Sc2W3O12薄膜制备及其负热膨胀性能

doi:10.15541/jim20150219

无机材料学报 ›› 2015, Vol. 30 ›› Issue (12): 1278-1282.DOI: 10.15541/jim20150219 CSTR: 32189.14.10.15541/jim20150219

Sc₂W₃O₁₂薄膜制备及其负热膨胀性能

张志萍^1,2, 刘红飞², 潘坤旻², 陈小兵², 曾祥华²

(1. 扬州大学广陵学院, 扬州 225009; 2. 扬州大学物理科学与技术学院, 扬州 225002)

收稿日期:2015-05-08 修回日期:2015-06-17 出版日期:2015-12-20 网络出版日期:2015-11-24
作者简介:张志萍(1982–), 女, 博士研究生, 讲师. E-mail: zp-hf@163.com
基金资助:
国家自然科学基金(51102207);江苏省高校自然科学基金( 14KJB430025);扬州大学科技创新基金(2010CXJ081)

Synthesis of Negative Thermal Expansion Sc₂W₃O₁₂ Thin Film

ZHANG Zhi-Ping^1,2, LIU Hong-Fei², PAN Kun-Min², CHEN Xiao-Bing², ZENG Xiang-Hua²

(1. Guangling College, Yangzhou University, Yangzhou 225009, China; 2. College of Physics Science and Technology, Yangzhou University, Yangzhou 225002, China)

Received:2015-05-08 Revised:2015-06-17 Published:2015-12-20 Online:2015-11-24
About author:ZHANG Zhi-Ping. E-mail: zp-hf@163.com
Supported by:
National Natural Science Foundation of China (51102207);University Natural Science Research Foundation of Jiangsu Province (14KJB430025);Yangzhou University Science and Technique Innovation Foundation (2010CXJ081)

摘要/Abstract

摘要：

采用脉冲激光沉积法制备了斜方相Sc₂W₃O₁₂薄膜。利用X射线衍射仪(XRD)和场发射扫描电镜(FESEM)对Sc₂W₃O₁₂靶材和Sc₂W₃O₁₂薄膜组分、表面形貌和靶材断面形貌进行表征, 研究衬底温度与氧分压对薄膜制备的影响。采用变温XRD和热机械分析仪(TMA)分析了Sc₂W₃O₁₂陶瓷靶材和薄膜的负热膨胀特性。实验结果表明: 经1000℃烧结6 h得到结构致密的斜方相Sc₂W₃O₁₂陶瓷靶材, 其在室温到600℃的温度范围内平均热膨胀系数为-5.28×10^-6 K^-1。在室温到500℃衬底温度范围内脉冲激光沉积制备的Sc₂W₃O₁₂薄膜均为非晶态, 随着衬底温度的升高, 薄膜表面光滑程度提高; 随着沉积氧压强增大, 表面平整性变差。非晶膜经1000℃退火处理7 min后得到斜方相Sc₂W₃O₁₂多晶薄膜, 在室温到600℃温度区间内, Sc₂W₃O₁₂薄膜的平均热膨胀系数为-7.17×10^-6 K^-1。

关键词: 负热膨胀, 薄膜, 脉冲激光沉积, 钨酸钪

Abstract:

Orthorhombic Sc₂W₃O₁₂ thin films were deposited by pulsed laser deposition method. The microstructure, composition and morphology of the Sc₂W₃O₁₂ ceramic target and thin films were investigated using the X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). The effects of the substrate temperature and oxygen pressure on the Sc₂W₃O₁₂ thin films were studied. The negative thermal expansion (NTE) properties of the Sc₂W₃O₁₂ ceramic target and thin film were characterized using high temperature XRD and thermal mechanical analysis (TMA). Results indicate that the compact orthorhombic Sc₂W₃O₁₂ ceramic target with excellent NTE can be prepared by sintering at 1000℃ for 6 h. The average thermal expansion coefficient of the orthorhombic Sc₂W₃O₁₂ ceramic target is -5.28×10^-6 K^-1 from room temperature to 600℃. All the as-deposited Sc₂W₃O₁₂ thin films are amorphous. The surface of the as-deposited Sc₂W₃O₁₂ thin film becomes smoother, but it becomes uneven when the substrate temperature increases. The Sc₂W₃O₁₂ thin film with excellent NTE is crystallized after annealing at 1000℃ for 7 min. The thermal expansion coefficient of the orthorhombic Sc₂W₃O₁₂ thin film is calculated to be -7.17×10^-6 K^-1 in the temperature range from room temperature to 600℃.

Key words: negative thermal expansion, thin film, pulsed laser deposition, Sc2W3O12

中图分类号:

O484
TB43

张志萍, 刘红飞, 潘坤旻, 陈小兵, 曾祥华. Sc₂W₃O₁₂薄膜制备及其负热膨胀性能[J]. 无机材料学报, 2015, 30(12): 1278-1282.

ZHANG Zhi-Ping, LIU Hong-Fei, PAN Kun-Min, CHEN Xiao-Bing, ZENG Xiang-Hua. Synthesis of Negative Thermal Expansion Sc₂W₃O₁₂ Thin Film[J]. Journal of Inorganic Materials, 2015, 30(12): 1278-1282.

图/表 7

图1 在1000℃烧结6 h制备得到Sc2W3O12靶材的XRD图谱

Fig. 1 XRD pattern of Sc2W3O12 ceramic target sintered at 1000℃ for 6 h

图2 Sc2W3O12陶瓷靶材的断面SEM照片

Fig. 2 Cross-section SEM image of Sc2W3O12 ceramic target

图3 Sc2W3O12陶瓷靶材的热膨胀曲线

Fig. 3 Thermal expansion curve of the ceramic Sc2W3O12 target

图4 Sc2W3O12靶材和薄膜的XRD图谱

Fig. 4 XRD patterns of Sc2W3O12 target and thin films. (a) Sc2W3O12 target;(b) Sc2W3O12 thin film;(c) Amorphous Sc2W3O12 thin film

图5 不同条件下沉积制备的Sc2W3O12薄膜的SEM图片

Fig. 5 SEM images of as-deposited and annealed Sc2W3O12 thin films prepared at different conditions. (a) Room temperature, 5 Pa; (b) 300℃, 5 Pa; (c) 500℃, 5 Pa; (d) 500℃, 5 Pa; (e) 500℃, 10 Pa; (f) 500℃,20 Pa; (g) Annealed at 1000℃ for 7 min; (h) Annealed at 1000℃ for 7 min

图6 斜方相Sc2W3O12薄膜的变温XRD图谱

Fig. 6 High temperature XRD patterns of the orthorhombic Sc2W3O12 thin film

图7 斜方相Sc2W3O12薄膜的晶格常数与温度关系曲线和拟合曲线

Fig. 7 Fitting curve and lattice constants of the orthorhombic Sc2W3O12 thin film as a function of temperature

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Sc₂W₃O₁₂薄膜制备及其负热膨胀性能

Synthesis of Negative Thermal Expansion Sc₂W₃O₁₂ Thin Film

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