立方相Y掺杂ZrO2纳米晶薄膜的制备与辐照效应研究

doi:10.15541/jim20140651

摘要/Abstract

摘要：

采用溶胶-凝胶结合旋涂法在单晶Si衬底上制备了立方相Y掺杂ZrO₂纳米晶薄膜(YSZ), 并分析了制备工艺参数对YSZ成膜的影响。采用光学显微镜、扫描电子显微镜、X射线衍射和透射电镜等手段对样品进行了表征和分析。结果表明, 加入PVA作为分散剂、采用分级干燥工艺以及提高匀胶转速可大大提高YSZ薄膜的成膜质量, 制备的YSZ薄膜表面十分平整, 没有出现裂纹。YSZ薄膜为立方相结构, 没有出现其它相。薄膜由平均晶粒尺寸为9.4 nm的纳米晶组成, 薄膜的厚度约为60 nm。在室温条件下, 低剂量的Xe离子辐照YSZ薄膜后出现微裂纹, 而当辐照剂量比较高时, 由于热峰效应, 辐照引起的微裂纹逐渐发生愈合。并且, 随着辐照剂量的增加, YSZ薄膜的平均晶粒尺寸增大。

关键词: ZrO2纳米晶薄膜, 溶胶-凝胶法, 立方相, 辐照效应

Abstract:

Nanocrystalline cubic yttrium-stabilized ZrO₂ films (YSZ) were prepared on silicon substrate via Sol-Gel combined with spin-coating method. The as-grown films were characterized by optical microscope, SEM, XRD and TEM. It was found that preparation parameters have obvious effect on quality of the YSZ film. The quality of YSZ thin films can be greatly improved by adding PVA as dispersing agent, adopting the grading drying process and increasing the spin speed. Smooth films without any cracks can be obtained by optimum growth conditions. XRD result shows that the film is cubic structure with no other phase. The thickness of the YSZ film is about 60 nm, and its average grain-size is 9.4 nm. When the samples are irradiated by Xe ions with low dose at room-temperature, microscopic cracks are detected in the YSZ films. As the ion irradiation dose increases, the irradiation-induced cracks are gradually recovered, which might attribute to the thermal spike effect on the film. In addition, the average grain-size of the YSZ film grows with irradiation dose increasing.

Key words: nanocrystalline ZrO2 film, Sol-Gel, cubic phase, irradiation effect

中图分类号:

TB43

王卡, 万康, 张静, 陈林, 陈琼, 常永勤, 龙毅. 立方相Y掺杂ZrO₂纳米晶薄膜的制备与辐照效应研究[J]. 无机材料学报, 2015, 30(6): 593-598.

WANG Ka, WAN Kang, ZHANG Jing, CHEN Lin, CHEN Qiong, CHANG Yong-Qin, LONG Yi. Fabrication and Irradiation of Nanocrystalline Yttrium-stabilized Cubic ZrO₂ Film[J]. Journal of Inorganic Materials, 2015, 30(6): 593-598.

图/表 8

图1 (a)未加入PVA的YSZ薄膜的SEM形貌和(b)自然干燥条件下YSZ薄膜的光学显微镜照片, 最优化工艺条件下YSZ薄膜的SEM形貌(c)和BSD图片(d)

Fig. 1 (a) SEM image of YSZ film without adding PVA, (b) optical microscope image of YSZ film dried in air, SEM image (c) and BSD image (d) of YSZ film without cracks prepared under optimal conditions

图2 样品的截面SEM照片

Fig. 2 Cross-sectional SEM image of the YSZ film

图3 YSZ纳米晶薄膜的(a)XRD和(b)GIXRD图谱

Fig. 3 (a) XRD and (b) GIXRD patterns of the nanocrystalline YSZ film

图4 YSZ薄膜样品的剖面TEM照片(a)及对应区域的SEAD图案(b), STEM模式下从YSZ到硅片的成分分布 (c)及其部分放大(d)

Fig. 4 Cross-sectional TEM image (a) and corresponding SAED pattern (b) of YSZ film, STEM-EDS line scan profile from the YSZ film to Si substrate (c) and its enlarged part (d)

表1 样品表面平整处和突起处的元素成分

Table 1 Element compositions at flat and crack position on the surface of sample

Element line	Flat site /at%	Crack site/at%
O K	17.00	14.22
Si K	79.91	83.25
Zr L	3.10	2.53
Total	100.00	100.00

图5 YSZ薄膜经不同剂量Xe离子辐射后的SEM照片

Fig. 5 SEM images of the YSZ films irradiated with different irradiation doses

图6 YSZ 薄膜在1.0 dpa Xe离子辐照剂量下的高倍SEM照片(a)及其对应的BSD图片(b)和沿裂纹方向的EDS线扫描分析曲线(c)

Fig. 6 High magnification SEM image of the YSZ films irradiated with 1.0 dpa irradiation dose (a), and corresponding BSD image (b) as well as its EDS line scan profile across the crack (c)

图7 晶粒尺寸随辐照剂量变化关系

Fig. 7 Plot of average grain-size as a function of irradiation dose

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立方相Y掺杂ZrO₂纳米晶薄膜的制备与辐照效应研究

Fabrication and Irradiation of Nanocrystalline Yttrium-stabilized Cubic ZrO₂ Film

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