硅酸盐学报

二乙醇胺辅助溶胶–凝胶法低温合成锆钛酸铅纳米粉体

作者：孟庆华朱孔军邵斌董娜娜裘进浩

关键词：锆钛酸铅二乙醇胺纳米粉体溶胶–凝胶

分类号：TQ174.4

出版年,卷(期):页码：2012,40(2):271-276

DOI：

摘要：

摘要：以醋酸铅[Pb(CH₃COO)₂·3H₂O]、硝酸锆[Zr(NO₃)₄·5H₂O]和钛酸四丁酯[Ti(C₄H₉O)₄]为原料，以二乙醇胺(diethanolamine，DEA)为聚合剂，用溶胶–凝胶法制备了锆钛酸铅(PbZr_xTi₁_–_xO₃，PZT)纳米陶瓷粉体。研究了DEA对溶胶–凝胶法合成PZT陶瓷粉体的影响。通过Fourie变换红外光谱、热重–差热仪、X射线衍射仪、扫描电子显微镜和能谱仪等对所得到的粉体进行了表征。结果发现：DEA能有效促进钙钛矿相PZT结晶，最佳的DEA体积掺量为10%，430℃便可生成纯相PZT纳米粉体，随着煅烧温度升高结晶性逐渐增强。

Abstract: The nano-particles of lead zirconate titanate (PbZr_xTi₁_–xO₃, PZT) were synthesized by a sol–gel method using Pb(CH₃COO)₂? 3H₂O, Zr(NO₃)₄·5H₂O and Ti(OC₄H₉)₄ as starting materials. Diethanolamine (DEA) was used as a polymerizing agent. The effect of DEA on the sol–gel synthesis of PZT powders was investigated. The product powders were characterized by Fourier transform infrared spectroscopy, thermogravimetric–differential thermal analysis, X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy, respectively. The results show that DEA can accelerate the transformation to perovskite, and the optimum content of DEA is 10% in volume. The phase pure PZT nano-particles were synthesized at 430℃. The crystallinity could be improved when the calcination temperature was increased.

基金项目：

国家自然科学基金(50872053，50830201，51172108)；教育部新世纪优秀人才支持计划(NCET-10-0070)；教育部长江学者创新团队(IRT0968)；江苏高校优势学科建设工程资助项目；航空科学基金(2009ZF52058)；南京航空航天大学专项科研(NJ2010010，NZ2010001)资助项目。

作者简介：

第一作者：孟庆华(1984—)，男，硕士研究生。通信作者：朱孔军(1971—)，男，教授。

参考文献：

[1] HAERTLING G H. Ferroelectric ceramics: history and technology [J]. J Am Ceram Soc, 1999, 82(4): 797–818.

[2] ZENG T, DONG X L, CHEN S T, et al. Processing and piezoelectric properties of porous PZT ceramics [J]. Ceram Int, 2007, 33: 395–399.

[3] VITTAYAKORN N, RUJIJANAGUL G, CANN D P. Investigation of the influence of thermal treatment on the morphologies, dielectric and ferroelectric properties of PZT-based ceramics [J]. J Alloys Compd, 2007, 440: 259–264.

[4] SHROUT TR, PAPET P, KIM S, et al. Conventionally prepared submicrometer lead-based perovskite powders by reactive calcinations [J]. J Am Ceram Soc, 1990, 73(7): 1862–1867.

[5] KONG L B, MA J, ZHU W, et al. Highly enhanced sinter ability of commercial PZT powders by high-energy ball milling [J]. Mater Lett, 2000, 46(5): 274–280.

[6] 刘大格, 蔡伟, 张洪喜, 等. 以硝酸氧锆为锆源溶胶–凝胶合成PZT米晶的研究[J]. 硅酸盐学报, 1998, 26(3): 313–318.

LIU Dage, CAI Wei, ZHANG Hongxi, et al. J Chin Ceram Soc, 1998, 26(3): 313–318.

[7] LINARDOS S, ZHANG Q, ALCOCK J R. Preparation of sub-micron PZT particles with the sol–gel technique [J]. J Eur Ceram Soc, 2006, 26: 117–123.

[8] KHORSAND ZAK A, MAJID ABD W H. Effect of solvent on structure and optical properties of PZT nanoparticles prepared by sol–gel method, in infrared region [J]. Ceram Int, 2011, 37: 753–758.

[9] SANGSUBUN C, WATCHARAPASORN A, JIANSIRISOMBOON S. Densification and microstructure of lead zirconate titanate ceramics fabricated from a triol sol–gel powder [J]. Curr Appl Phys, 2008, 8: 61–65.

[10] XU Z J, CHU R Q, LI G R, et al. Preparation of PZT powders and ceramics via a hybrid method of sol–gel and ultrasonic atomization [J]. Mater Sci Eng B, 2005, 117: 113–118.

[11] LINARDOS S, ZHANG Q, ALCOCK J R. An investigation of the parameters effecting the agglomerate size of a PZT ceramic powder prepared with a sol–gel technique [J]. J Eur Ceram Soc, 2007, 27: 231–235.

[12] CHANG T I, WANG S C, LIU C P, et al. Thermal behaviors and phase evolution of lead zirconate titanate prepared by sol–gel processing: The role of the pyrolysis time before calcination [J]. J Am Ceram Soc, 2008, 91(8): 2545–2552.

[13] KIM S H, KOMARNENI S. Synthesis of PZT fine particles using Ti³⁺ precursor at a low hydrothermal temperature of 110℃ [J]. Ceram Int, 2011, 37: 1101–1107.

[14] XU G, JIANG W, QIAN M, et al. Hydrothermal synthesis of lead zirconate titanate nearly free-standing nanoparticles in the size regime of about 4nm [J]. Cryst Growth Des, 2009, 9(1): 13–16.

[15] LIN Y, LIU Y, SODANO H A. Hydrothermal synthesis of vertically aligned lead zirconate titanate nanowire arrays [J]. Appl Phys Lett, 2009, 95: 122901–122903.

[16] 徐刚, 赵高凌, 翁文剑, 等. 两步沉淀法合成锆钛酸铅相形成的反应机理[J]. 硅酸盐学报, 2008, 36(6): 733–738.

XU Gang, ZHAO Gaoling, WENG Wenjian, et al. J Chin Ceram Soc, 2008, 36(6): 733–738.

[17] 王西成. 湿化学方法制备Pb(Zr_xTi_1–x)O₃陶瓷微粉的研究[J]. 硅酸盐学报, 1997, 25(5): 542–546.

WANG Xicheng. J Chin Ceram Soc, 1997, 25(5): 542–546.

[18] XU G, WENG W, YAO J, et al. Low temperature synthesis of lead zirconate titanate powder by hydroxide co-precipitation [J]. Microelectron Eng, 2003, 66: 566–568.

[19] 刘红梅, 张德庆, 林海波, 等. 溶胶–凝胶法制备纳米PZT粉体及结构表征[J]. 材料工程, 2006, 3: 52–59.

LIU Hongmei, ZHANG Deqin, LIN Haibo, et al. J Mater Eng, 2006, 3: 52–59.

[20] POLLI A D, LANGE F F. Pyrolysis of Pb(Zr_0.5Ti_0.5)O₃ precursors: avoiding lead partitioning [J]. J Am Ceram Soc, 1995, 78(12): 3401–3404.

[21] FAHEEM Y, SHOAIB M. Sol–gel processing and characterization of phase-pure lead zirconate titanate nano-powders [J]. J Am Ceram Soc, 2006, 89(6): 2034–2037.

[22] TAHAR R B H, TAHAR N B H, SALAH A B. Preparation and characterization of PZT solid solutions via sol–gel process [J]. J Cryst Growth, 2007, 307: 40–43.

[23] TAHAR R B H, TAHAR N B H, SALAH A B. Low-temperature processing and characterization of single-phase PZT powders by sol–gel method [J]. J Mater Sci, 2007, 42: 9801–9806.

[24] GHASEMIFARD M, HOSSEINI S M, KHORSAND Z A, et al. Microstructural and optical characterization of PZT nanopowder prepared at low temperature [J]. Physica E, 2009, 41: 418–422.

[25] 彭秧锡, 张萍, 胡传跃. 锆钛酸铅纳米粉体的凝胶燃烧法制备及表征[J]. 硅酸盐学报, 2011, 39(3): 387–390.

PENG Yangxi, ZHANG Ping, HU Chuanyue. J Chin Ceram Soc, 2011, 39(3): 387–390.

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