玻璃粉对铜导体浆料烧结膜性能的影响

doi:10.11901/1005.3093.2016.553

材料研究学报

2017, Vol. 31

Issue (6): 472-480 DOI: 10.11901/1005.3093.2016.553

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玻璃粉对铜导体浆料烧结膜性能的影响

马小强¹,朱晓云¹(

),龙晋明²,曹梅³

1 昆明理工大学材料科学与工程学院昆明 650093
2 昆明贵信凯科技有限公司昆明 650093
3 昆明理工大学理学院昆明 650093

Effect of Glass Powder on Performance of Copper Conductor Film Prepared via Sintering Cu-glass Paste

Xiaoqiang MA¹,Xiaoyun ZHU¹(

),Jinming LONG²,Mei CAO³

1 School of Materials Science and Engineering, Kunming University of Science and Technology, Kunming 650093, China
2 Kunming Guixinkai Science and Technology Ltd, Kunming 650093, China
3 School of Science, Kunming University of Science and Technology, Kunming 650093, China

引用本文:

马小强,朱晓云,龙晋明,曹梅. 玻璃粉对铜导体浆料烧结膜性能的影响[J]. 材料研究学报, 2017, 31(6): 472-480.
Xiaoqiang MA, Xiaoyun ZHU, Jinming LONG, Mei CAO. Effect of Glass Powder on Performance of Copper Conductor Film Prepared via Sintering Cu-glass Paste[J]. Chinese Journal of Materials Research, 2017, 31(6): 472-480.

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摘要:

使用不同组成和含量的玻璃粉配制铜浆,将其印在Al₂O₃基片表面并在850℃烧结后得到铜膜,研究玻璃粉对铜膜的导电性和附着力等性能的影响。用四探针法测定铜膜方阻,使用拉力试验机测定铜膜附着力。用金相显微镜、X射线衍射仪(XRD)、扫描电子显微镜(SEM)以及热重分析仪(TGA)等手段对铜膜的显微组织、物相、形貌以及玻璃粉物理化学性质进行了表征。结果表明,组成为SiO₂-B₂O₃-ZnO的G3玻璃粉的玻璃性能良好且其转变温度合适,制备出的铜膜试样表面平整,微观组织致密,导电性好。当G3玻璃粉含量(质量分数)为4.8%时铜膜的方阻为9.5 mΩ/□, 与Al₂O₃基体间的附着力为24 N/mm²。为了验证铜膜在使用过程中的可靠性,测试了G3-3铜膜的抗氧化和老化性能。结果表明,G3-3铜膜在室温氧化28 d后平均增重率为3.5%,电阻变化率的平均值为0.79%;在20℃~160℃高温老化后铜膜的电阻变化率平均值为12.63%、平均增重率为4.63%,具有良好的抗氧化性和抗老化性能。

关键词 ：复合材料, 玻璃粉, 铜膜, 方阻, 附着力, 可靠性

Abstract：

Copper pastes with different glass powders were prepared and then printed on Al₂O₃ substrate and finally sintered at 850℃ to produce Cu film on the Al₂O₃ substrate surface. The produced Cu-films and glass powder were characterized by means of metallographic microscope, X-ray diffractometer, scanning electron microscope and thermo gravimetric analyzer. While the effect glass powder on the conductivity and adhesive performance of Cu films was also assessed. The results show that glass powder G3 composited of SiO₂-B₂O₃-ZnO possesses appropriate transition temperature, with which a compact copper film with flat surface and good electrical conductivity can easy be made. When the Cu-paste with 4.8 mass% of glass powder G3, the produced Cu-film presents electrical resistance of 9.5 mΩ/□ and adhesive strength of 24 N/mm² to the Al₂O₃ substrate. In order to verify the reliability of Cu-film in service, the oxidation resistance and aging properties of Cu-film G3-3 were examined. It was found that the average mass gain rate of the Cu-film was 3.5% after 28 days oxidation at room temperature, the resistance change average rate was 0.79%. After aging test at 20~160^oC for 12 h, the average change rate of the Cu-film resistance was 12.63% and the average mass gain rate was 4.63%, which demonstrated that film has the good oxidation resistance and anti-aging performance.

Key words： composite glass powder copper film sheet resistance adhesion reliability

收稿日期: 2016-09-22

基金资助:国家科技型中小企业创新资金(14C26215303257),昆明市科技计划重点项目(2015-2-G-01945),昆明理工大学人才培养基金(kk23201351006)

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https://www.cjmr.org/CN/10.11901/1005.3093.2016.553 或 https://www.cjmr.org/CN/Y2017/V31/I6/472

表1 铜粉的性能指标

表2 玻璃粉的性能指标

表3 有机载体的配方

表4 铜浆的配方(质量分数,%)

图1 850℃氮气中的烧结曲线

图2 烧结铜膜试样

图3 玻璃粉G1~G4 的XRD衍射图

图4 铜模试样G1~G4的典型XRD衍射图

图5 玻璃粉G1与G3 的TG和DTG曲线图

图6 铜膜试样的金相显微照片

图7 铜膜试样的表面SEM照片

图8 铜膜试样截面的SEM照片

图9 铜膜试样的方阻

图10 铜膜试样的附着力

图11 后期烧结的铜膜试样

表5 室温环境下铜膜试样导电性变化情况

表6 高温老化试验前后铜膜试样氧化增重情况

图13 高温老化对铜膜试样导电性的影响

[1]	Li D M, Long J P, Zhang B.Study on the preparation and properties of PbO-B2O3 leaded electrical conductive copper paste[J]. Mater. Rev., 2014, 28B(8): 32
[1]	(李冬梅, 龙剑平, 张博. PbO-B2O3系含铅导电铜浆的制备及性能研究[J]. 材料导报, 2014, 28B(8): 32)
[2]	Zhang F J, Zhu X Y.Research progress and development tendency of organic carrier for electronic paste[J]. Mater. Rev., 2013, 27A(3): 81
[2]	(张飞进, 朱晓云. 电子浆料用有机载体的研究现状及发展趋势[J]. 材料导报, 2013, 27A(3): 81)
[3]	Lu G G, Xuan T P.Development tendency and research progress of the electronic paste[J]. Metall. Funct. Mater., 2008, 15(1): 48
[3]	(陆广广, 宣天鹏. 电子浆料的研究进展与发展趋势[J]. 金属功能材料, 2008, 15(1): 48)
[4]	Li Q, Xie Q, Ma R, et al.Study on research status and development tendency of the thick film resistor[J]. Mater. Rev., 2014, 28A(4): 31
[4]	(李强, 谢泉, 马瑞等. 厚膜电阻的研究现状及发展趋势[J]. 材料导报, 2014, 28A(7): 31)
[5]	Kim J M, Kim Y K.Thin crystalline silicon solar cell bonded to sintered substrate with aluminum paste[J]. Solar Energy Mater. Solar Cells, 2013, 86: 577
[6]	Li B, Wang J B, Su X L, et al.Research progress in improving processing of base metal electric conduction phase in electronic paste[J]. Mater. Rev., 2013, 27A(11): 35
[6]	(李冰, 王俊勃, 苏晓磊等. 电子浆料中的贱金属导电相的改善工艺研究进展[J]. 材料导报, 2013, 27A(11): 35)
[7]	He W, Yang Y, Wang S X, et al.Preparation technology and application progress of conductive inks[J]. Mater. Rev.: Summar., 2009, 23(21): 30
[7]	(何为, 杨颖, 王守绪等. 导电油墨制备技术及应用进展[J]. 材料导报: 综述篇, 2009, 23(21): 30)
[8]	Wang Y P, Su X L, Qu Y H, et al.Preparation and property of copper electronic pastes[J]. J. Mater. Sci. Eng., 2015, 33: 908
[8]	(王艳萍, 苏晓磊, 屈银虎等. 铜电子浆料的制备及性能[J]. 材料科学与工程学报, 2015, 33: 908)
[9]	Meng Q, Qu Y H, Cheng X L, et al.The effects of the lead-free glass powders on performances of copper electronic paste[J]. J. Funct. Mater., 2016, 47: 2130
[9]	(蒙青, 屈银虎, 成小乐等. 无铅玻璃粘结相对铜导电浆料性能的影响[J]. 功能材料, 2016, 47: 2130)
[10]	Gan W P, Zhou H, Zhang J L.Investigation of sintering process and electrical conductivity of the lead-free Ag paste[J]. Electron. Compon. Mater., 2010, 29(4): 65
[10]	(甘卫平, 周华, 张金玲. 无铅银浆烧结工艺与导电性能研究[J]. 电子元件与材料, 2010, 29(4): 65)
[11]	Ma G C, Zhu X Y, Pei Z L, et al.Effect of glass systems on the properties of copper paste[J]. Chin. J. Struct. Chem., 2014, 27: 1013
[11]	(马国超, 朱晓云, 裴占玲等. 玻璃体系对铜浆性能的影响[J]. 传感技术学报, 2014, 27: 1013)
[12]	Wu S P.Preparation of ultra-fine copper powder and its lead-free conductive thick film[J]. Mater. Lett., 2007, 61: 3526
[13]	Hong Y J, Jung D S, Koo H Y, et al.Characteristic of ZnO-B2O3-SiO2-CaO glass frits prepared by spray pyrolysis as inorganic binder for cu electrode[J]. J. Alloy Compounds, 2011, 509: 8077
[14]	Li S T.X-ray Diffraction of Crystals [M]. Beijing: Metallurgical Industry Press, 1990
[14]	(李树堂. 晶体X射线衍射学基础 [M]. 北京: 冶金工业出版社, 1990)
[15]	Shim S B, Kim D S, Hwang S, et al.Wetting and surface tension of bismate glass mel[J]. Thermochim. Acta, 2009, 496: 93
[16]	Ghosh A, Das S K, Biswas H S, et al.The effect of ZnO addition on the densification and properties of magnesium aluminate spinel[J]. Ceram. Int., 2000, 26: 605
[17]	Xu B, Cao J W, Liang K M.Influence of CaO and ZnO content on the crystallization and foaming of CaO-Al2O3-SiO2 glass-ceramics[J]. J. Inorgan. Mater., 2012, 27: 191
[17]	(徐博, 曹建尉, 梁开明. ZnO和CaO含量对CaO-Al2O3-SiO2系泡沫微晶玻璃析晶与发泡的影响[J]. 无机材料学报, 2012, 27: 191)
[18]	Yu S Y, Fu R L, Zhang J.Research progress and development trends of glass used in electronic paste[J]. Electronics Packaging, 2015, 15(1): 41
[18]	(余守玉, 傅仁利, 张捷. 电子浆料用玻璃的研究及发展趋势[J]. 电子与封装, 2015, 15(1): 41)
[19]	Ketkar S A, Umarji G G, Phatak G J, et al.Effect of glass content variation on properties of photoimageable silver conductor paste[J]. Mater. Chem. Phys., 2006, 96: 145
[20]	Bian H, Su X L, Li B, et al.Aging properties of low copper electronic pastes[J]. J. Mater. Sci. Eng., 2016, 34: 619
[20]	(边慧, 苏晓磊, 李冰等. 铜粉电子浆料的老化性能[J]. 材料科学与工程学报, 2016, 34: 619)

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