7 at all acceleration levels. To identify the reasons for the differences in the predicted lifetimes of the coatings, the degradation behavior of each specimen was investigated by observing the changes in morphology. Fig. 5 shows the surface of ablated spots in the coated specimens prior to the failure point. Fig. 5(a) shows that pores appear on the surface after ve pulses at all acceleration levels, while the size of the surface porosity is larger at the 30% level, as shown in Fig. 5(a)(c). For the TiN coatings,

Fig. 5(d) and (e) shows that cracks and pores form on the coating surface after ve pulses at 10% and 20% levels, and that the size of the surface cracks increases as the laser energy level is increased to 30% (shown in Fig. 5(f)) The dominant degradation behavior of the coating is pore formation in the TiAlN coating and surface cracking in the TiN coating. The degree of the surface degradation rapidly increases at the highacceleration level (i.e. at 30%). Fig. 6 shows the surface of ablated spots in failed specimens where the hardness decreased to less than 50% of their initial value. Surface cracking and delamination of the coating layer are seen as the failure mode in both coatings under all laser output. Because of the failure mode, these outputs are considered to be appropriate laser output levels for the accelerated testing [9]. Fig. 6(c) and (f) shows the increase

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in the size of the cracks and their coalescence after repeated laser ablation. Cross-sections of the ablated spots at the 20% laser energy level were observed in order to compare the degradation of the coating-substrate system with the increased number of laser pulses. Fig. 7(a) and (b) shows that the thickness of the TiAlN coatings decreased as the number of laser pulses increased. Cracks in the direction toward the substrate are not found, while some pores are observed near the coating surface. For the TiN coating, Fig. 7(d) and (e) shows that the coating thickness decreased, and the depth of cracks, which originated at the coating surface, increased as the laser pulses increased.

The decrease in hardness without the coalescence of surface cracks as seen in Fig. 6(c) and (f) is attributed to the decreasing coating thickness, due to the repeated laser ablation. In addition, the surface cracks in the TiAlN coating (Fig. 6(a) (c)) are expected, since these cracks are formed by a burst of the substrate (Fig. 7(c)). In contrast, the surface cracks in the TiN coating (Fig. 6(d) and (e)) seem primarily to be cracks initiated at the coating surface (Fig. 7(d) and (e)). The adhesion between the coating and the substrate is well maintained in the TiAlN coated specimens, as seen in Fig. 7(c). The substrate under the TiN coating melts and the coating layer spalls from the substrate due to melting of the substrate after 25 pulses, as seen in Fig. 7(f). The difference in the substrate burst phenomenon can be explained by the difference of thermal conductivity of the two coatings. The higher thermal conductivity of TiN compared to that of TiAlN causes heat (coming from the pulsed laser) to transfer into the substrate for TiN coating to a greater extent, as compared to the TiAlN coating, so that the higher thermal expansion of the substrate occurred in the TiN coating than in the TiAlN coating [42,43]. Hence, the substrate under TiN coating layer melts and bursts into the coating. In addition, it was expected that the higher hot
Table 4 Results of accelerated tests for the coated specimens. Acceleration level Scale parameter (Weibull characteristic time) in cycles 10% 20% 22.2 13.2 30% 16.6 9.9

Fig. 3. Example of hardness change of the coated specimens with laser pulses at 30% energy level.

TiAlN TiN

33.4 20.4

Fig. 4. Weibull probability plots of (a) TiAlN and (b) TiN coatings after accelerated life testing. Please cite this article as: S. Jeon, et al., Degradation of TiAlN coatings by the accelerated life test using pulsed laser ablation, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.01.085

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Fig. 5. Surface of ablated spots after 5 pulses at (a) 10%, (b) 20%, (c) 30% laser energy level in TiAlN coating, and at (d) 10%, (e) 20%, and (f) 30% laser energy level in TiN coating.

Fig. 6. Surface of ablated spots after (a) 33 pulses with 10%, (b) 21 pulses with 20%, (c) 15 pulses with 30% laser energy level in the TiAlN coating, (d) 23 pulses with 10%, (e) 13 pulses with 20%, and (f) 9 pulses with 30% laser energy level in the TiN coating.

hardness of TiAlN coating than that of TiN coating prevented the substrate bursts [44,45]. From these morphological observations, the resistance to crack propagation and spalling by the pulsed laser thermal shock is higher in the TiAlN coated specimen as compared to that in the TiN coated specimen. The TiAlN coating has better adhesion between the coating and the substrate. To understand the atomic changes in the ablated regions after laser thermal shock, the SIMS analysis was conducted on

the coated specimens. Fig. 8 shows that the coating layers were uniformly deposited on the substrates without variation for both types of coatings. The concentration of elements in the coating and the substrate reverse at a depth location. The location of this reversal indicates the interface region [46,47]. The interface moves closer to the surface with an increasing number of laser pulses. This decrease in depth indicates that the coating layer decreases in size due to the laser thermal shock, as previously observed in Fig. 7. The broadening of the

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Fig. 7. Cross-sections of ablated spots after (a) 5, (b) 25, and (c) 35 pulses in the TiAlN coating and after (d) 5, (e) 15, and (f) 25 pulses in the TiN coating at 20% laser energy level.

Fig. 8. SIMS depth proles of the ablated spots at 20% laser energy level: (a) as-deposited, (b) after 15, (c) 25 pulses in TiAlN coating, (d) as-deposited, (e) after 5, and (f) after 15 pulses in TiN coating.

interfacial regions mean that the thermal diffusion of the coatings and the substrate atoms occurred by the repeated laser ablation, and it increased as the number of laser pulses. Fig. 8(a) clearly shows the presence of oxides on the surface for the as-deposited TiAlN coating. These oxides indicate the presence of Al2O3 and TiO2 alumina in the TiAlN coating,

which formed during the deposition [6]. For the ablated spots in the TiN coating, the O-16 count rates increase from  101 to  1023 near the surface as the number of laser pulses increases, as seen in Fig. 8(d)(f). This increase in oxygen indicates that the coating surface oxidizes during the laser ablation [48,49]. The decrease in the TiAlN coating layer

Please cite this article as: S. Jeon, et al., Degradation of TiAlN coatings by the accelerated life test using pulsed laser ablation, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.01.085

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thickness is also shown in Fig. 8(b) and (c). Oxidation occurs during the laser ablation on the coating surface in the TiAlN coating, but the amount of oxidation is less than in the TiN coating because of the higher thermal oxidation resistance of TiAlN than TiN [5052]. The decrease in hardness shown in Fig. 3 after the pulsed laser ablation is attributed to the formation of surface cracks and surface oxidation. Considering all of the results, the TiAlN coating appears to be better than the TiN coating after repeated thermo-mechanical loading, due to its better thermal resistance, oxidation resistance, and lower decrease in hardness during the loading. 4. Conclusions The degradation behavior of both TiAlN and TiN coating were investigated using accelerated testing based on a pulsed laser ablation system. From observations of the surfaces and the cross-sections of the ablated spots, the acceleration levels were appropriate to evaluate the coatings. The TiAlN coating maintained adhesion to the substrate and was more resistant to various types of failure, such as surface crack propagation, as compared to the TiN coating. The coating thickness decreased in both coatings due to the repeated laser ablation. The substrate burst observed in the TiN coating specimen is caused by the higher thermal conductivity of the TiN as compared to TiAlN. There is a higher predicted life for the TiAlN coatings compared to that of TiN coatings. This better performance is attributed to the surface oxidation and spalling of the TiN coating layer, which causes the higher decrease in the hardness than that in the TiAlN coating. Further investigation will be progressed to determine the effects of residual stress and phase transition of hard coatings by the pulsed laser ablation. Acknowledgment This work was supported by the National Research Foundation of Korea (NRF) grant funded by the Korea government (MSIP) through GCRC-SOP (No. 2011-0030013). References
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Please cite this article as: S. Jeon, et al., Degradation of TiAlN coatings by the accelerated life test using pulsed laser ablation, Ceramics International (2014), http://dx.doi.org/10.1016/j.ceramint.2014.01.085