SrTiO_3基双功能陶瓷及纳米掺杂改性的研究
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摘要
本实验采用一次烧成工艺制备了SrTiO_3基双功能陶瓷并对其压敏特性和介电特性进行了系统研究。
试样首先在N_2+C弱还原气氛中于1420℃保温2.5h烧成，获得良好的半导化SrTiO_3烧结体，然后随炉冷却至1180℃，通氧气进行保温热处理20min，使晶界绝缘化。实验表明：掺杂施主离子的种类及浓度、掺杂受主离子的种类、烧结温度等因素均对微观结构、电性能产生重要影响。双施主La_2O_3+Nb_2O_5掺杂、单施主La_2O_3掺杂，分别以MnCO_3和CuO为受主掺杂均能获得低压敏电压兼高介电常数的SrTiO_3基双功能陶瓷，表现出良好的压敏性能与介电性能。相比较而言，单施主La_2O_3掺杂以CuO为受主的试样具有较低压敏电压(V_(1mA)<10V／mm)、高介电常数(ε>0000)的优势；双施主La_2O_3+Nb_2O_5掺杂以MnCO_3为受主的试样具有非线性高(α>8)、烧结温度宽的特点。
为了改善材料烧结性和优化电性能，采用有机配合物前驱体法制备La_2O_3施主掺杂剂的纳米粉体，采用化学共沉淀法分别制备Si-Al-Mn、Si-Al-Cu受主掺杂剂及助溶剂复合纳米粉体，对SrTiO_3进行纳米掺杂改性。结果表明：采用合理的配方及工艺可获得压敏电压极低(V_(11mA)<3V／mm)、介电常数非常高(ε>00000)的纳米改性SrTiO_3基双功能陶瓷，同时有效地降低烧结温度，拓宽烧结温度范围(1360℃～1420℃烧成)。
SrTiO3 based dual-functional ceramics were fabricated by the single-fired method and the varistor characteristics and dielectric properties of the materials were investigated in this paper.
The samples were firstly fired at 1420C for 2.5h in a N2+C reducing atmosphere to obtain good semiconducting sintered specimens, then cooled to 1180C , at this temperature heat treatment was carried out for 20min in the oxygen atmosphere so as that grain boundaries were insulated. The experiment results show that the kinds of donor ions and dopant concentration, the kinds of acceptor ions, and firing temperature have significant influence on the microstructure and electrical properties.
The SrTiO3 based dual-functional ceramics with La2O3+Nb2O5 as double donors or La2O3 as single donor and doped MnCO3 or CuO as acceptor, exhibit lower varistor and higher dielectric constant characteristics, respectively. Comparatively, the samples doped La2O3 as single donor and CuO as acceptor have superiority on lower varistor voltage (V1mA<10V/mm) and higher dielectric constant ( >0000) . The samples doped La2O3+Nb2O5 as donors and doped MnCO3 as acceptor have advantage of high nonlinear coefficient ( a >8) and wider firing temperature.
Nano-scaled La2O3 were prepared by organic chelate precursor technology, and nano-scaled composite Si-Al-Mn and Si-Al-Cu synthesized by chemical precipitation method. The as-prepared La2O3, Si-Al-Mn and Si-Al-Cu were doped into SrTiO3 as dopant, to improve the sintering characteristics and optimizing electrical properties. The results show that SrTiO3 based dual-functional ceramics doped by nano-dopant with much lower varistor voltage (V1mA<3V/mm) and much higher dielectric constant ( >00000 ) can be obtained by using optimal ingredients and technology. Meanwhile, nano-dopant can effectively decrease the sintering temperature and widen the range of the sintering temperature(1360C~1420C).
试样首先在N_2+C弱还原气氛中于1420℃保温2.5h烧成，获得良好的半导化SrTiO_3烧结体，然后随炉冷却至1180℃，通氧气进行保温热处理20min，使晶界绝缘化。实验表明：掺杂施主离子的种类及浓度、掺杂受主离子的种类、烧结温度等因素均对微观结构、电性能产生重要影响。双施主La_2O_3+Nb_2O_5掺杂、单施主La_2O_3掺杂，分别以MnCO_3和CuO为受主掺杂均能获得低压敏电压兼高介电常数的SrTiO_3基双功能陶瓷，表现出良好的压敏性能与介电性能。相比较而言，单施主La_2O_3掺杂以CuO为受主的试样具有较低压敏电压(V_(1mA)<10V／mm)、高介电常数(ε>0000)的优势；双施主La_2O_3+Nb_2O_5掺杂以MnCO_3为受主的试样具有非线性高(α>8)、烧结温度宽的特点。
为了改善材料烧结性和优化电性能，采用有机配合物前驱体法制备La_2O_3施主掺杂剂的纳米粉体，采用化学共沉淀法分别制备Si-Al-Mn、Si-Al-Cu受主掺杂剂及助溶剂复合纳米粉体，对SrTiO_3进行纳米掺杂改性。结果表明：采用合理的配方及工艺可获得压敏电压极低(V_(11mA)<3V／mm)、介电常数非常高(ε>00000)的纳米改性SrTiO_3基双功能陶瓷，同时有效地降低烧结温度，拓宽烧结温度范围(1360℃～1420℃烧成)。
SrTiO3 based dual-functional ceramics were fabricated by the single-fired method and the varistor characteristics and dielectric properties of the materials were investigated in this paper.
The samples were firstly fired at 1420C for 2.5h in a N2+C reducing atmosphere to obtain good semiconducting sintered specimens, then cooled to 1180C , at this temperature heat treatment was carried out for 20min in the oxygen atmosphere so as that grain boundaries were insulated. The experiment results show that the kinds of donor ions and dopant concentration, the kinds of acceptor ions, and firing temperature have significant influence on the microstructure and electrical properties.
The SrTiO3 based dual-functional ceramics with La2O3+Nb2O5 as double donors or La2O3 as single donor and doped MnCO3 or CuO as acceptor, exhibit lower varistor and higher dielectric constant characteristics, respectively. Comparatively, the samples doped La2O3 as single donor and CuO as acceptor have superiority on lower varistor voltage (V1mA<10V/mm) and higher dielectric constant ( >0000) . The samples doped La2O3+Nb2O5 as donors and doped MnCO3 as acceptor have advantage of high nonlinear coefficient ( a >8) and wider firing temperature.
Nano-scaled La2O3 were prepared by organic chelate precursor technology, and nano-scaled composite Si-Al-Mn and Si-Al-Cu synthesized by chemical precipitation method. The as-prepared La2O3, Si-Al-Mn and Si-Al-Cu were doped into SrTiO3 as dopant, to improve the sintering characteristics and optimizing electrical properties. The results show that SrTiO3 based dual-functional ceramics doped by nano-dopant with much lower varistor voltage (V1mA<3V/mm) and much higher dielectric constant ( >00000 ) can be obtained by using optimal ingredients and technology. Meanwhile, nano-dopant can effectively decrease the sintering temperature and widen the range of the sintering temperature(1360C~1420C).
引文
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[6] 张立德，纳米材料研究的新进展在21世纪的战略地位，中国粉体技术，2000，6(1)：1
[7] 白春礼，中国纳米科技研究的现状及思考，物理，2002，31(2)：65-70
[8] 翟华嶂，李建保，黄勇等，纳米材料和纳米科技的进展、应用及产业化现状，材料工程，2001(11)：43-48
[9] 周竹发，纳米材料与陶瓷，江苏陶瓷，2002，35(1)：1-3
[10] Tapan K.Gupta, J.Am.Geram.soc.,1990, 73 (7): 1817-1840
[11] W.Y. Wang.,D.F. Zhang,T. Xu,et al, Nonlinear electrical characteristics and dielectric properties of Ca, Ta-doped TiO_2 varistors, Appl.Phys., 2003, 76(A): 71-75
[12] Yang Seng-Lu, Wu Jenn-Ming, Novel niobium-doped titania varistor with added barium and bismuth, J.Am.Ceram. Soc.,1993, 76(1): 145-152
[13] L.M. Lionel, H.R.Philipp, Zinc oxide varistors-a review, Ceram. Bull, 1986,65(4): 639-646
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[15] T.K. Gupta, Application of zinc oxide varistors, J. Am. Ceram. Sot., 1990, 73(7): 1817-1840
[16] 王豫，胡一帆，碳化硅压敏电阻非线性机理研究，功能材料，1995，26(6)：521-523
[17] T.R.N.Kutty, V.Ravi, Varistors based on n- BaTiO_3 ceramics, Materials Science and Engineering, 1993, B20:271-279
[18] (美)田增英主编，《来自西方的知识，精密陶瓷及应用》，科学普及出版社，1993
[19] N.Yamaoka and M. Masuyama, SrTiO_3-based boundary layer capacitors have varistor characteristics, J. Am. Ceram.Soc., 1983,2(6): 698-703
[20] 龙香楷，高非线性指数的压敏瓷，电子元件与材料，2002，21(7)：19-20
[21] 张丛春，周东祥等，Sb_2O_3掺杂对ZnO压敏陶瓷晶界特性和电性能的影响，硅酸盐学报，2001，29(6)：602-605
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