Effect of Heat-treatment on Wear Performance of Nanolayer WN/TiN Coating S.H. YAO 1,a, Y.L. SU 2,b and W.H. KAO 3,c
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1 Applied Mechanics and Materials Vols (213) pp (213) Trans Tech Publications, Switzerland doi:1.428/ Effect of Heat-treatment on ear Performance of anolayer / Coating S.H. YAO 1,a, Y.L. SU 2,b and.h. KAO 3,c 1 Chang Jung Christian University, Kway Jen, Tainan 7111, Taiwan 2 ational Cheng Kung University, Department of Mechanical Engineering, Tainan 711, Taiwan 3 Chienkuo Technology University, Institute of Mechatronoptic Systems, Zhanghua 594, Taiwan a shyao@mail.cjcu.edu.tw, b ylsu@mail.ncku.edu.tw, c n @yahoo.com.tw Keywords: anolayer Coating,,, Heat-treatment, ear. Abstract. A nanolayer / coating was grown using an industrial-scale four-target reactive sputtering system. Effects of heat treatment on fundamental properties and wear performance of the nanolayer coating were studied. For comparison, a single layer was used as a reference. Characterization was carried out using a nano hardness tester, GDOES, XRD and SEM. ear performance was evaluated using an SRV wear tester. It was found that the as-deposited nanolayer / coating showed relatively high nano hardness and wear resistance as compared with the single layer. The heat treatment resulted in performance degradation of the nanolayer coating. After 6 heat-treatment, the nanolayer coating showed very poor mechanical performance. Introduction Surface coatings have been used as protective and functional layers in various engineering fields for many years. The current trend for PVD coatings is to develop multi-component and multilayer coatings. It has been learned that coatings with multilayer structure show improved strength and toughness [1]. For example, Chen et al. [2] found that the multilayer /Si coating shows enhanced hardness as compared to a single layer. A study by u et al. [3] was done on multi-component (Cr,) and multilayer /Cr coatings. It showed that at the period 24 nm, the hardness of multilayer coating reaches 3.5 GPa, which is higher than that of multi-component coating by 8 GPa. In this case, the period of the multilayer coating was controlled down to nano scale, which is called nanolayer coating alternatively. transfers to O 3 in air when the temperature is higher than 6. The O 3 phase has been proven to be a good solid lubricant [4]. A fully exploration on literature database found no study regarding nanolayer / coatings. In this work, a nanolayer / coating was prepared first. Then some of samples were heat treated in air at different temperature, aiming to understand the effects of heat treatment on fundamental properties and wear behavior. Experimental details Coating Preparation. The coatings were prepared by using a TEER UDP-45 industrial-scale four-target reactive DC closed-field unbalanced magnetron sputtering ion plating system (CFUBMSIPS TM ) [5]. The four targets, each with dimension of 3 mm 19 mm 1 mm (length width thickness), were vertically and orthogonally mounted on the chamber wall. In the center of chamber was a rotator, which carried a one-fold rotational specimen holder. The substrate material was JIS SKH51 steel, with a hardness HRc 51 after heat treatment. The substrates were polished to surface roughness Ra <.1 µm prior to deposition. The nanolayer coating studied here was composed of, from bottom to top, a interface, four periods of succesively alternative and layers with initiating, and finally a layer. The thickness of each or layer was controlled constant at 1 nm, and that of the interface ~.1µm. All rights reserved. o part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP, (ID: /11/12,2:12:23)
2 284 Frontiers of Manufacturing and Design Science III The coating procedures consisted of three main steps: 1) substrates degreasing and targets cleaning; 2) substrates conditioning using Ar + at parameters of DC substrate bias (U B ) = -35V, substrate holder rotating speed (ω) = 3 rpm, Ar flow rate = 5 sccm, duration = 15 min; and finally 3) growth of interface layer and nanolayer coating. To control accurately the thickness of each layer within the nanolayer coating, the deposition rate for or layer was studied first. It was determined that the deposition rate for layer was nm/min using one target at current = 3A, pulsed DC U B = ~-1V, pulse frequency (f) = 5 khz, duty cycle = 5%, ω = 3 rpm, distance between target and substrate (D s-t ) = 1mm, 2 flow rate = 2 sccm and Ar flow rate = 3 sccm. That for layer was nm/min using three targets at current = 3.5A while the rest conditions were identical to those used for the layer. ith the above conditions, the coating chamber was loaded with one and three targets. By controlling the power applied to the or targets and deposition intervals, a coating with nanolayer structure were obtained. The conditions for preparing the interface were using three targets at current 3A, duration 1 min., 2 flow rate = sccm and the rest was the same as those for the layer. The referenced single layer coating of thickness ~2.5 µm was grown using the same deposition system. The heat-treatment was conducted using an air furnace. The procedure was as follows: putting the samples into the heating chamber at room temperature; heating at a rate 5 /min until the set temperature; holding one hour and then furnace-cooling. Two temperatures, 5 and 6, were used. Characterization. Standard metallographic polishing techniques were used to prepare the cross-sectional samples. The hardness values were taken using a nano-hardness tester operated at an applied load 1m. Each hardness value presented was an average of ten measurements. The crystalline structure and phases of coatings were identified by an XRD at 2Θ=2-8 degree and a scanning rate of 4 deg/min using grazing angle diffraction technique with X-ray incident angle of 2 and Cu Kα radiation operated at 4 kv and 1 ma. The chemical composition profile through coatings was determined by using a glow discharge optical emission spectroscopy (GDOES). The cross-sectional microstructure of coatings and worn morphology on coatings after wear tests were examined using an SEM equipped with an EDX. ear Test. The wear tests were performed using an SRV reciprocating sliding wear tester (Schwingung Reibung and Verschleiss tester, Optimol Instruments Prüftechnik GmbH, Germany). The ball-on-disk point-contact geometric configuration was used, employing a ball with a dimension of 1mm (diameter) and a disk with that of 24mm 7.9mm (diameter thickness). The details of the SRV wear machine and specimen configuration can be referred in the article of Yao et al. [6]. The material of the balls was Si 3 4. The wear test conditions were: no lubrication, applied load 1, stroke 1 mm, frequency 5Hz and duration 2 min. The friction coefficient was on-line picked up and recorded in a PC. The wear scar were measured for wear depth using a surface profilometer with a diamond stylus. An average of five sets of wear test results was presented. Results and discussion Coatings. Figure 1 is an SEM photo of cross-sectional microstructure of the as-deposited / nanolayer coating, which shows the definite multilayer configuration in nano scale. The darker layers are and the lighter ones. ith the multilayer structure, or element fluctuated with depth as shown in Figure 1. In Figure 2, one can see that, after 5 heat treatment, the coating surface ( layer) was highly oxidized, and the rest part, from the layer immediate next to surface layer to the interface, remained nearly intact, as evidenced in Figure 2. hen the coating was after 6 heat treatment (Figure 3a), its multilayer structure was largely affected, leading to some ambiguity. However, the whole coating was fully oxidized, as shown in Figure 3. Figure 4 shows the result of XRD analyses. Figure 4 shows that the as-deposited / nanolayer coating was consisted of, and 2 phases. The coating after 5 heat treatment, in addition to formation of little O 2, was composed of the phases identical to those of the as-deposited coating, as shown in Figure 4. The XRD patterns, shown in Figure 4(c), indicates the formation of O 3 and O 2, being consistent with the results shown above in Figure 3.
3 Applied Mechanics and Materials Vols Figure 5 shows a comparison of nano hardness and Young s modulus of the / nanolayer coating and the single layer coating. The as-deposited / nanolayer coating showed much higher hardness as compared with the referenced coating. The hardness of / coating after 5 heat treatment reduced, probably due to release of residual compressive stress. After 6 heat treatment, both the nanolayer coating and 1 single layer coating showed very poor 8 performance in hardness and Young s modulus because of severe oxidation. ear test. Figure 6 shows the wear test results. Lacking of data for the single layer coating after 6 heat treatment was because the coating was fully detached from the substrate due to severe oxidation. As can been seen, the as-deposited nanolayer coating showed the best wear performance. The nanolayer coating after 5 heat treatment was to some extent less wear resistant than the as-deposited one. However, both showed wear resistance superior to the referenced single layer. On bases of the study of Greenwood et al. [4], the formation of O 3 helps for reducing friction coefficient and thus increasing wear resistance. Here, by means of 6 heat treatment, the Figure 1. Cross-sectional microstructure of as-deposited / nanolayer coating; elemental distribution vs. distance of Figure 2. Cross-sectional microstructure of / nanolayer coating after 5 heat treatment; elemental distribution vs.distance of Figure 3. Cross-sectional microstructure of / nanolayer coating after 6 heat treatment; elemental distribution vs. distance of. O O
4 286 Frontiers of Manufacturing and Design Science III Figure 4. XRD diffraction patterns of nanolayer / coating: as-deposited; after 5 and (c) 6 heat treatment. layers transferred to O 3 phase. However, as shown in Fig 6, it showed very poor wear performance, which in conclusion resulted from the following facts: 1) The hardness of O 3 is of very low value about 7 GPa [7]. 2) The layers were damaged due to severe oxidation, transferring into O 2, which has been known to be very wear irresistant [8]. 3) Due to a large difference in coefficient of thermal expansion between O 3 ( K -1 ) [9] and O 2 ( K -1 ) layers [1], the coating collapsed layer by layer, as shown in Figure 7. Hardness (GPa) / Young's modulus, E (GPa) Figure 5. anohardness and Young s modulus of nanolayer / coating and single layer coating at as-deposited and after heat treated conditions. Summary e prepared a nanolayer / coating by using an industrial-scale four-target reactive sputtering system loaded with one target and three targets. Then, some of these samples were heat treated at 5 or 6 in air, aiming to obtain enhancement in wear performance by a formation of O 3 within the coating. The research founding is as follows: The as-deposited nanolayer / coating showed great enhancement in nano hardness and wear resistance as compared with the single layer. The 5 heat treatment for the nanolayer coating resulted in a minor reduction in wear performance but a substantial decrease in hardness. The nanolayer coating after 6 heat treatment demonstrated very poor wear performance due to structural destruction of the whole coating.
5 Applied Mechanics and Materials Vols Therefore, it is of no use by post heat treatment to achieve improvement in hardness and wear performance of the nanolayer / coating. However, the gaining by the as-deposited nanolayer / coating is very inspiring. ear depth(µm) Friction coefficient (µ). /.3 Figure 6. ear test results of nanolayer / coating and single layer coating at as-deposited and after heat treated conditions. Figure 7. Layered collapse of nanolayer / coating after 6 heat treatment. Acknowledgment The authors wish to express their thanks for the finical support by ational Science Council under the contract of SC E Grateful thanks are also dedicated to Center for Micro/ano Science and Technology of and The Instrument Center of ational Cheng Kung University for their supports for analyzing equipment. References [1] H. Jensen, J. Sobata, et al.: J. Vac.Sci. Tech. Vol. 15 (1997), p [2] Yu-Hsia Chen, Murat Guruz, et al.: Surf. & Coat. Tech. Vol. 154 (22), p [3] Fan-Bean u, Shih-Kang en, et al.: Surf. & Coat. Tech. Vol. 2 (25), p [4] O.D Greenwood, S.C Moulzolf, et. al.: ear Vol. 232 (1999), p. 84 [5] TEER FILMS LTD., UK Patent o , page= cfubmsip. [6] S.H. Yao,. H. Kao, et. al.:: Mater. Sci. Engin. A Vol. 392 (25), p. 38. [7].M.G. Parreira,.J.M. Carvalho, et. al.: Thin Solid Films Vol. 51 (26), p [8] R. uhrer,.y. Yeung, et. al.: Thin Solid Films Vol , (1996), p [9] C. Rosen, E. Banks, et. al.: Acta Cryst. Vol. 9 (1956), p [1] Solomon Musikant: hat Every Engineer Should Know About Ceramics (Marcel Dekker, Inc, ew York 199).
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