纳米晶氧化锆陶瓷的制备及性能研究
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摘要
本研究比较系统地研究了纳米氧化锆陶瓷的合成与成型机理，特别是讨论了纳米氧化锆陶瓷的稳定性，为防止纳米颗粒在外场作用下的团聚和长大提供了理论基础和实验数据，具体工作有以下几方面：
(1)采用共沉淀法和共沉淀-凝胶法制备了纳米氧化锆粉体，并分析了pH值和稳定剂含量对粉体性能的影响；(2)采用新型无压烧结工艺制备了纳米氧化锆陶瓷，并分析了成型压力和烧结温度对烧结体性能的影响；(3)采用低温无压烧结工艺制备出添加纳米铜的功能性纳米氧化锆复合陶瓷，并分析了烧结体的微观尺度和电学性能的变化以及影响因素；(4)通过自创的“鸡蛋清外敷法”在真空镀膜台上对纳米氧化锆粉体(团)进行包敷碳颗粒(团)的表面处理，并采用真空烧结工艺制得相应烧结体，初步开始解决陶瓷烧结过程中团聚长大这一传统难题；(5)通过分析纳米颗粒在制备烧结体过程中的实际特点，提出了“三球烧结数学模型”，通过引入坯体相对密度和孔隙率的相对关系分析并通过自行编写的数学拟合软件，验证了这一数学模型。
This dissertation scrutinizingly discusses the synthesis and molding mechanism in detail, especially the stability of nano crystalline zirconia ceramics, provides some comprehensive theoretical basis and experiment data about aggregation control of nano particulate materials under the effect of outfield. The mian works are as follows:
(1)By coprecipitation technique and coprecipitation- gel technique the nano zirconia powder was produced, factors affecting the properties of nano zirconia powder such as pH and the content of stabilizator are analyzed;(2)By the new pressless sintering process, the nano zirconia ceramic was produced, factors which can affecting the properties of nano zirconia sinter body such as moulding press and the sinter temperature are analyzed;(3)By the microtherm pressless sintering process, the nano copper added functional zirconia ceramic composite was produced, microscopic dimensionality and electric properties of such sinter body and the factors affecting such sinter body are analyzed;(4)By the self-invented "external albumen coating" technique the zirconia powder (group) was successfully coated by carbon in the corresponding sinter body, which can help solve the traditional aggregation problem to some degree;(5)Based on analyze the characteristics in the nano powder sinter process, the "three-ball sinter model" w
as proposed, for the relationship between the relative density and porosity of sinter body, by mathematical fitting, such model was successfully verified.
(1)采用共沉淀法和共沉淀-凝胶法制备了纳米氧化锆粉体，并分析了pH值和稳定剂含量对粉体性能的影响；(2)采用新型无压烧结工艺制备了纳米氧化锆陶瓷，并分析了成型压力和烧结温度对烧结体性能的影响；(3)采用低温无压烧结工艺制备出添加纳米铜的功能性纳米氧化锆复合陶瓷，并分析了烧结体的微观尺度和电学性能的变化以及影响因素；(4)通过自创的“鸡蛋清外敷法”在真空镀膜台上对纳米氧化锆粉体(团)进行包敷碳颗粒(团)的表面处理，并采用真空烧结工艺制得相应烧结体，初步开始解决陶瓷烧结过程中团聚长大这一传统难题；(5)通过分析纳米颗粒在制备烧结体过程中的实际特点，提出了“三球烧结数学模型”，通过引入坯体相对密度和孔隙率的相对关系分析并通过自行编写的数学拟合软件，验证了这一数学模型。
This dissertation scrutinizingly discusses the synthesis and molding mechanism in detail, especially the stability of nano crystalline zirconia ceramics, provides some comprehensive theoretical basis and experiment data about aggregation control of nano particulate materials under the effect of outfield. The mian works are as follows:
(1)By coprecipitation technique and coprecipitation- gel technique the nano zirconia powder was produced, factors affecting the properties of nano zirconia powder such as pH and the content of stabilizator are analyzed;(2)By the new pressless sintering process, the nano zirconia ceramic was produced, factors which can affecting the properties of nano zirconia sinter body such as moulding press and the sinter temperature are analyzed;(3)By the microtherm pressless sintering process, the nano copper added functional zirconia ceramic composite was produced, microscopic dimensionality and electric properties of such sinter body and the factors affecting such sinter body are analyzed;(4)By the self-invented "external albumen coating" technique the zirconia powder (group) was successfully coated by carbon in the corresponding sinter body, which can help solve the traditional aggregation problem to some degree;(5)Based on analyze the characteristics in the nano powder sinter process, the "three-ball sinter model" w
as proposed, for the relationship between the relative density and porosity of sinter body, by mathematical fitting, such model was successfully verified.
引文
[1] M.D.Lechner etc. Material Science Forum 352,2000:87-90
[2] 王零森 陶瓷工程 31，1997：43
[3] S.C.Carniglia J. Am. Ceram. Soc 55,1972:243
[4] L.Radonjic Materials Science Forum 282-283,1999:11-18
[5] 陆厚根 粉体工程导论 同济大学出版社 1993
[6] 硅酸盐物理化学 浙江大学 1997
[7] E.Ivanov Materials Science Forum 88-90,1992:475
[8]J.L.Katz etc. Nanostructured Material 4,1994:511
[9]T. Ikemoto etc. J.Material. Science. Japan 93,1985:585
[10]J.Ding etc. J.Am.Ceramic. Soc 79,1996:2956
[11]D.Vollath etc. Nanostructured Material 1,1992:427
[12]I.W. Chen etc. J.Am. Ceramic. Soc 33,1989:223
[13]T.C.Chou etc. Thin Solid Films 205,1991:131
[14]王义华 硕士论文：纳米Al_2O_3的尺寸效应 中国科技大学 1993
[15]G. Gaggoiotti etc. Sensor and Actuators B24-25,1995:516
[16]谢玉群 材料研究学报 Vol．14 增刊，2000：45-48
[17]N.Yamazde etc. Surface Science 86,1995:335
[18]王昕等 复合材料学报 16(1)1999：105-111
[19]王昕等 复合材料学报 16(3)1999：83-86
[20]徐跃萍 博士论文：氧化锆陶瓷的超细粉末制备、烧结动力学及显微结构的研究 中科院上海硅酸盐研究所 1991
[21]李蔚 博士论文：纳米氧化锆粉体制备与纳米氧化锆材料烧结的研究 中科院上海硅所 1999
[22]孟国文 博士论文：ZrO_2基纳米粉体及陶瓷的制备工艺研究 西北工业大学 1996
[23]物理化学第三版 天津大学出版社 1995
[24]M.J.Ready etc. J.Am.Ceramic. Soc 73,1990:1499
[25]S.L.Jonesetc. J.Am. Ceramic. Soc 71,1988:C190
[26]D.J.Chen etc. Nanostructured Material 2,1993:469
[27]M.J.Mayo International Materials Reviews 41,1996:85
[28]Joanna R.Groza NanoStructured Materials 12,1999:987-992
[29]L.P. Ferroni etc. Nanotecnology 10,1999:90-96
[30]G.S.A.M.Theunissen etc. J.Eur. Ceram. Soc. 11,1993:315
[31]古堂生 博士论文：纳米氧化物微结构特征与晶粒生长行为的研究 中山大学 1999
[32]M.F. Yan Material Science& Engineering 48,1981:58
[33]U.Betz etc. NanoStructured Materials 12,1999:689-692
[34]R. Vaben etc. Advanced in Powder Metallurgy and Particulate Materials vol 17,Princeton NJ. 1992:19
[35]G. Skandan Nanostructional Materials 5,1995:111
[36]S.L.Hwang etc. J. Am. Ceram. Soc. 73,1990:3269
[37]P. Merkert etc. NanoStructured Materials 12,1999:689-692
[38]C.D.Sagel-Ransijn etc. J.Eur. Ceram. Soc 17,1997:1133
[39]I.W. Chen etc. J.Am. Ceram. Soc. 73,1990:3269
[40]U.Betz etc. NanoStructured Materials 12,1999:911-914
[41]原效坤 许并社 Cryic Synthesize Mechanism and Properties of Nano Functional Compound Zirconia Ceramic (在投)
[42]J.R.Groza NanoStructured Materials 12,1999:987-992
[43]L.Radonjic Materials Science Forum 282-283,1999:11-18
[44]Hu,Yue Ph.D Thesis:Synthesis and Evaluation of Novel Polymer-Coated Zirconia as Reversed and Ion-Exchange Stationary Phases University of Minnesota 1999
[45]Zhao,JianHong Ph.D Thesis:Synthesis,Evaluation,Application and Modification of a Novel Aromatic Polymer-Coated Zirconia HPLC Support University of Minnesota 2000
[46]邵忠财 无机材料学报 14(3)，1999：397-401
[47]J.Fitz-Gerald etc. NanoStructured Materials 12,1999:1167-1171
[48]原效坤 许并社 全国第二届纳米技术和应用会议 2000：C83-85
[49]W.B.David C.C.Barry Transmission Electron Microscopy(Ⅰ) Plenum Press Newyork 1996
[50]Quan Xuejun etc. China Powder Science and Technology 6(6),2000:14-20
[51]F.F. Lange etc, J.cm. Ceram. Soc. 72,1989:735
[52]B.J.Kellet etc. J.cm. Ceram. Soc. 72,1989:725
[53]R.J.Cobel J.Appl.Phys 41,1970:4978
[54]J.D.Mcclell J.Am. Ceram. Soc. 44,1961:526
[55]R.J.Cobel etc. J.Am.Ceramic. Soc. 46,1964:438
[56]H.E.Exner Rev. Powder Meter. Phys.Ceram. 1,1979:7
[57]R.J.Cobel ibid. 36,1965:2327
[2] 王零森 陶瓷工程 31，1997：43
[3] S.C.Carniglia J. Am. Ceram. Soc 55,1972:243
[4] L.Radonjic Materials Science Forum 282-283,1999:11-18
[5] 陆厚根 粉体工程导论 同济大学出版社 1993
[6] 硅酸盐物理化学 浙江大学 1997
[7] E.Ivanov Materials Science Forum 88-90,1992:475
[8]J.L.Katz etc. Nanostructured Material 4,1994:511
[9]T. Ikemoto etc. J.Material. Science. Japan 93,1985:585
[10]J.Ding etc. J.Am.Ceramic. Soc 79,1996:2956
[11]D.Vollath etc. Nanostructured Material 1,1992:427
[12]I.W. Chen etc. J.Am. Ceramic. Soc 33,1989:223
[13]T.C.Chou etc. Thin Solid Films 205,1991:131
[14]王义华 硕士论文：纳米Al_2O_3的尺寸效应 中国科技大学 1993
[15]G. Gaggoiotti etc. Sensor and Actuators B24-25,1995:516
[16]谢玉群 材料研究学报 Vol．14 增刊，2000：45-48
[17]N.Yamazde etc. Surface Science 86,1995:335
[18]王昕等 复合材料学报 16(1)1999：105-111
[19]王昕等 复合材料学报 16(3)1999：83-86
[20]徐跃萍 博士论文：氧化锆陶瓷的超细粉末制备、烧结动力学及显微结构的研究 中科院上海硅酸盐研究所 1991
[21]李蔚 博士论文：纳米氧化锆粉体制备与纳米氧化锆材料烧结的研究 中科院上海硅所 1999
[22]孟国文 博士论文：ZrO_2基纳米粉体及陶瓷的制备工艺研究 西北工业大学 1996
[23]物理化学第三版 天津大学出版社 1995
[24]M.J.Ready etc. J.Am.Ceramic. Soc 73,1990:1499
[25]S.L.Jonesetc. J.Am. Ceramic. Soc 71,1988:C190
[26]D.J.Chen etc. Nanostructured Material 2,1993:469
[27]M.J.Mayo International Materials Reviews 41,1996:85
[28]Joanna R.Groza NanoStructured Materials 12,1999:987-992
[29]L.P. Ferroni etc. Nanotecnology 10,1999:90-96
[30]G.S.A.M.Theunissen etc. J.Eur. Ceram. Soc. 11,1993:315
[31]古堂生 博士论文：纳米氧化物微结构特征与晶粒生长行为的研究 中山大学 1999
[32]M.F. Yan Material Science& Engineering 48,1981:58
[33]U.Betz etc. NanoStructured Materials 12,1999:689-692
[34]R. Vaben etc. Advanced in Powder Metallurgy and Particulate Materials vol 17,Princeton NJ. 1992:19
[35]G. Skandan Nanostructional Materials 5,1995:111
[36]S.L.Hwang etc. J. Am. Ceram. Soc. 73,1990:3269
[37]P. Merkert etc. NanoStructured Materials 12,1999:689-692
[38]C.D.Sagel-Ransijn etc. J.Eur. Ceram. Soc 17,1997:1133
[39]I.W. Chen etc. J.Am. Ceram. Soc. 73,1990:3269
[40]U.Betz etc. NanoStructured Materials 12,1999:911-914
[41]原效坤 许并社 Cryic Synthesize Mechanism and Properties of Nano Functional Compound Zirconia Ceramic (在投)
[42]J.R.Groza NanoStructured Materials 12,1999:987-992
[43]L.Radonjic Materials Science Forum 282-283,1999:11-18
[44]Hu,Yue Ph.D Thesis:Synthesis and Evaluation of Novel Polymer-Coated Zirconia as Reversed and Ion-Exchange Stationary Phases University of Minnesota 1999
[45]Zhao,JianHong Ph.D Thesis:Synthesis,Evaluation,Application and Modification of a Novel Aromatic Polymer-Coated Zirconia HPLC Support University of Minnesota 2000
[46]邵忠财 无机材料学报 14(3)，1999：397-401
[47]J.Fitz-Gerald etc. NanoStructured Materials 12,1999:1167-1171
[48]原效坤 许并社 全国第二届纳米技术和应用会议 2000：C83-85
[49]W.B.David C.C.Barry Transmission Electron Microscopy(Ⅰ) Plenum Press Newyork 1996
[50]Quan Xuejun etc. China Powder Science and Technology 6(6),2000:14-20
[51]F.F. Lange etc, J.cm. Ceram. Soc. 72,1989:735
[52]B.J.Kellet etc. J.cm. Ceram. Soc. 72,1989:725
[53]R.J.Cobel J.Appl.Phys 41,1970:4978
[54]J.D.Mcclell J.Am. Ceram. Soc. 44,1961:526
[55]R.J.Cobel etc. J.Am.Ceramic. Soc. 46,1964:438
[56]H.E.Exner Rev. Powder Meter. Phys.Ceram. 1,1979:7
[57]R.J.Cobel ibid. 36,1965:2327
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