稀土改性ZnO导电陶瓷粉的制备
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摘要
本文分别采用溶胶-凝胶法和沉淀法制备了ZnO粉体，确定了粉体制备的工艺条件；对ZnO粉体进行了La、Pr气相扩渗，制备了新型ZnO导电粉；对稀土气相扩渗后ZnO粉体的组成、结构和导电性能的变化进行了研究。
溶胶-凝胶法制备ZnO粉体的工艺条件：室温，搅拌3h，煅烧温度840℃，烧结制度为200℃保温1h，400℃保温2h，840℃保温1h。沉淀法制备ZnO粉体的工艺条件：分步洗涤，滴速80滴／min，煅烧温度200℃。与溶胶-凝胶法相比，沉淀法制备出的ZnO粉体粒度分布均匀，粒径较小，在100nm左右。
对所制备的纳米ZnO粉体进行了La、Pr气相扩渗，实验结果表明，La、Pr扩渗能明显改善ZnO粉体的导电性能。当La的扩渗浓度为2％(wt)，扩渗时间为4h，扩渗温度为420℃时，改性ZnO的室温电阻率最低，由扩渗前的10~(14)Ω·cm下降到1.6×10~6Ω·cm；当Pr的扩渗浓度为2％(wt)，扩渗时间为4h，扩渗温度为400℃时，改性ZnO的室温电阻率最低，由扩渗前的10~(14)Ω·cm下降到1.9×10~6Ω·cm。
XRD测试表明，经过La、Pr气相扩渗，ZnO粉体的主体特征峰没有明显变化，但分别在29.5°和30.5°出现了与稀土有关的特征峰，说明La、Pr渗入了ZnO粉体，并导致了ZnO粉体导电性的提高。SEM测试表明ZnO粉体经稀土La、Pr扩渗后晶粒明显细化，团聚现象减弱。热重分析表明La扩渗后的ZnO粉体具有较好的热稳定性，有良好的应用前景。
ZnO powders were prepared by sol-gel method and precipitation method. The preparation parameters for ZnO powders were studied. ZnO conductive powders were penetrated by gaseous penetration of La and Pr in gaseous state. The composition, structure and electric conductivity of ZnO powders were studied.
The preparation parameters of ZnO powders by sol-gel method: room temperature, stirring 3h, sintering at 840°C, sintering 1h at 200°C, 2h at 400°C, and 1h at 400°C. The process parameters of precipitation method are: sequential washing, 80 drops/min, sintering at 200°C. ZnO powders prepared by precipitation method are uniform. The grain size is about 100nm, which is smaller than that of ZnO powders prepared by sol-gel method.
ZnO conductive powders were prepared by gaseous penetration of La and Pr in gaseous state. Experiment results show that La and Pr can evidently improve the electric conductivity of ZnO powders. When the La content is 2%(wt), the penetration time is 4h, the penetration temperature is 420°C, the resistivity of modified ZnO powders is lowest, which decreased from 10~(14)Ω·cm to 1.6×10~6Ω·cm. When the Pr content is 2%(wt), the penetration time is 4h, the penetration temperature is 400°C, the resistivity of modified ZnO powders is lowest, which decreased from 10~(14)Ω·cm to 1.9×10~6Ω·cm.
XRD analysis show that, after gaseous penetration of La and Pr in gaseous state, the main peaks of ZnO powders did not change, but there are two small peaks at 29.5° and 30.5°, which are relating to La and Pr. It indicated that La and Pr have penetrated into ZnO powders and leaded to the increase in electric conductivity. SEM results show that, after gaseous penetration, grains of the powders are refined evidently and agglomeration behavior is decreased. Thermogravimetric analysis show that ZnO powders penetrated by La has good thermal stability, which has a good application in the future.
溶胶-凝胶法制备ZnO粉体的工艺条件：室温，搅拌3h，煅烧温度840℃，烧结制度为200℃保温1h，400℃保温2h，840℃保温1h。沉淀法制备ZnO粉体的工艺条件：分步洗涤，滴速80滴／min，煅烧温度200℃。与溶胶-凝胶法相比，沉淀法制备出的ZnO粉体粒度分布均匀，粒径较小，在100nm左右。
对所制备的纳米ZnO粉体进行了La、Pr气相扩渗，实验结果表明，La、Pr扩渗能明显改善ZnO粉体的导电性能。当La的扩渗浓度为2％(wt)，扩渗时间为4h，扩渗温度为420℃时，改性ZnO的室温电阻率最低，由扩渗前的10~(14)Ω·cm下降到1.6×10~6Ω·cm；当Pr的扩渗浓度为2％(wt)，扩渗时间为4h，扩渗温度为400℃时，改性ZnO的室温电阻率最低，由扩渗前的10~(14)Ω·cm下降到1.9×10~6Ω·cm。
XRD测试表明，经过La、Pr气相扩渗，ZnO粉体的主体特征峰没有明显变化，但分别在29.5°和30.5°出现了与稀土有关的特征峰，说明La、Pr渗入了ZnO粉体，并导致了ZnO粉体导电性的提高。SEM测试表明ZnO粉体经稀土La、Pr扩渗后晶粒明显细化，团聚现象减弱。热重分析表明La扩渗后的ZnO粉体具有较好的热稳定性，有良好的应用前景。
ZnO powders were prepared by sol-gel method and precipitation method. The preparation parameters for ZnO powders were studied. ZnO conductive powders were penetrated by gaseous penetration of La and Pr in gaseous state. The composition, structure and electric conductivity of ZnO powders were studied.
The preparation parameters of ZnO powders by sol-gel method: room temperature, stirring 3h, sintering at 840°C, sintering 1h at 200°C, 2h at 400°C, and 1h at 400°C. The process parameters of precipitation method are: sequential washing, 80 drops/min, sintering at 200°C. ZnO powders prepared by precipitation method are uniform. The grain size is about 100nm, which is smaller than that of ZnO powders prepared by sol-gel method.
ZnO conductive powders were prepared by gaseous penetration of La and Pr in gaseous state. Experiment results show that La and Pr can evidently improve the electric conductivity of ZnO powders. When the La content is 2%(wt), the penetration time is 4h, the penetration temperature is 420°C, the resistivity of modified ZnO powders is lowest, which decreased from 10~(14)Ω·cm to 1.6×10~6Ω·cm. When the Pr content is 2%(wt), the penetration time is 4h, the penetration temperature is 400°C, the resistivity of modified ZnO powders is lowest, which decreased from 10~(14)Ω·cm to 1.9×10~6Ω·cm.
XRD analysis show that, after gaseous penetration of La and Pr in gaseous state, the main peaks of ZnO powders did not change, but there are two small peaks at 29.5° and 30.5°, which are relating to La and Pr. It indicated that La and Pr have penetrated into ZnO powders and leaded to the increase in electric conductivity. SEM results show that, after gaseous penetration, grains of the powders are refined evidently and agglomeration behavior is decreased. Thermogravimetric analysis show that ZnO powders penetrated by La has good thermal stability, which has a good application in the future.
引文
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2 刘艳，田胜军，李海娜．导电粉的市场及研究开发现状．湿法冶金．2004，(3)：1～5
3 董晓红．导电聚合物．中国化工百科全书．化学工业出社．1997：55～61
4 Maki, Seiichi, Takemoto, et al. Semi-conductive powder for cabke ciatubg. Wire Journal International. 1981,14(11):86～91
5 杜仕国．电磁屏蔽材料的现状与发展．化工新型材料．1995，(4)：12～16
6 杨丽梅．导电云母粉的制法及其应用．涂料工业．1998，(11)：19～21
7 H.T. Okabe, Oh Yeon Lee, Chuel Ro Lee, et al. Semi-continuous production of tantalum powder by electronically mediated reaction (EMR). Materials Transactions. 2002,43(8):2080～2086
8 胡春艳，王树根，贾桂芹．棉织物纳米材料防电磁波辐射整理剂的研究．印染助剂．2005，22(8)：25～27
9 郝素娥，韦永德．Sm对PbTiO_3陶瓷的气相扩渗及其电性能研究．压电与声光．2004，26(4)：312～314
10 郝素娥，孙亮，黄金祥．稀土气相扩渗BaTiO_3基PTC陶瓷的NTCR效应．高等学校化学学报．2005，26(12)：2207～2210
11 郝素娥，韦永德．Sm对BaTiO_3陶瓷的气相扩渗及其电性能．材料科学与工艺．2004，12(3)：261～264
12 马宏文，矫立男，杨雪．固相法合成纳米ZnO及其光催化性能研究．化学与生物工程．2006，26(4)：17～21
13 边继明，李效民，赵俊亮．PLD法生长高质量ZnO薄膜及其光电导特性研究．无机材料学报．2006，26(5)：701～706
14 Osada, Takenor, Okato, et al. Fabrication and characterization of hexagonally assembled ZnO and ZnO:N thin films with buffer layer by pulsed-laser deposition. Proceedings of SPIE. The International Society for Optical Engineering. 2005, (6): 319～326
15 马建军，徐光亮．氧化锌压敏电阻粉体的制备工艺．中国粉体技术．2004，(2)：29～35
16 袁方利，黄淑兰，凌远兵．等离子法热解制备导电ZnO陶瓷粉．化工冶金．1998，19(3)：212～216
17 任文娥，于钦学，刘辅宜．氧化锌半导电粉料的研究．电瓷避雷器．1999，(2)：40～44
18 刘宇，许启明，刘珊．氧化锌半导体材料的性能研究与制备进展．无机盐工业．2006，(3)：3～6
19 S. Choopun, R. D. Vispute, W. Noch, et al. Oxygen pressure-tuned epitaxy and optoelectronic properties of laser-deposited ZnO films on sapphire. Applied Physics Letters. 1999, (75):3947
20 王凯，周祚万，刘菁菁．一维纳米结构ZnO掺杂的研究进展．材料科学与工程学报．2006，26(3)：471～476
21 刘学超，施尔畏，宋力昕．固相反应法制备Co掺杂ZnO的磁性和光学性能研究．物理学报．2006，55(5)：2557～2561
22 陈仕国，戈早川．聚合物／碳黑气敏导电复合材料的研究进展．工程塑料应用．2006，34(3)：65～68
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