退火温度对Bi3.15(Eu0.7Nd0.15)Ti3O12铁电薄膜力学性能的影响

doi:10.3724/SP.J.1077.2013.12201

无机材料学报 ›› 2013, Vol. 28 ›› Issue (2): 131-135.DOI: 10.3724/SP.J.1077.2013.12201 CSTR: 32189.14.SP.J.1077.2013.12201

退火温度对Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂铁电薄膜力学性能的影响

蒋大洞, 郑学军, 龚跃球, 朱哲, 彭金峰

(湘潭大学材料与光电物理学院, 湘潭 411105)

收稿日期:2012-04-01 修回日期:2012-05-20 出版日期:2013-02-10 网络出版日期:2013-01-23
作者简介:蒋大洞(1987–), 男, 硕士研究生. E-mail: kaditin@gmail.com
基金资助:
教育部长江学者和创新团队发展计划([2011]20);国家自然科学基金(10825209);长江学者奖励计划([2009]17);湘潭大学博士科研启动基金(11QDZ24)

Effect of Annealing Temperature on the Mechanical Properties of Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂ Ferroelectric Thin Films

JIANG Da-Dong, ZHENG Xue-Jun, GONG Yue-Qiu, ZHU-Zhe, PENG Jin-Feng

(Faculty of Materials and Optoelectronic Physics, Xiangtan University, Xiangtan 411105, China)

Received:2012-04-01 Revised:2012-05-20 Published:2013-02-10 Online:2013-01-23
About author:JIANG Da-Dong. E-mail: kaditin@gmail.com
Supported by:
Changjiang Scholars and Innovative Research Team in University (PCSIRT[2011]20);National Natural Science Foundation of China (10825209);Changjiang Scholar Incentive Program ([2009]17);Start-up Fund Dr of Xiangtan University (11QDZ24)

摘要/Abstract

摘要：

利用金属有机物分解法(MOD)在Pt/Ti/SiO₂/Si(111)衬底上制备了Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂ (BENT)薄膜, 并经600℃、650℃、700℃、750℃退火处理。通过纳米压痕法测试了薄膜的硬度和弹性模量, 采用X射线衍射(XRD)测量了薄膜的残余应力。BENT薄膜的晶粒尺寸随着退火温度的升高而不断变大。当晶粒尺寸从37 nm增大到46 nm时, 薄膜的硬度值从8.4 GPa减少到3.1 GPa, 弹性模量从171.5 GPa减小到141.6 GPa。随着退火温度从600℃升高到750℃时, 薄膜的残余压应力值从-743 MPa减小到了-530 MPa。退火温度为600℃的BENT薄膜具有最大的硬度和弹性模量。

关键词: 弹性模量, 硬度, 残余应力, 退火温度

Abstract:

Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂ (BENT) thin films were deposited on Pt/Ti/SiO₂/Si(111) substrates via metal- organic decomposition (MOD) and annealed at 600℃, 650℃, 700℃ and 750℃. The hardness and elastic modulus were measured by nanoindentation, and the residual stress was measured by X-ray diffraction (XRD). The grain sizes of the BENT thin films increase with the annealing temperatures increasing. With the grain size increasing from 37 nm to 46 nm, the hardness decreases from 8.4 GPa to 3.1 GPa and the elastic modulus decreases from 171.5 GPa to 141.6 GPa. While the annealing temperature increases from 600℃ to 750℃, the residual stress decreases from -743 MPa to -530 MPa. The BENT thin film annealed at 600℃ shows the largest hardness and elastic modulus.

Key words: elastic modulus, hardness, residual stress, annealing temperature

中图分类号:

TQ174

蒋大洞, 郑学军, 龚跃球, 朱哲, 彭金峰. 退火温度对Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂铁电薄膜力学性能的影响[J]. 无机材料学报, 2013, 28(2): 131-135.

JIANG Da-Dong, ZHENG Xue-Jun, GONG Yue-Qiu, ZHU-Zhe, PENG Jin-Feng. Effect of Annealing Temperature on the Mechanical Properties of Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂ Ferroelectric Thin Films[J]. Journal of Inorganic Materials, 2013, 28(2): 131-135.

图/表 7

图1 (a) 退火温度分别为600、650、700、750℃的BENT薄膜的XRD图谱, (b) 退火温度为750℃的BENT薄膜的EDS能谱分析

Fig. 1 (a) XRD patterns of BENT thin films annealed at 600℃, 650℃, 700℃, 750℃, (b) EDS analysis of BENT thin film annealed at 750℃

图2 退火温度为750℃的BENT薄膜的表面形貌图(a)和断面形貌图(b)

Fig. 2 Surface morphology (a) and typical cross-sectional micrograph (b) of BENT thin film annealed at 750℃

图3 四种不同退火温度的BENT薄膜典型的载荷-深度曲线

Fig. 3 Typical load-displacement indentation curves of BENT thin films annealed at different annealing temperatures

图4 BENT薄膜中硬度、弹性模量随退火温度的变化关系

Fig. 4 Hardness versus annealing temperature and elastic modulus vs annealing temperature curves for BENT thin films

图5 不同退火温度的BENT (117)晶面在不同倾斜角ψ下的XRD峰

Fig. 5 XRD peaks of BENT (117) plane for different annealing temperature with different tilt angles ψ

图6 不同退火温度下的BENT薄膜中2θψ -sin2ψ的关系

Fig. 6 Plots of 2θψ-sin2ψ for BENT thin films annealed at different temperature

图7 BENT薄膜的残余应力和晶粒尺寸随退火温度的变化关系

Fig. 7 Residual stress and grain size for BENT thin films as functions of annealing temperature

参考文献 20

[1]	Cross E. Materials science: lead-free at last. Nature, 2004, 432(7013): 24-25.
[2]	Chon U, Jang H M, Kim K B, et al. Layered perovskites with giant spontaneous polarizations for nonvolatile memories. Phys. Rev. Lett. , 2002, 89(8): 087601-1-4.
[3]	Lee H N, Hesse D, Zakharov N. Ferroelectric Bi3.25La0.75Ti3O12 films of uniform a-axis orientation on silicon substrates. Science, 2002, 296(5575): 2006-2009.
[4]	Liu C Y, Guo D Y, Wang C B, et al. Ferroelectric and dielectric properties of Bi4-xNdxTi3O12 thin films prepared by Sol-Gel method. J. Mater. Sci., 2012, 23(3): 802-806.
[5]	Zheng X J, He L, Zhou Y C, et al. Effects of europium content on the microstructural and ferroelectric properties of Bi4-xEuxTi3O12 thin films. Appl. Phys. Lett. , 2006, 89(25): 252908-1-3.
[6]	Fu C J, Huang Z X, Li J, et al. Preparation and ferroelectric properties of Ho3+/Mo6+ cosubstituted Bi4Ti3O12 thin films by Sol-Gel method. J. Electron Mater., 2010, 39(2): 258-261.
[7]	Zhang S T, Chen Y F, Wang J, et al. Ferroelectric properties of La and Zr substituted Bi4Ti3O12 thin films. Appl. Phys. Lett., 2004, 84(18): 3660-3662.
[8]	Zhong X L, Hu Z S, Li B, et al. Microstructures and electrical properties of Nd3+/V5+-cosubstituted Bi4Ti3O12 thin films. J. Cryst. Growth, 2008, 310(21): 4516-4520.
[9]	Wen H, Wang X H, Li L T. Mechanical properties of Sol-Gel derived BiScO3-PbTiO3 thin films by nanoindentation. J. Appl. Phys. , 2006, 100(8): 084315-1-5.
[10]	Zheng X J, Yi W M, Chen Y Q, et al. The effects of annealing temperature on the properties of Bi3.15Nd0.85Ti3O12 thin films. Scripta. Mater., 2007, 57(8): 675-678.
[11]	Zhang D Z, Zheng X J, Feng X, et al. Ferro-piezoelectric properties
[12]	of 0.94(Na0.5Bi0.5)TiO3-0.06BaTiO3 thin film prepared by metal- organic decomposition. J. Alloys Compd., 2010, 504(1): 129-133.
[13]	YAO Su-Wei, ZHANG Lu, ZHANG Wei-Guo, et al. Nanomechanics properties research of anodic aluminium oxide film. Journal of Inorganic Materials, 2006, 21(3): 736-740.
[14]	Wang Y H, Moitreyee M R, Kumar R, et al. The mechanical properties of ultra-low-dielectric-constant films. Thin Solid Films, 2004, 462-463: 227-230.
[15]	Conrad H. Effect of grain size on the lower yield and flow stress of iron and steel. Acta Metall., 1963, 11(1): 75-77.
[16]	Li J C M. Petch relation and grain boundary sources. Trans. Metall. Soc. AIME, 1963, 227: 239-247.
[17]	Ashby M F. The deformation of plastically non-homogeneous materials. Philos. Mag., 1970, 21(170): 399-424.
[18]	Delobelle P, Guillon O, Blanc E F, et al. True Young modulus of Pb(Zr,Ti)O3 films measured by nanoindentation. Appl. Phys. Lett., 2004, 85(22): 5185-5187.
[19]	Liu W L, Xia H R, Han H, et al. Structural, morphology and electrical studies of Sm-modified bismuth titanate thin films on Si (100). J. Solid State Chem., 2004, 177(9): 3021-3027.
[20]	杨卫. 力电失效学. 北京: 清华大学出版社, 2001: 18-19.

退火温度对Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂铁电薄膜力学性能的影响

Effect of Annealing Temperature on the Mechanical Properties of Bi_3.15(Eu_0.7Nd_0.15)Ti₃O₁₂ Ferroelectric Thin Films

RichHTML

PDF (PC)

可视化