醋酸铜基无颗粒型导电墨水的制备和性能研究

发布时间：2018-01-22 04:17

  本文关键词： 印刷电子 醋酸铜 无颗粒型导电墨水 烧结涂层 电阻率　出处：《郑州大学》2017年硕士论文　论文类型：学位论文

【摘要】：随着印刷电子的高速发展,印刷电子成为微电子领域的一种革命性先进制造技术,引起全球电子行业、制造行业等相关行业的广泛关注。电子器件向着高精度、低成本的目标发展,并且对材料、工艺的要求逐渐提高。导电墨水凭借其优异的导电性和广泛的应用领域等特点,必将成为电子印刷研究的核心技术。其中,金属基导电墨水除了具有导电性外,还可以通过印刷的方式来制备电子线路、图案,因此其在标签线路、柔性显示器、传感器等电子设备上将广泛应用。传统的导电墨水是以金或银等贵金属为导电源,但因其成本过高,将限制其更为广泛的应用。铜凭借低成本、高导电性等优势逐渐受到人们广泛关注。基于以上原因,本课题通过对导电墨水配方的优化,制备出了以醋酸铜为前驱体具有较高导电性的无颗粒型墨水,考察了铜胺配比、铜酸配比、溶剂配比等对烧结涂层导电性能的影响,同时对烧结条件对涂层导电性能的影响也做了初步探究,实现了醋酸铜基无颗粒型导电墨水的低温烧结。首先以醋酸铜为前驱体,通过对醋酸铜基无颗粒导电墨水的络合剂和醇溶剂进行优化选择,制备出了具有较高导电性的墨水。采用1,2丙二胺、异丙醇胺、正辛胺、N,N-二甲基乙醇胺、2-氨基-2-甲基-1-丙醇(AMP)这五种胺作为络合剂,并对所形成的络合物进行热稳定性分析。结果表明,有机胺能够较大程度地降低醋酸铜的热分解温度,并且以AMP为络合剂时,导电墨水的烧结涂层电阻率最低,为8.5μ??m。以甲酸为还原剂,通过改变导电墨水中醇溶剂的类型,调节体系的表面张力、粘度等,得到具有良好稳定性的导电墨水。在丙三醇和正丙醇为醋酸铜导电墨水的复合溶剂时,其烧结涂层电阻率低至3.4μ?·m。其次,在上述基础上,确定了以AMP为络合剂,丙三醇、正丙醇为复合醇溶剂,制备醋酸铜基无颗粒型导电墨水,进一步研究了墨水中铜胺配比、铜酸配比、溶剂配比对导电墨水导电性能的影响。当铜、胺、酸的物质的量配比为1:2.5:4,溶剂v(丙三醇):v(正丙醇):v(水)的体积比为3:3:2时,所制备的导电墨水的烧结涂层电阻率最低为3.4μ?·m。最后,对导电墨水烧结过程中烧结温度和时间对烧结涂层导电性能的影响进行了初步的研究。结果表明,烧结温度较低时,烧结涂层的电阻率较高,当烧结温度达到180℃时,电阻率低至3.4μ??m。伴随着烧结温度的继续上升,烧结涂层电阻率呈现上升的趋势;导电墨水在180℃下烧结得到的烧结涂层导电性能随着烧结时间的增加呈现出先升高后降低的趋势,并在烧结时间为0.5 h时,电阻率最低为3.4μ??m;并且在无需通入还原性气体的120℃空气气氛炉中进行烧结,能够得到均匀、致密、电阻率较低(4.4μ??m)的烧结涂层,初步实现了无颗粒型导电墨水在空气氛围中的低温烧结。
[Abstract]:With the rapid development of printing electronics, printing electronics has become a revolutionary advanced manufacturing technology in the field of microelectronics. Low cost target development, and the requirements of materials, technology gradually increased. Conductive ink, due to its excellent conductivity and wide range of applications, will become the core technology of electronic printing research. In addition to its electrical conductivity, metal-based conductive ink can also be printed to prepare electronic circuits and patterns, so that it can be used in label lines and flexible displays. Sensors and other electronic devices will be widely used. The traditional conductive ink is based on gold or silver as the guide power supply, but its high cost will limit its wider application. Copper with low cost. The advantages of high conductivity have been paid more and more attention. Based on the above reasons, through optimizing the formula of conductive ink, a kind of non-granular ink with copper acetate as precursor has been prepared. The effects of copper-amine ratio, copper-acid ratio and solvent ratio on the conductive properties of the sintered coatings were investigated. At the same time, the effects of sintering conditions on the conductive properties of the sintered coatings were also preliminarily investigated. The low temperature sintering of copper acetate based granular conductive ink was realized. Firstly, the complexing agent and alcohol solvent of copper acetate free conductive ink were optimized by using copper acetate as precursor. The ink with high conductivity was prepared by using 1o 2 propylenediamine, isopropanolamine, n-octylamine N- dimethyl ethanolamine. 2-amino-2-methyl-1-propanol (AMP) was used as a complexing agent, and the thermal stability of the complex was analyzed. Organic amines can lower the thermal decomposition temperature of copper acetate, and when AMP is used as complexing agent, the resistivity of conductive ink is the lowest, 8.5 渭? ? Using formic acid as reducing agent, by changing the type of alcohol solvent in conductive ink, adjusting the surface tension and viscosity of the system, etc. Conductive ink with good stability was obtained. When glycerol and n-propanol were used as composite solvents for copper acetate conductive ink, the resistivity of the sintered coating was as low as 3.4 渭? Secondly, on the basis of the above, the copper-free conductive acetic acid ink was prepared by using AMP as the complexing agent, glycerol and n-propanol as the complex alcohol solvent, and the ratio of copper amine in the ink was further studied. The effect of copper-acid ratio and solvent ratio on the conductivity of conductive ink. When the ratio of copper, amine and acid is 1: 2.5: 4. When the volume ratio of the solvent v: v is 3: 3: 2, the resistivity of the sintered coating of the conductive ink prepared by the solvent is the lowest 3.4 渭? Finally, the effect of sintering temperature and time on the conductive properties of the sintered coating was studied. The results showed that the resistivity of the sintered coating was higher when the sintering temperature was lower. When the sintering temperature reaches 180 鈩，

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