CN104715807B - 导电胶组合物与电极的形成方法 - Google Patents
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Abstract
本发明提供了一种导电胶组合物,其包括:100重量份的铜粉;40至150重量份的银粉;0.1至3重量份的碳材;1至5重量份的玻璃粉;以及5至15重量份的粘合剂。上述导电胶组合物可施加至基板上,再在一般大气下高温烧结该导电胶组合物,从而在该基板上形成电极。
Description
技术领域
本发明涉及导电胶组合物,更特别关于其应用。
背景技术
导电胶是以粘合剂(如树脂)与导电填充物(如金属)所制成的复合材料,常见于电子产业中。它的特点是兼具导电性(来自金属)与粘合性及粘度(来自树脂),且可根据加工需求调整上述性质。导电胶的导电性取决于填充导电金属粉体的种类、形状、及大小。若导电填充物彼此接触的点越多,便可增加导电性。一般导电胶具有高含量(>75wt%)的导电填充物,在有机树脂粘合剂内的导电填充物即相互连结,经由热压接着或硬化后可形成网状连结并与上下电极接触,从而形成电流及信号传导途径。
导电胶是电子组件封装、电极和互联的关键材料,主要分为高温锻烧型,与低温固化型两大类。锻烧型导电胶主要用在太阳能电池等产业。固化型导电胶则广泛的应用在印刷电路以及电子封装等产业。其中铜粉是一种良好的导电填充物。然而,铜于200℃以上的高温下容易氧化,为了对其进行锻烧来形成电极,需要于氮气等惰性气氛环境下进行锻烧的特殊步骤来避免铜氧化。
综上所述,目前亟需新的导电胶组合物以降低铜胶易氧化等问题。
发明内容
本发明的实施方式提供一种导电胶组合物,其包括:100重量份的铜粉;40至150重量份的银粉;0.1至3重量份的碳材;1至5重量份的玻璃粉;以及5至15重量份的粘合剂。
本发明一种实施方式提供一种电极的形成方法,其包括:将上述导电胶组合物施加至基板上;以及在一般大气下高温烧结导电胶组合物,从而在该基板上形成电极。
具体实施方式
本发明提供的导电胶组合物包含100重量份的铜粉、约40至150重量份的银粉、约0.1至3重量份的碳粉、约1至5重量份的玻璃粉、和约5至15重量份的粘合剂。上述导电胶组合物中的碳粉在高温锻烧时,可抑制铜的氧化现象并还原氧化铜,从而形成电阻率低的电极。
在本发明的一种实施方式中,铜粉的粒径约为1μm至10μm。若铜粉的粒径过大,则印刷时有塞版的疑虑且印刷后的图案不够细致。若铜粉的粒径过小,则因比表面积较大导致氧化的程度增加。此外,铜粉粒径大于银粉粒径。若银粉粒径大于或等于铜粉粒径,则银粉无法有效的包覆于铜粉的表面,达到阻绝氧化的效果。
在本发明一种实施方式中,银粉的粒径约为0.1μm至2μm。若银粉的粒径过大,则银粉包覆于铜粉的表面效果不佳。若银粉的粒径过小,则银粉容易产生聚集而不易分散。此外,若银粉的比例过高,则会大幅增加导电胶的成本。若银粉的比例过低,则无法使高温烧结后形成的电极具有足够的导电率。
在本发明一种实施方式中,碳粉可为石墨烯、活性碳、碳纳米管、人造石墨、或天然石墨。在本发明一种实施方式中,碳粉的比表面积约为200m2/g至1000m2/g。若碳粉的比表面积过低,则无法有效抑制高温烧结时的铜氧化现象。此外,若碳粉的比例过高,将降低烧结后形成的电极的导电率。若碳粉的比例过低,则无法有效抑制高温烧结时的铜氧化现象。
在本发明一种实施方式中,玻璃粉的软化点小于或等于600℃,且结晶化起始温度超过600℃。上述玻璃粉可为购自冈本硝子的BBG-3或VBP。
在本发明一种实施方式中,粘合剂包含环氧树脂与硬化剂。举例来说,环氧树脂可为含双酚的环氧树脂、邻-甲酚酚醛清漆环氧树脂、脂环族环氧树脂、或其他环氧树脂。举例来说,含双酚的环氧树脂可为购自Shell公司的EPON828、购自DIC公司的H-4032D、或购自DIC公司的EXA-830LVP;邻-甲酚酚醛清漆环氧树脂可为购自长春化工的CNE202;脂环族环氧树脂可为购自U.C.公司的ERL4221E或ERL4206、购自CVC公司的EPALLOYTM5200、或购自CVC公司的EPALLOYTM5001,其他环氧树脂,例如为购自CVC公司的GS120、或购自CVC公司的GE20。硬化剂可为胺类硬化剂或酸酐类硬化剂。胺类硬化剂如购自Huntsman的D230、D400、D2000、或其组合,酸酐类硬化剂如购自Lonza的MHHPA-MW、MTHPA、NMA、或其组合、或阳离子型硬化剂如购自三新化工的SI-45、SI-60、SI-B2A、SI-B3、SI-B3A、或其组合,或其组合。在本发明一种实施方式中,粘合剂可进一步包含反应促进剂。反应促进剂可降低环氧树脂硬化反应的温度,比如购自SAN-APRO的SA102、购自TCI的2E4MZ、或购自Aldrich的TMAH。
在另一种实施方式中,上述导电胶组合物可进一步添加溶剂、增稠剂、分散剂、触变剂、消泡剂、或其组合,以改良导电胶的加工性。
在本发明一种实施方式中,将上述导电胶组合物施加至基板上,再在一般大气下高温烧结该导电胶组合物,从而在基板上形成电极。在本发明一种实施方式中,基板可为陶瓷基板或硅晶圆等耐高温烧结的基板,且高温烧结的温度为约500℃至900℃,或约600℃至900℃,或约700℃至900℃。经上述高温烧结后可形成高导电率(低电阻)的电极,适用于太阳能电池的表面电极或其他耐高温制程的组件。由于碳粉可抑制铜的氧化现象及还原氧化铜,因此上述高温烧结制程可在一般大气下操作,可不需要在惰性气体或还原气氛下操作,可简化制程。
为让本发明的上述和其他目的、特征、和优点能更明显易懂,下文特举出实施例作详细说明如下:
实施例1
取16.76gEPON828、52.6gERL4221E、57.92gMHHPA-MW以及0.694g四甲基氢氧化铵(TMAH),混合形成粘合剂A。取70g铜粉(购自DOWA,平均粒径10μm)、30g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、0.1g石墨烯(制备方法请参考H.A.Becerill,J.Mao,Z.Liu,R.M.Stoltenberg,Z.Bao,and Y.Chen,ACSNano2,463(2008),比表面积约为500m2/g)、与15g实施例1的粘合剂A高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表1所示。
实施例2
与实施例1类似,差别在于石墨烯的添加量增加至0.5g。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
实施例3
与实施例1类似,差别在于使用的铜粉粒径为4.7μm(购自Fukuda Cu-HWQ)、银粉的粒径为0.8μm(购自DOWA AG-2-1C)以及0.1g石墨烯改为0.1g碳纳米管(购自SeedchemCompany Pty.,Ltd.的MWCNT,其比表面积约为200m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
实施例4
与实施例1类似,差别在于使用的铜粉粒径为4.7μm(购自Fukuda Cu-HWQ)、银粉粒径为0.8μm(购自DOWA AG-2-1C)以及0.1g石墨烯改为0.5g碳纳米管(购自SeedchemCompany Pty.,Ltd.的MWCNT,其比表面积约为200m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
比较例1
与实施例1类似,差别在于未添加任何碳材。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
比较例2
与实施例1类似,差别在于0.1g石墨烯改为0.1g石墨(购自TIMCAL graphite的KS-6,其比表面积约为20m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
比较例3
与实施例1类似,差别在于0.1g石墨烯改为0.5g石墨(购自TIMCAL graphite的KS-6,其比表面积约为20m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例1。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
表1
由表1可知,除了石墨烯以外,亦可采用高比表面积的碳纳米管降低导电胶的体积电阻率。此外,并非所有的碳材均可用于降低导电胶的体积电阻率。举例来说,低比表面积的石墨无法降低导电胶的体积电阻率。
实施例5
取20gEPALLOYTM5200、20gERL4221E、以及1.2gSI-60混合形成粘合剂B。取50g铜粉(购自DOWA,平均粒径10μm)、50g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、0.1g石墨烯(制备方法参考H.A.Becerill,J.Mao,Z.Liu,R.M.Stoltenberg,Z.Bao,and Y.Chen,ACSNano2,463(2008),比表面积约为500m2/g)、与15g粘合剂B高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表2所示。
实施例6
与实施例5类似,差别在于石墨烯的用量增加至0.2g。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例6。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
比较例4
与实施例5类似,差别在于未添加任何碳材。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例5。最后形成的电极的附着力为5B,其体积电阻率如表1所示。
表2
由表2可知,石墨烯可降低导电胶的体积电阻率。
实施例7
取40g铜粉(购自DOWA,平均粒径10μm)、60g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、0.1g石墨烯(制备方法参考H.A.Becerill,J.Mao,Z.Liu,R.M.Stoltenberg,Z.Bao,and Y.Chen,ACSNano2,463(2008),比表面积约为500m2/g)、与15g实施例1的粘合剂A高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟以形成电极,其附着力为5B,且其体积电阻率如表3所示。
实施例8
与实施例7类似,差别在于石墨烯的用量增加至0.2g。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
实施例9
与实施例7类似,差别在于使用的铜粉粒径为4.7μm(购自Fukuda Cu-HWQ)、银粉粒径为0.8μm(购自DOWA AG-2-1C)以及0.1g石墨烯改为0.1g碳纳米管(购自SeedchemCompany Pty.,Ltd.,其比表面积约为200m2/g)。其余玻璃粉、及粘合剂用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
实施例10
与实施例7类似,差别在于使用的铜粉粒径为4.7μm(购自Fukuda Cu-HWQ)、银粉粒径为0.8μm(购自DOWA AG-2-1C)以及0.1g石墨烯改为0.2g碳纳米管(购自SeedchemCompany Pty.,Ltd.,其比表面积约为200m2/g)。其余玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例5
与实施例7类似,差别在于未添加任何碳材。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例6
与实施例7类似,差别在于0.1g石墨烯改为3g镍粉(购自鸿钧)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例7
与实施例7类似,差别在于0.1g石墨烯改为3g铝粉(购自鸿钧)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例8
与实施例7类似,差别在于0.1g石墨烯改为0.1g石墨(购自TIMCAL graphite的KS-6,其比表面积约为20m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例9
与实施例7类似,差别在于0.1g石墨烯改为0.5g石墨(购自TIMCAL graphite的KS-6,其比表面积约为20m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
比较例10
与实施例7类似,差别在于0.1g石墨烯改为10g石墨(购自TIMCAL graphite的KS-6,其比表面积约为20m2/g)。其余铜粉、银粉、玻璃粉、及粘合剂的用量,以及混合、研磨分散、印刷、与烧结形成电极等步骤均同实施例7。最后形成的电极的附着力为5B,其体积电阻率如表3所示。
表3
由表3可知,除了石墨烯以外,亦可采用高比表面积的碳纳米管降低导电胶的体积电阻率。此外,并非所有的碳材均可用于降低导电胶的体积电阻率。举例来说,低比表面积的石墨无法降低导电胶的体积电阻率。另一方面,金属粉如镍粉或铝粉亦无法降低导电胶的体积电阻率。
比较例11
取40g铜粉(自制,制备方法参考H.T.Zhu et al.,Journal of CrastalGrowth270,722(2004),平均粒径0.1μm)、60g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、与15g实施例1的粘合剂A高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表4所示。
比较例12
取40g铜粉(自制,制备方法参考H.T.Zhu et al.,Journal of CrastalGrowth270,722(2004),平均粒径0.1μm)、60g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、0.5g碳纳米管(购自Seedchem Company Pty.,Ltd.的MWCNT,其比表面积约为200m2/g)、与15g实施例1的粘合剂A高速搅拌后,再以三滚筒研磨分散3次形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表4所示。
比较例13
取40g铜粉(自制,制备方法参考H.T.Zhu et al.,Journal of CrastalGrowth270,722(2004),平均粒径0.1μm)、60g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、1.0g碳纳米管(购自Seedchem Company Pty.,Ltd.的MWCNT,其比表面积约为200m2/g)、与15g实施例1的粘合剂A高速搅拌后,再以三滚筒研磨分散3次形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟以形成电极,其附着力为5B,且其体积电阻率如表4所示。
表4
由表4可知,粒径过小的铜粉将大幅增加产品的体积电阻率。
比较例14
取80g铜粉(购自DOWA,平均粒径10μm)、20g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)与15g实施例1的粘合剂A高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表5所示。
比较例15
取80g铜粉(购自DOWA,平均粒径10μm)、20g银粉(购自Ferro,平均粒径为2.0μm)、5g玻璃粉(购自冈本硝子,平均粒径3.0μm)、1g石墨烯(自制,制备方法参考H.A.Becerill,J.Mao,Z.Liu,R.M.Stoltenberg,Z.Bao,and Y.Chen,ACSNano2,463(2008),比表面积约为500m2/g)、与15g实施例1的粘合剂A高速搅拌后,再研磨分散形成导电胶。将导电胶网版印刷于多晶硅基材上后,置于800℃烘箱烧结30分钟从而形成电极,其附着力为5B,且其体积电阻率如表5所示。
表5
由表5可知,当铜粉比例过高时将大幅增加产品的体积电阻率。
上述实施例所提供之导电胶组合物,可用于硅晶太阳能电池的高温烧结制程,除了利用不同粒径尺度的金属粒子(铜/银)混掺调配提高填充密度,提升导电度。藉由添加高比表面积的碳材如石墨烯或碳纳米管提升导电胶的抗氧化能力,可解决银价格昂贵、且现今技术于高温制程容易使铜氧化的技术瓶颈,为极佳的太阳能电池的高温烧结制程所用的导电胶组合物。
虽然本发明已以数个实施例揭露如上,然其并非用以限定本发明,任何所属技术领域中具有通常知识者,在不脱离本发明之精神和范围内,当可作任意之更动与润饰,因此本发明之保护范围当视后附之申请专利范围所界定者为准。
Claims (4)
1.一种导电胶组合物,其包括:
100重量份的铜粉;
40至150重量份的银粉;
0.1至3重量份的碳粉;
1至5重量份的玻璃粉;以及
5至15重量份的粘合剂,
其中该铜粉的粒径大于该银粉的粒径,该铜粉的粒径为1μm至10μm,该银粉的粒径为0.1μm至2μm,以及该碳粉的比表面积为200m2/g至1000m2/g。
2.权利要求1所述的导电胶组合物,其中该粘合剂包括环氧树脂。
3.一种电极的形成方法,其包括:
将权利要求1所述的导电胶组合物施加至基板上;以及
在一般大气下高温烧结该导电胶组合物,从而在该基板上形成电极。
4.权利要求3所述的电极的形成方法,其中高温烧结该导电胶组合物的温度为600℃至900℃。
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CN113913133B (zh) * | 2021-11-09 | 2022-11-29 | 无锡创达新材料股份有限公司 | 一种导电热固性树脂组合物的应用 |
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US20150171238A1 (en) | 2015-06-18 |
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US9780236B2 (en) | 2017-10-03 |
CN104715807A (zh) | 2015-06-17 |
EP2886671A2 (en) | 2015-06-24 |
TW201525100A (zh) | 2015-07-01 |
TWI480357B (zh) | 2015-04-11 |
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