改性AZO粉体的制备及其在导电胶中的应用
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摘要
采用共沉淀法制备了AZO粉体,对所制备的AZO粉体进行了稀土La的气相扩渗改性,对改性前后AZO粉体的组成、结构和导电性能的变化进行了研究;并将改性AZO粉体应用于导电胶的制备,对所制备的导电胶的力学性能和导电性能进行了研究。
共沉淀法制备AZO粉体的工艺条件为:反应温度50℃,反应溶液pH=7,烘干温度150℃,烘干时间10h,焙烧温度500℃,焙烧时间2h。采用共沉淀法制备出的AZO粉体粒度分布均匀,粒径较小,可以达到纳米级别,电阻率为4.24×107? cm。稀土La气相扩渗能进一步改善AZO粉体的导电性能。正交实验结果表明,当Al掺杂浓度为3.0wt%、La扩渗浓度为2wt%、扩渗温度为480℃、扩渗时间为5h时,改性AZO粉体的室温电阻率为1.37×104? cm。扩渗前后粉体的电阻率下降了3个数量级。XRD测试结果表明,改性AZO粉体和ZnO粉体相对比,主体特征峰没有明显变化,但分别在11o和68.5o出现了与La有关的特征峰。SEM测试表明AZO粉体经稀土La扩渗后有大的晶粒出现,存在明显的团聚现象。EDAX测试结果表明La已进入AZO粉体,并导致导电性能的提高。
以所制备的改性AZO粉体为导电填料,不饱和聚酯树脂为基体制备了导电胶。当固化剂和促进剂的添加量为2wt%时,所制备出的样品表面平整无龟裂现象,反应速度适中。制备出的导电胶的电阻率最低值为5.3×105? cm。随着改性AZO粉体添加量的增加,剪切强度逐渐变小,冲击强度逐渐增大。当改性AZO粉体添加量为40wt%时,剪切强度为11.48MPa,冲击强度为19.6kJ m-2,满足应用要求。
AZO powders were prepared by co-precipitation method. After that gaseous penetration of rare-earth element La was carried out to modify the AZO powders. The composition, structure and conductivity after modification were studied. The AZO powders were applied to the preparation of conductive glues. The mechanical and conductive properties of the prepared glues were investigated.
The method to prepare the AZO powders by co-precipitation was that the reaction time was 50℃, the pH value of the solution was 7, the drying temperature was 150℃, drying time was 10h, the calcinations temperature was 500℃and calcinations time was 2h. The AZO powders prepared through co-precipitation exhibited an even distribution of grain size, which could reach nanometer scale. The resistivity of such powder was 4.24×107? cm. Modifying such powder with La by gaseous penetration could further improve the conductivity of AZO powders. The results of orthogonal experiment showed that the resistivity of modified AZO powders reach 1.37×104? cm when Al doping content is 3.0wt%, La doping content was 2.0wt%, penetration temperature was 480℃and penetration time is 5h. The resistivity after penetration dropped three orders of magnitude. XRD results showed that, compared with ZnO powders, the main peaks of modified AZO powders showed no obvious difference, but new peaks at 11o and 68.5o, which were related to La element. SEM results showed that there were large grains and obvious agglomeration after La penetration into AZO powders. EDAX results showed that La entered AZO and rendered the improvement of conductivity.
Conductive glues were prepared with the prepared AZO powders as conductive fillings and unsaturated polyester resin as matrix. When the additive amount of curing agent and accelerant are 2wt%, the surface of samples prepared was smooth and free of cracks, and the reaction speed was moderate. The resistivity reached the lowest point of 5.3×105? cm. As the additive amount of modified AZO powders increased, the shear strength gradually decreased and the impact strength gradually increased. When the additive amount of modified AZO powders was 40wt%, the shear strength was 11.48MPa and the impact strength was 19.6kJ m-2, which could meet the need of application.
共沉淀法制备AZO粉体的工艺条件为:反应温度50℃,反应溶液pH=7,烘干温度150℃,烘干时间10h,焙烧温度500℃,焙烧时间2h。采用共沉淀法制备出的AZO粉体粒度分布均匀,粒径较小,可以达到纳米级别,电阻率为4.24×107? cm。稀土La气相扩渗能进一步改善AZO粉体的导电性能。正交实验结果表明,当Al掺杂浓度为3.0wt%、La扩渗浓度为2wt%、扩渗温度为480℃、扩渗时间为5h时,改性AZO粉体的室温电阻率为1.37×104? cm。扩渗前后粉体的电阻率下降了3个数量级。XRD测试结果表明,改性AZO粉体和ZnO粉体相对比,主体特征峰没有明显变化,但分别在11o和68.5o出现了与La有关的特征峰。SEM测试表明AZO粉体经稀土La扩渗后有大的晶粒出现,存在明显的团聚现象。EDAX测试结果表明La已进入AZO粉体,并导致导电性能的提高。
以所制备的改性AZO粉体为导电填料,不饱和聚酯树脂为基体制备了导电胶。当固化剂和促进剂的添加量为2wt%时,所制备出的样品表面平整无龟裂现象,反应速度适中。制备出的导电胶的电阻率最低值为5.3×105? cm。随着改性AZO粉体添加量的增加,剪切强度逐渐变小,冲击强度逐渐增大。当改性AZO粉体添加量为40wt%时,剪切强度为11.48MPa,冲击强度为19.6kJ m-2,满足应用要求。
AZO powders were prepared by co-precipitation method. After that gaseous penetration of rare-earth element La was carried out to modify the AZO powders. The composition, structure and conductivity after modification were studied. The AZO powders were applied to the preparation of conductive glues. The mechanical and conductive properties of the prepared glues were investigated.
The method to prepare the AZO powders by co-precipitation was that the reaction time was 50℃, the pH value of the solution was 7, the drying temperature was 150℃, drying time was 10h, the calcinations temperature was 500℃and calcinations time was 2h. The AZO powders prepared through co-precipitation exhibited an even distribution of grain size, which could reach nanometer scale. The resistivity of such powder was 4.24×107? cm. Modifying such powder with La by gaseous penetration could further improve the conductivity of AZO powders. The results of orthogonal experiment showed that the resistivity of modified AZO powders reach 1.37×104? cm when Al doping content is 3.0wt%, La doping content was 2.0wt%, penetration temperature was 480℃and penetration time is 5h. The resistivity after penetration dropped three orders of magnitude. XRD results showed that, compared with ZnO powders, the main peaks of modified AZO powders showed no obvious difference, but new peaks at 11o and 68.5o, which were related to La element. SEM results showed that there were large grains and obvious agglomeration after La penetration into AZO powders. EDAX results showed that La entered AZO and rendered the improvement of conductivity.
Conductive glues were prepared with the prepared AZO powders as conductive fillings and unsaturated polyester resin as matrix. When the additive amount of curing agent and accelerant are 2wt%, the surface of samples prepared was smooth and free of cracks, and the reaction speed was moderate. The resistivity reached the lowest point of 5.3×105? cm. As the additive amount of modified AZO powders increased, the shear strength gradually decreased and the impact strength gradually increased. When the additive amount of modified AZO powders was 40wt%, the shear strength was 11.48MPa and the impact strength was 19.6kJ m-2, which could meet the need of application.
引文
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3 M. Bouguettaya, N. Vedie and C. Cherrot. New Conductive Adhesives for Surface Mount Solder Replacemen. Synthetic Metals, 1999,(102):1428~1431
4 H. K. Kim, F. G. Shi. Electrical Reliability of Electrically Conductive Adhesive Joints:Dependence on Curing Condition and Current Density Microelectronics Joumal. 2001,(32):315~321
5 M. Mizuno, M. Saka and H. Abe. Mechanism of Clectrical Conduction though Ansotropically Conductive Adhesive films. IEEE Transactions on CPMT-Part A. 1996,194:546~553
6田民波.电子封装中的无铅化.印制电路信息. 2002,(10):3~10
7 M. Kitajima, T. Shono. Department of the Tin-Zinc-Aluminum (Sn-Zn-Al)Solder Alloys. International Conference on Electronics Packaging. 2003:339~344
8 W. J. Jeong, H. Nishikawa. Characteristics of Conductive Adhesive for High Conductivity in Electronics Packaging. International Conference on Electronics Packaging. 2003:366~369
9邬博义,吴懿平,张乐福等.新一代绿色电子封装材料.微电子学. 2002,32(5):357~361
10田民波,梁彤祥,何卫.电子封装技术与封装材料.半导体情报. 1995,32(4):42~61
11 R. R. Tummala, E. J. Rymaszeuski, A. G. Klopfenstein等.微电子封装手册.第二版.北京:国防出版社. 2000:3~11
12 J. E. Morris. IEEE Forward:Electrically Conductive Adhesives. Transactions on CPMT-Part B. 1995,18(2):282~283
13 M. Lyons, E. Hall, Y. H. Wong, et al. A New Approach to Using Anisotropically Conductive Adhesives for FliP-Chip Assembly. IEEE Transactions on CPMT-Part A. 1996,19(l):5~11
14 P. Wong, D. Lu. Development of Solder Replacement Isotropically Adhesives. Electronics Packaging Technology Conference. 2000:214~221
15 S. Liong, C. P. Wong. An Altemative to Epoxy Resin for Application in Isotropically Adhesive. International Symposium on Advanced Packaging Maierials. 2001:13~18
16 J LiL, E. Morris. Elcetrical Conduction Models for Isotropiecally Conductive Adhesive Joints. IEEE Transactions on CPMT-Part A. 1997,20(l):3~8
17 D. D. Chang, P. A. Crawford, J. A. Fulton, et al. An Overview and Evaluation of Anisotropically ConductiveAdhesive Film for Fine Pitch Electronic Assembly. IEEE Transactions on Components, Hybrids and Manufacturing Technology.1993,16(8):828~835
18 D. P. Beck. Printed Electrical Resistor. U. S. Patent. 2,866,057,1958
19 H. Wolfson, G. Elliott. Electrically Conducting Cements Containing Epoxy Resins and Silver. U.S.Patent. 2,774,747,1956
20范志新,陈久琳,孙以材. AZO透明导电薄膜的特性、制备与应用.真空. 2000,(5):10
21夏志林.电子束蒸发制备AZO薄膜的光电性能研究.武汉:武汉理工大学. 2004:3~5
22巩锋.溶胶凝胶法制备Al 3+: ZnO薄膜及其性能研究.北京:北京工业大学. 2003:5~7
23 G Alan, Jack, O. Andersson. Iron Powder in Electrical Machines Possibilities and Limitations. Advances in Powder Metallurgy and Particulate Materials. 2001,48(5):1240~1249
24 B. J. ngram, T. O. Mason. Powder-solution-composite Technique for Measuring Electrical Conductivity of Ceramic Powders. Journal of the Electrochemical Society. 2003,150(8):396~402
25 J. Kozak, M. Rozenek and L. Dabrowski. Study of Electrical Discharge Machining Using Powder-suspended Working Media. Proceedings of the Institution of Mechanical Engineers. Journal of Engineering Manufacture. 2003,217(11):1597~1602
26 P. Pecas, E. Henriques. Influence of Silicon Powder-mixed Dielectric on Conventional Electrical Discharge Machining. International Journal of MachineTools and Manufacture. 2003, 43(14):1465~1471
27 Zois Haralampos, A. Lazaros and Yevgen Mamunya. Structure-electrical Properties Relationships of Polymer Composites Filled with Fe-powder. Macromolecular Symposia. 2003,194(4):351~359
28 Wenderothk, Pertermant. Effect of Pressure on the Impregnation of Thermoplastic Resin into a Unidirectional Fiber Bundle. Polym Composition. 1989,10(1):52~63
29 Z. Wang, F. Q. Xue and Y. He. An Adaptive Neuro-fuzzy Inference System for Engineering Vehicle Shift Decisions. Materials and Engineering. 2004, (20):3441~3443
30傅敏.导电涂料以及导电材料在导电涂料中的应用发展概况.涂料技术与文摘. 2006, (6):67~70
31姜雨泽.烟气净化用防腐涂料导电特性的实验研究.环境科学与技术. 2006, (5):25~29
32 Oboulhas, Tsahat, X. F. Xu, et al. Multi-plant Purchase Co-ordination Based on Multi-agent System in an ATO Environment. Journal of Manufacturing Technology Management. 2005,16(6):654~669
33 N. Venkatathri. Synthesis and Characterization of Vanadium Containing ATO and AFO type Molecular Sieves. Applied Catalysis. 2003, 242(6):393~401
34 X. C. Chen. Synthesis and Characterization of ATO/SiO2 Nanocomposite Coating Obtained by Sol-gel Method. Materials Letters. 2005, 59(10):1239~1242
35曾光群,康青,万步勇.碳纤维对水泥基复合材料电磁屏蔽性能的影响.材料科学与工程学报. 2006, (3):95~97
36奚文骏,冯玉光.导电衬垫在电磁屏蔽中的应用.电子元器件应用. 2005, (4):54~58
37 D. W. Kim, D. S. Kim and Y. G. Kim. Preparation of Hard Agglomerates Free and Weakly Agglomerated Antimony Doped Tin Oxide (ATO) Nanoparticles by Coprecipitation Reaction in Methanol Reaction Medium. Materials Chemistry and Physics. 2006,97(2):452~457
38 G. Du, X. Q. Liu, J. Yan, et al. Preparation of Conductive Coatings Filled with Nano ATO. Beijing Ligong Daxue Xuebao/Transaction of Beijing Institute of Technolog. 2005,25(9):285~288 - 44 -
39 Z. H. Chen, P. Y. Huang and X. G. Wu. Influences of Dehydrating Process on Properties of ATO Nano-powders. Transactions of Nonferrous Metals Society of China (English Edition). 2004,14(6):1123~1128
40 J. M. Montes, F. G. Cuevas and J. A. Rodriguez. Electrical Conductivity of Sintered Powder Compacts. Powder Metallurgy. 2005,48(4):343~344
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