靶成分和溅射参数对碳化钒薄膜微结构与力学性能的影响

doi:10.3724/SP.J.1077.2012.00536

无机材料学报 ›› 2012, Vol. 27 ›› Issue (5): 536-540.DOI: 10.3724/SP.J.1077.2012.00536 CSTR: 32189.14.SP.J.1077.2012.00536

靶成分和溅射参数对碳化钒薄膜微结构与力学性能的影响

沈洁, 李冠群, 李玉阁, 李戈扬

(上海交通大学金属基复合材料国家重点实验室, 上海 200240)

收稿日期:2011-07-16 修回日期:2011-12-06 出版日期:2012-05-10 网络出版日期:2012-03-31
作者简介:沈洁(1986-), 女, 硕士研究生. E-mail: ziyisj@126.com
基金资助:
国家自然科学基金(51071104) National Natural Science Foundation of China (51071104)

Effect of Target Composition and Sputtering Parameters on Microstructure and Mechanical Properties of Vanadium Carbide Films

SHEN Jie, LI Guan-Qun, LI Yu-Ge, LI Ge-Yang

(State Key Lab of Metal Matrix Composites, Shanghai Jiao Tong University, Shanghai 200240, China)

Received:2011-07-16 Revised:2011-12-06 Published:2012-05-10 Online:2012-03-31
About author:SHEN Jie. E-mail: ziyisj@126.com

摘要/Abstract

摘要：

为了提高碳化物靶溅射薄膜的结晶程度和相应的力学性能, 采用等化学计量比的VC靶(n(C):n(V)=1:1)和富V的VC靶(n(C):n(V)=0.75:1)通过磁控溅射方法制备了一系列VC薄膜, 利用EDS、XRD、SEM和微力学探针研究了靶成分、溅射气压和基片温度对薄膜化学成分、微结构和力学性能的影响. 结果表明, 对于等化学计量比的VC靶, 在Ar气压为2.4~3.2 Pa的范围内可获得结晶程度和硬度较高的VC薄膜, 其最高硬度为28 GPa. 而采用富V的VC靶时, 在较低的Ar气压(0.6~1.8 Pa)下就可获得结晶程度高的VC薄膜, 其硬度达到31.4 GPa. 可见, 相对于溅射参数的Ar气压和基片温度, 靶的成分对于所获薄膜的成分、微结构和力学性能影响更显著, 因而适当提高靶中金属组分的含量是获得结晶良好且具高硬度的VC薄膜更为有效的途径.

关键词: 碳化钒, 薄膜, 微结构, 力学性能, 磁控溅射

Abstract:

To improve the crystalinity and mechanical properties of the films sputtering with carbide target, a series of vanadium carbide films were prepared by magnetron sputtering in an argon atmosphere using the stoichiometric VC target (n(C):n(V)=1:1) and substoichiometric VC target (n(C):n(V)=0.75:1). Energy-dispersive X-ray spectroscopy, X-ray diffraction, scanning electron microscopy and nanoindentation were employed to characterize their composition, microstructure and mechanical properties. The results show that for the VC target (n(C):n(V)=1:1), only when the Ar pressure is between 2.4 Pa and 3.2 Pa, the films can obtain fine crystallized structure and attain high hardness, of which the highest hardness is 28 GPa. For the V-rich VC target, fine crystallized films and high hardness (31.4 GPa) could be gained in lower Ar pressure (0.6-1.8 Pa). Compared with argon pressure and substrate temperature, target composition is the main factor of the film composition, microstructure and mechanical properties, thus proper increasing the content of metal component of the target is a more effective way to get VC films with good crystalinity and high hardness.

Key words: vanadium carbide, film, microstructure, mechanical properties, magnetron sputtering

中图分类号:

O484

沈洁, 李冠群, 李玉阁, 李戈扬. 靶成分和溅射参数对碳化钒薄膜微结构与力学性能的影响[J]. 无机材料学报, 2012, 27(5): 536-540.

SHEN Jie, LI Guan-Qun, LI Yu-Ge, LI Ge-Yang. Effect of Target Composition and Sputtering Parameters on Microstructure and Mechanical Properties of Vanadium Carbide Films[J]. Journal of Inorganic Materials, 2012, 27(5): 536-540.

图/表 7

图1 VC薄膜的成分随溅射气压的变化

Fig. 1 Composition of VC films sputtering at different pressures

图2 不同Ar气压下VC-Ⅰ薄膜和VC-Ⅱ薄膜的XRD图谱

Fig. 2 XRD patterns of VC-Ⅰ (a) and VC-Ⅱ(b) films sputtering at different Ar pressures

图3 VC-Ⅰ薄膜截面断口的SEM照片显示, 低气压时(0.32 Pa)的薄膜断口平整, 具有非晶断口的特征(图3(a)); 气压升至3.2 Pa时, 薄膜呈现明显的柱状晶生长特征(图3(b)); 进一步增加溅射气压至4.0 Pa以上时, 薄膜的柱状晶形貌已经很不明晰, 而具有非晶断口的特征(图3(c)). 这些薄膜断口的观察结果与XRD分析结果有很好的一致性.

图3 不同溅射气压下VC-Ⅰ薄膜截面的SEM照片

Fig. 3 Cross-sectional SEM images of VC-Ⅰ films sputtering at different Ar pressures

图4 VC薄膜硬度随溅射气压的变化

Fig. 4 Hardness of VC films as a function of sputtering pressure

图5 不同基片温度下VC-Ⅰ薄膜(PAr =2.4 Pa)的XRD图谱

Fig. 5 XRD patterns of VC-Ⅰfilms (PAr =2.4 Pa) sputtering at different substrate temperatures

图6 VC-Ⅰ薄膜(PAr=2.4 Pa)和VC-Ⅱ薄膜(PAr=1.2 Pa)硬度随基片温度的变化

Fig. 6 Hardness of VC-Ⅰfilms (PAr =2.4 Pa) and VC-Ⅱfilms (PAr =1.2 Pa) sputtering at different substrate temperatures

参考文献 12

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靶成分和溅射参数对碳化钒薄膜微结构与力学性能的影响

Effect of Target Composition and Sputtering Parameters on Microstructure and Mechanical Properties of Vanadium Carbide Films

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