喷墨印刷导电墨水的研究
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摘要
为了研究适用于薄膜印刷电子产业的喷墨导电墨水,得到厚度薄、表面电阻低的导电层。在制备得到粒径小、浓度较高的纳米银稳定悬浮液后,通过对其进行喷墨印刷适性调试,得到可上机打印的喷墨导电墨水,并对打印样张的导电性能及其影响因素进行了研究。
采用液相化学还原法,通过调节银盐和水合肼的摩尔比,在高分子保护剂聚乙烯吡咯烷酮(PVP)的作用下,反应得到平均直径为50 nm的纳米银悬浮液。利用丙酮和去离子水清洗反应后的悬浮液,除去反应杂质,然后在高速离心的作用下,分离得到较为纯净的高浓度的纳米银沉淀。将纳米银沉淀重新分散,调整其pH值、粘度、电导率和表面张力等参数,最终得到了银含量为2.5%的喷墨导电墨水。经耐候性测试实验发现,常温下,喷墨导电墨水在较长时间内的稳定性能良好。
在EPSON ME1+打印机上进行墨水打印测试,通过对不同打印精度、打印次数和不同介质的样张进行对比,得出最佳打印条件。对得到的打印样张进行不同手段的后处理,比较后处理前后样张导电性能的变化。研究发现,喷墨导电墨水在高精度打印设置下,在相纸上重复打印三遍形成导电层的导电性能较好,其厚度小于1μm。在对样张进行水洗、低温烧结和激光扫描后处理后,导电性能进一步改善,最低可达到4Ω／□。
To study the inkjet printing conductive ink applied to the film electronic industry, to obtain thin,low surface resistance conductive coating.Stable nanosized silver suspension of small size and high concentrations was prepared in this thesis and through its inkjet Printability adjusting,finally obtain the conductive ink which could be on the ink-jet printing,the conductive properties of the printing sample and its effects Factors were studied.
Adopting the liquid-phase chemical reduction,by regulating the molar ratio of the silver salt and hydrazine hydrate, in the polymer agent PVP role,the response has been an average diameter of 50 nm nanosized silver suspension. To washing the suspension using acetone and deionized water, to remove impurities,and then in the role of high-speed centrifuge,isolated pure high concentration nanosized silver deposition.The nanosized silver precipitation will be re-distributed,to adjust its pH value,viscosity, surface tension and electrical conductivity, and other parameters, and finally the silver content of 2.5 percent of the conductive ink-jet ink. After weathering testing,it found that the conductive ink has good performance and stability in an extended period in the room temperature.
The printer EPSON ME1+was used for the printing tests by different printing accuracy, the numbers of printing and different printing stock. After comparing the samples,obtain the best printing condition.The print samples were treated by different means of post-treatment. The conductivity of the samples were compared before and after post-treatment. It found that in the set of high-precision,and repeat to print three times in the printing stock, the conductive performance of the conductive layer is good,and its thickness is less than 1μm.The samples after water washing,sintering processing and laser scanning,have a better electric conductivity, the minimum can reached 4Ω/□.
采用液相化学还原法,通过调节银盐和水合肼的摩尔比,在高分子保护剂聚乙烯吡咯烷酮(PVP)的作用下,反应得到平均直径为50 nm的纳米银悬浮液。利用丙酮和去离子水清洗反应后的悬浮液,除去反应杂质,然后在高速离心的作用下,分离得到较为纯净的高浓度的纳米银沉淀。将纳米银沉淀重新分散,调整其pH值、粘度、电导率和表面张力等参数,最终得到了银含量为2.5%的喷墨导电墨水。经耐候性测试实验发现,常温下,喷墨导电墨水在较长时间内的稳定性能良好。
在EPSON ME1+打印机上进行墨水打印测试,通过对不同打印精度、打印次数和不同介质的样张进行对比,得出最佳打印条件。对得到的打印样张进行不同手段的后处理,比较后处理前后样张导电性能的变化。研究发现,喷墨导电墨水在高精度打印设置下,在相纸上重复打印三遍形成导电层的导电性能较好,其厚度小于1μm。在对样张进行水洗、低温烧结和激光扫描后处理后,导电性能进一步改善,最低可达到4Ω／□。
To study the inkjet printing conductive ink applied to the film electronic industry, to obtain thin,low surface resistance conductive coating.Stable nanosized silver suspension of small size and high concentrations was prepared in this thesis and through its inkjet Printability adjusting,finally obtain the conductive ink which could be on the ink-jet printing,the conductive properties of the printing sample and its effects Factors were studied.
Adopting the liquid-phase chemical reduction,by regulating the molar ratio of the silver salt and hydrazine hydrate, in the polymer agent PVP role,the response has been an average diameter of 50 nm nanosized silver suspension. To washing the suspension using acetone and deionized water, to remove impurities,and then in the role of high-speed centrifuge,isolated pure high concentration nanosized silver deposition.The nanosized silver precipitation will be re-distributed,to adjust its pH value,viscosity, surface tension and electrical conductivity, and other parameters, and finally the silver content of 2.5 percent of the conductive ink-jet ink. After weathering testing,it found that the conductive ink has good performance and stability in an extended period in the room temperature.
The printer EPSON ME1+was used for the printing tests by different printing accuracy, the numbers of printing and different printing stock. After comparing the samples,obtain the best printing condition.The print samples were treated by different means of post-treatment. The conductivity of the samples were compared before and after post-treatment. It found that in the set of high-precision,and repeat to print three times in the printing stock, the conductive performance of the conductive layer is good,and its thickness is less than 1μm.The samples after water washing,sintering processing and laser scanning,have a better electric conductivity, the minimum can reached 4Ω/□.
引文
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[2]胡维友.数字印刷与计算机直接制版技术[M].印刷工业出版社,2007
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[4]李媛媛.溶剂／颜料型彩色数字打样用喷墨油墨的研究[D].北京印刷学院硕士学位论文,2006.
[5]李路海.印刷油墨着色剂[M],印刷工业出版社,2008
[6]王雪峰,黄毓礼,孙芳,等.水基喷墨打印墨水性能研究[J].北京化工大学学报,2004,31(2)：53-57.
[7]李路海.印刷油墨着色剂[M],印刷工业出版社,2008
[8]张俊,李忠平,董川.表面活性剂在墨水制造中的应用[J].日用化学工业,2004,34(6)：383-387.
[9]杨俊玲.泡沫及消泡技术[J].表面活性剂工业,1995,12(4)：29-32.
[10]Burden. A. P, Brierley. M, Brierley. M. Solid-State Electronics,2001, 45(06):987.
[11]Howard. E, Katz. Chem. Mate,2004,16(23):4748.
[12]H. Sirringhaus, T. Kawase, R. H. Friend,T. Shimoda, M. Inbasekaran, W. Wu, E. P. Woo. Science,2000,290:2123.
[13]莫黎昕.导电油墨构成与导电性能关系的研究[D].北京印刷学院硕士学位论文,2008.
[14]Shirakawa H, Louis E J, MacDiarmid A G, et al.J. Chem. Soc.Chem. Commun,1977, 16:578.
[15]S.R.WANG, J.P.DOUGHERTY, W. HUEBNER and J. G. PEPIN, J. Amer. Ceram. Soc.77(1994) 3051.
[16]N. SCALTER, in "Electronics Technology Handbook" (McGraw-Hill,New York,1999) p.509.
[17]Idem. IEEE Trans. Comp. Hybrids and Manuf. Tech.11(1988) 291.R. K. F TENG, A. M. AZADPOUR and A. KARIM, IEEE
[18]R.K.F TENG, A. M. AZADPOUR and A. KARIM, IEEE Trans. Ind. Electron.37(1990) 419. B. A. GLOWACKI,Supercond. Sci.Technol.13 (2000) 584.
[19]D.J.HAYES, W. R. COX and M. E. GROVE, J. Electron. Manuf.8(1998) 209.
[20]Idem. http://www.microfab.com/papers/paper-pdf/displayworks-99.PDF(Accessed 8 Aug 2000).
[21]M. H. CHEONG and S. WAGNER, IEEE Electron Dev. Lett.21 (2000) 384.
[22]M. J. EDIRISINGHE, in Proc.1998 TMS Fall Meeting, Rosemont,Illinois,USA, October 1998, edited by T. S.Srivatsanand K. A. Khor
[23]The Minerals, Metals and Materials Society, Warrendale, USA,1998) p.139.
[24]Alan Rae,Dana Hammer-Fritzinger.采用导电喷墨墨水形成金属和非金属的纳米系统[J].半导体科技,2006(6)
[25]张伟.喷墨打印技术的发展现状[J].染料与染色,2005,12(6)：9-12.
[26]王景翰,刘淑霞,孙里春,谷颖颖.喷墨打印墨水分析技术的回顾及展望[J].辽宁警专学报,2006,1(1)：3-6.
[27]Kan-Sen Chou,Kuo-Cheng Huang,Hsien-Hsuen Lee. Fabrication and sintering effect on the morphologies and conductivity of nano-Ag particle films by the spin coating method[J].Nanotechnology,2005(16)779-784.
[28]Hsien-Hsueh Lee,Kan-Sen Chou,Kuo-Cheng Huang. Inkjet printing of nanosized silver colloids[J]Nanotechnology,2005(16)2436-2441
[29]周更生,李贤学,高振裕,卢育杰.纳米银[J].科技发展,2006,12(408)：32-39
[30]石川,程谟杰,曲振平等.纳米银催化的甲烷选择还原NO反应研究[J].复旦学报(自然科学版),2002,41(3)：269-279.
[31]董维国,陈岁元,张继良.微细银粉的制备与应用[J].材料与冶金学报,2002,1(3)：171-205.
[32]司民真,武荣国,李世荣.纳米银的制备及有关光学性质简介[J].楚雄师专学报,1999,14(3)：4-8.
[33]Nishimura K, Honbo H, Takeuchi S, et al. Design and performance of 10 Wh rechargeable lithium batteries[J].Journal of Power Sources,1997,68(2):436-439.
[34]Franco H, Bossy J, Godfrin H. Properties of sintered silver powders and their application in heat exchangers at millikelvin temperatures[J].Cryogenics,1984, 24(9):477.
[35]何发泉,李勇军.银粉的用途和制备[J].中国粉体技术,2001,7(3)：45-47.
[36]陈水挟,罗颖,许瑞梅等.银型抗菌活性碳纤维的结构及其抗菌性能的研究[J].材.料科学与工程,2001,19(4)：66-79.
[37]姜会庆,汪军,胡心宝等.纳米银敷料在烧伤创面的应用[J].医学研究生学报,2001,(5)：439.
[38]李敏娜.纳米银粒子制备及应用研究进展[J].化工进展
[39]J. H. SONG, M. J. EDIRISINGHE and J. R. G. EVANS[J].ibid.82(1999)3374.
[40]B. Y.TAY, H. RASHID and M. J. EDIRISINGHE. J. Mater. Sci[J].Lett.19(2000)799.
[41]W. D. TENG, M. J. EDIRISINGHE and J. R. G. EVANS,J.Amer[J].Ceram. Soc.80(1997)486.
[42]W.D. TENG and M.J. EDIRISINGHE[J].ibid.81(1998)1033.
[43]刘冲,刘红莉.喷墨打印墨水组分的性能研究[J].丝网印刷,2007,12：22-25：13-15
[44]吕海宁.喷墨打印墨水组成成分的性能研究状况[J].江苏化工市场七日讯,2006,(24)。
[45]简子桀.喷墨用纳米银胶之合成研究.台湾大同大学硕士论文
[2]胡维友.数字印刷与计算机直接制版技术[M].印刷工业出版社,2007
[3]付冰.喷墨打印技术的进展和发展趋势[J].信息记录材料,2002
[4]李媛媛.溶剂／颜料型彩色数字打样用喷墨油墨的研究[D].北京印刷学院硕士学位论文,2006.
[5]李路海.印刷油墨着色剂[M],印刷工业出版社,2008
[6]王雪峰,黄毓礼,孙芳,等.水基喷墨打印墨水性能研究[J].北京化工大学学报,2004,31(2)：53-57.
[7]李路海.印刷油墨着色剂[M],印刷工业出版社,2008
[8]张俊,李忠平,董川.表面活性剂在墨水制造中的应用[J].日用化学工业,2004,34(6)：383-387.
[9]杨俊玲.泡沫及消泡技术[J].表面活性剂工业,1995,12(4)：29-32.
[10]Burden. A. P, Brierley. M, Brierley. M. Solid-State Electronics,2001, 45(06):987.
[11]Howard. E, Katz. Chem. Mate,2004,16(23):4748.
[12]H. Sirringhaus, T. Kawase, R. H. Friend,T. Shimoda, M. Inbasekaran, W. Wu, E. P. Woo. Science,2000,290:2123.
[13]莫黎昕.导电油墨构成与导电性能关系的研究[D].北京印刷学院硕士学位论文,2008.
[14]Shirakawa H, Louis E J, MacDiarmid A G, et al.J. Chem. Soc.Chem. Commun,1977, 16:578.
[15]S.R.WANG, J.P.DOUGHERTY, W. HUEBNER and J. G. PEPIN, J. Amer. Ceram. Soc.77(1994) 3051.
[16]N. SCALTER, in "Electronics Technology Handbook" (McGraw-Hill,New York,1999) p.509.
[17]Idem. IEEE Trans. Comp. Hybrids and Manuf. Tech.11(1988) 291.R. K. F TENG, A. M. AZADPOUR and A. KARIM, IEEE
[18]R.K.F TENG, A. M. AZADPOUR and A. KARIM, IEEE Trans. Ind. Electron.37(1990) 419. B. A. GLOWACKI,Supercond. Sci.Technol.13 (2000) 584.
[19]D.J.HAYES, W. R. COX and M. E. GROVE, J. Electron. Manuf.8(1998) 209.
[20]Idem. http://www.microfab.com/papers/paper-pdf/displayworks-99.PDF(Accessed 8 Aug 2000).
[21]M. H. CHEONG and S. WAGNER, IEEE Electron Dev. Lett.21 (2000) 384.
[22]M. J. EDIRISINGHE, in Proc.1998 TMS Fall Meeting, Rosemont,Illinois,USA, October 1998, edited by T. S.Srivatsanand K. A. Khor
[23]The Minerals, Metals and Materials Society, Warrendale, USA,1998) p.139.
[24]Alan Rae,Dana Hammer-Fritzinger.采用导电喷墨墨水形成金属和非金属的纳米系统[J].半导体科技,2006(6)
[25]张伟.喷墨打印技术的发展现状[J].染料与染色,2005,12(6)：9-12.
[26]王景翰,刘淑霞,孙里春,谷颖颖.喷墨打印墨水分析技术的回顾及展望[J].辽宁警专学报,2006,1(1)：3-6.
[27]Kan-Sen Chou,Kuo-Cheng Huang,Hsien-Hsuen Lee. Fabrication and sintering effect on the morphologies and conductivity of nano-Ag particle films by the spin coating method[J].Nanotechnology,2005(16)779-784.
[28]Hsien-Hsueh Lee,Kan-Sen Chou,Kuo-Cheng Huang. Inkjet printing of nanosized silver colloids[J]Nanotechnology,2005(16)2436-2441
[29]周更生,李贤学,高振裕,卢育杰.纳米银[J].科技发展,2006,12(408)：32-39
[30]石川,程谟杰,曲振平等.纳米银催化的甲烷选择还原NO反应研究[J].复旦学报(自然科学版),2002,41(3)：269-279.
[31]董维国,陈岁元,张继良.微细银粉的制备与应用[J].材料与冶金学报,2002,1(3)：171-205.
[32]司民真,武荣国,李世荣.纳米银的制备及有关光学性质简介[J].楚雄师专学报,1999,14(3)：4-8.
[33]Nishimura K, Honbo H, Takeuchi S, et al. Design and performance of 10 Wh rechargeable lithium batteries[J].Journal of Power Sources,1997,68(2):436-439.
[34]Franco H, Bossy J, Godfrin H. Properties of sintered silver powders and their application in heat exchangers at millikelvin temperatures[J].Cryogenics,1984, 24(9):477.
[35]何发泉,李勇军.银粉的用途和制备[J].中国粉体技术,2001,7(3)：45-47.
[36]陈水挟,罗颖,许瑞梅等.银型抗菌活性碳纤维的结构及其抗菌性能的研究[J].材.料科学与工程,2001,19(4)：66-79.
[37]姜会庆,汪军,胡心宝等.纳米银敷料在烧伤创面的应用[J].医学研究生学报,2001,(5)：439.
[38]李敏娜.纳米银粒子制备及应用研究进展[J].化工进展
[39]J. H. SONG, M. J. EDIRISINGHE and J. R. G. EVANS[J].ibid.82(1999)3374.
[40]B. Y.TAY, H. RASHID and M. J. EDIRISINGHE. J. Mater. Sci[J].Lett.19(2000)799.
[41]W. D. TENG, M. J. EDIRISINGHE and J. R. G. EVANS,J.Amer[J].Ceram. Soc.80(1997)486.
[42]W.D. TENG and M.J. EDIRISINGHE[J].ibid.81(1998)1033.
[43]刘冲,刘红莉.喷墨打印墨水组分的性能研究[J].丝网印刷,2007,12：22-25：13-15
[44]吕海宁.喷墨打印墨水组成成分的性能研究状况[J].江苏化工市场七日讯,2006,(24)。
[45]简子桀.喷墨用纳米银胶之合成研究.台湾大同大学硕士论文