环保导电银浆的制备及其电子纸的性能研究
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摘要
导电银浆是制备电子元器件的关键功能材料。以银和淀粉为做导电填料,按照淀粉/硝酸银质量比分别为2∶1,1∶1,1∶2和1∶3,用氧化还原法制备导电银浆。通过测量电阻研究物理因素(加热烧结、紫外光照照射、泡水、超声波等)对导电银浆导电性能的影响,用显微镜观察导电银浆的形貌。结果表明,淀粉/硝酸银为1∶3时,形成了均匀的淀粉为核、银粒子为壳的导电颗粒。比例为1∶2和1∶3时,在低温加热烧结过程中电阻率降低到初始值的60%～70%。所得银浆能耐受紫外光照、水泡和超声波。其中1∶3导电性最佳。最后,用淀粉/硝酸银比例为1∶3的银浆,分别与30%、45%和60%的墨水混合,涂布纸张,并经低温热烧结后,所得电子纸的电阻率为10 mΩ/cm。
Conductive silver paste is a key functional material for the preparation of electronic components. Conductive silver paste with silver and starch used as conductive fillers was prepared by redox method with molar ratio of starch to silver nitrate of 2∶1, 1∶1, 1∶2 and 1∶3. The effect of physical factors, such as heating and sintering, ultraviolet light irradiation, soaking water, and ultrasonic wave, on the conductivity of the conductive silver paste was studied by measuring resistance, and the morphology of the conductive silver paste was observed with a microscope. The results showed that when the starch/silver nitrate was 1∶3, the uniform conductive particles with starch as core and silver particles as shell were formed. When the ratio was 1∶2 and 1∶3, the resistivity decreased to 60% to 70% of the initial value during the low-temperature heating and sintering. The resulting silver paste was resistant to UV light, blisters and ultrasound. Among them, the conductivity for the sample prepared with the molar ratio of 1∶3 was the best. Finally, a silver paste with a starch/silver nitrate ratio of 1∶3 was mixed with 30%, 45%, or 60% of the ink, coated with paper, and subjected to low-temperature thermal sintering, and the resulting electronic paper had a resistivity of 10 mΩ/cm.
Conductive silver paste is a key functional material for the preparation of electronic components. Conductive silver paste with silver and starch used as conductive fillers was prepared by redox method with molar ratio of starch to silver nitrate of 2∶1, 1∶1, 1∶2 and 1∶3. The effect of physical factors, such as heating and sintering, ultraviolet light irradiation, soaking water, and ultrasonic wave, on the conductivity of the conductive silver paste was studied by measuring resistance, and the morphology of the conductive silver paste was observed with a microscope. The results showed that when the starch/silver nitrate was 1∶3, the uniform conductive particles with starch as core and silver particles as shell were formed. When the ratio was 1∶2 and 1∶3, the resistivity decreased to 60% to 70% of the initial value during the low-temperature heating and sintering. The resulting silver paste was resistant to UV light, blisters and ultrasound. Among them, the conductivity for the sample prepared with the molar ratio of 1∶3 was the best. Finally, a silver paste with a starch/silver nitrate ratio of 1∶3 was mixed with 30%, 45%, or 60% of the ink, coated with paper, and subjected to low-temperature thermal sintering, and the resulting electronic paper had a resistivity of 10 mΩ/cm.
引文
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[22] Güzel R,üstünda,Ek?i H,et al.Effect of Au and Au@Ag core-shell nanoparticles on the SERS of bridging organic molecules[J].Journal of Colloid & Interface Science,2010,351(1):35-42.
[23] Yasuhiro Y,Tomoyoshi B,Tsukasa Y,et al.Synthesis and characterization of ZnO-Ag core-shell nanocomposites with uniform thin silver layers[J].Applied SurfaceScience,2010,256(20):6076-6082.
[24] Mancier V,Roussebertrand C,Dille J,et al.Sono and electrochemical synthesis and characterization of copper core-silver shell nanoparticles[J].Ultrasonics Sonochemistry,2010,17(4):690-696.
[2] Shen Bo.Preparation and properties of graphene composites containing silver,copper and bismuth [D].Beijing:China University of Geosciences,2014(in Chinese).沈博.含银、铜、铋的石墨烯复合材料的制备和性能研究[D].北京:中国地质大学,2014.
[3] Gu Shanqun.Preparation,microstructure and electrical conductivity of graphene/silver nanocomposites [J].Journal of Composite Materials,2015,32 (4):1061-1066(in Chinese).顾善群.石墨烯/纳米银复合材料的制备、微结构及其导电性能[J].复合材料学报,2015,32(4):1061-1066.
[4] Gu Shanqun.Preparation,structure and electrical conductivity of graphene/silver nanocomposites [D].Nanjing:Nanjing University of Aeronautics and Astronautics,2015(in Chinese).顾善群.石墨烯/纳米银复合材料的制备、结构及导电性[D].南京:南京航空航天大学,2015.
[5] Cui Lina.Preparation and application of carbon nanotubes/silver nanowires composites by in-situ growth [D].Beijing:Beijing University of Chemical Technology,2014(in Chinese).崔丽娜.原位生长法制备碳纳米管/纳米银线复合材料及其应用研究[D].北京:北京化工大学,2014.
[6] Wang Suzhan,He Wei,Deng Yumin,et al.Progress in preparation and application of graphene/nano-silver composite [J].Chemical Research,2017,28 (6):775-780(in Chinese).王苏展,贺伟,邓玉敏,等.石墨烯/纳米银复合材料的制备及其应用研究进展[J].化学研究,2017,28(6):775-780.
[7] Peng Xiao.Preparation of nano-silver/graphene composite and its application in conductive adhesives [D].Wuhan:Huazhong University of Science and Technology,2014(in Chinese).彭霄.纳米银/石墨烯复合物的制备及其在导电胶中的应用[D].武汉:华中科技大学,2014.
[8] Liu Konghua.Preparation of graphene/nano-silver hybrid and its application in epoxy resin conductive adhesives [D].Guangzhou:South China University of Technology,2014(in Chinese).刘孔华.石墨烯/纳米银杂化物的制备及在环氧树脂导电胶中的应用基础研究[D].广州:华南理工大学,2014.
[9] Zhao Jie.Preparation and application of nano silver conductive paste[D].Wuhan:Wuhan University of Technology,2011(in Chinese).赵杰.纳米银导电浆料的制备及应用研究[D].武汉:武汉理工大学,2011.
[10] Cai Bin.Preparation and electrical properties of nano-silver coated bimetallic composites [D].Shanghai:East China Normal University,2017(in Chinese).才滨.纳米银包裹双金属复合材料的制备及电性能研究[D].上海:华东师范大学,2017.
[11] Wang Jiebing.New preparation methods of core-shell copper-silver bimetallic composite nanoparticles [D].Beijing:Beijing University of Chemical Technology,2014(in Chinese).王洁冰.核壳结构铜银双金属复合纳米粒子的新型制备方法的研究[D].北京:北京化工大学,2014.
[12] Lyu Xiaoya.Preparation and sintering property characterization of silver-coated copper nanoparticles with core-shell structure [D].Harbin:Harbin Institute of Technology,2017(in Chinese).吕潇雅.核壳结构银包铜纳米颗粒的制备工艺与烧结性能表征[D].哈尔滨:哈尔滨工业大学,2017.
[13] Yang Chunmei.Preparation and properties of copper-containing micro/nanomaterials at room temperature [D].Chongqing:Southwest University,2016(in Chinese).杨春梅.室温环保法制备含铜微/纳米材料及性能研究[D].重庆:西南大学,2016.
[14] Wen Jianghong.Shell structure regulation and properties of ag-coated lead core-shell composite particles [D].Wuhan:Wuhan University of Technology,2013(in Chinese).文江鸿.银包铅核壳复合粒子的壳层结构调控与性能研究[D].武汉:武汉理工大学,2013.
[15] Li Chuanyou,Wang Qun,Wang Che.Preparation of Ag/Al composite powders by electroless plating [J].Journal of Functional Materials,2010,41 (9):1525-1528(in Chinese).李传友,王群,王澈.化学法镀法制备Ag/Al复合粉末[J].功能材料,2010,41(9):1525-1528.
[16] Kobayashi Y,Inose H,Nakagawa T,et al.X-ray imaging 1:echnique using colloid solution of Au/silica core-shell nanoparticles[J].Journal of Nanostructure in Chemistry,2013,3(1):1-6.
[17] Giizel R,Ustiindag Z,Eksi H,et al.Effect of Au and Au@Ag core-shell nanoparticles on the SERS of bridging organic molecules[J].Journal of Colloid & Interface Science,2010,351(1):35-42.
[18] Yasuhiro Y,Tomoyoshi B,Tsukasa Y,et al.Synthesis and characterization of ZnO-Ag core-shell nanocomposites with uniform thin silver layers[J].Applied Surface Science,2010,256(20):6076-6082.
[19] Mancier V,Roussebertrand C,Dille J,et al.Song and electrochemical synthesis and characterization of copper core-silver shell nanoparticles[J].Ultrasonics Sonochemistry,2010,17(4):690-696.
[20] Jung D S,Lee H M,KangY C,et al.Air-stable silver-coated copper particles of sub-micrometer size[J].Journal of Colloid &IrUerface Science,2011,364(2):4-581.
[21] Tsai C H,Chen S Y,Song J M,et al.Thermal stability of Cu@Ag core-shell nanoparticles[J].Corrosion Science,2013,74(4):123-129.
[22] Güzel R,üstünda,Ek?i H,et al.Effect of Au and Au@Ag core-shell nanoparticles on the SERS of bridging organic molecules[J].Journal of Colloid & Interface Science,2010,351(1):35-42.
[23] Yasuhiro Y,Tomoyoshi B,Tsukasa Y,et al.Synthesis and characterization of ZnO-Ag core-shell nanocomposites with uniform thin silver layers[J].Applied SurfaceScience,2010,256(20):6076-6082.
[24] Mancier V,Roussebertrand C,Dille J,et al.Sono and electrochemical synthesis and characterization of copper core-silver shell nanoparticles[J].Ultrasonics Sonochemistry,2010,17(4):690-696.