CN116745048A - 接合用导电性组合物及使用其的接合结构及其制造方法 - Google Patents
接合用导电性组合物及使用其的接合结构及其制造方法 Download PDFInfo
- Publication number
- CN116745048A CN116745048A CN202180092639.5A CN202180092639A CN116745048A CN 116745048 A CN116745048 A CN 116745048A CN 202180092639 A CN202180092639 A CN 202180092639A CN 116745048 A CN116745048 A CN 116745048A
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- Prior art keywords
- copper
- conductive composition
- bonding
- mass
- carboxylic acid
- Prior art date
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- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
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- 229910052788 barium Inorganic materials 0.000 description 1
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- ZFZQOKHLXAVJIF-UHFFFAOYSA-N zinc;boric acid;dihydroxy(dioxido)silane Chemical compound [Zn+2].OB(O)O.O[Si](O)([O-])[O-] ZFZQOKHLXAVJIF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
- B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
接合用导电性组合物是铜粉与羧酸混合而成的。所述羧酸在其结构中具有支链碳链。铜粉包含第1铜颗粒以及第2铜颗粒,所述第1铜颗粒通过扫描型电子显微镜测定的粒度分布中小于1μm的区域中的累积体积50容量%的体积累积粒径D50为0.11μm以上且小于1μm,所述第2铜颗粒通过扫描型电子显微镜测定的粒度分布中1μm以上的区域中的累积体积50容量%的体积累积粒径D50为1μm以上且10μm以下。羧酸的含量相对于所述铜粉100质量份为6质量份以上且24质量份以下。
Description
技术领域
本发明涉及接合用导电性组合物及使用其的接合结构及其制造方法。
背景技术
随着电子器件的小型化、高性能化,在电子器件内的电子电路形成中,要求尺寸稳定性、导电性、与构件的接合强度等各种性能的提高。
在专利文献1中,公开了一种以提高耐氧化性、烧结性、导电性等为目的,包含平均凝聚粒径为0.5μm~20μm的铜填料、平均凝聚粒径为50nm~200nm的铜纳米颗粒以及脂肪族羧酸的导电性填料。
在专利文献2中公开了一种导体形成组合物,其以提高导体的生产率为目的,包含含铜颗粒和脂肪酸,脂肪酸的含量相对于含铜颗粒100质量份为0.1质量份~5.8质量份。
现有技术文献
专利文献
专利文献1:国际公开第2010/032841号小册子
专利文献2:日本特开2017-204371号公报
发明内容
在专利文献1和2中公开的组合物均在作为导电体彼此的接合材料烧结使用时,所得到的接合层不能说能够充分兼顾导电性和接合强度,存在进一步改良的余地。特别是,专利文献1和2中记载的技术在无加压接合时的接合强度不充分。
因而,本发明涉及能够同时显现出高导电性和高接合强度的接合用导电性组合物。
本发明涉及一种接合用导电性组合物,其是铜粉与羧酸混合而成的,
所述羧酸在其结构中具有支链碳链,
所述铜粉包含第1铜颗粒以及第2铜颗粒,所述第1铜颗粒通过扫描型电子显微镜测定的粒度分布中小于1μm的区域中的累积体积50容量%的体积累积粒径D50为0.11μm以上且小于1μm,所述第2铜颗粒通过扫描型电子显微镜测定的粒度分布中1μm以上的区域中的累积体积50容量%的体积累积粒径D50为1μm以上且10μm以下,
所述羧酸的含量相对于所述铜粉100质量份为6质量份以上且24质量份以下。
具体实施方式
以下,基于其优选的实施方式对本发明进行说明。本发明涉及用于将导电体等电子部件用材料彼此接合的组合物、即接合用的导电性组合物。该导电性组合物用于将电子部件用材料彼此在无加压下或加压下接合,优选适合于在除成为接合对象的材料的自重所产生的力、大气压以外不施加压力的无加压下将材料彼此接合时。在以下的说明中,只要没有特别说明,则将接合用导电性组合物简称为导电性组合物。
导电性组合物是铜粉与羧酸混合而成的混合物。铜粉至少包含第1铜颗粒和第2铜颗粒这两种铜颗粒。
第1铜颗粒和第2铜颗粒均由铜元素构成,除了不可避免的杂质以外,不包含除铜元素以外的其他元素。也就是说,第1铜颗粒和第2铜颗粒分别独立地容许不可避免地微量含有除铜元素以外的其他元素、各铜颗粒的表面不可避免地被微量氧化等而不可避免地微量含有氧元素。通常,各铜颗粒中的除铜元素以外的其他元素的含量分别独立地为5质量%以下。这些元素的含量例如能够通过ICP发射光谱分析法、非活性气体融解/非分散型红外线吸收法来测定。
导电性组合物所含的铜粉优选在通过扫描型电子显微镜测定的体积基准的粒度分布中,在粒径为0.11μm以上且小于1μm的区域具有至少一个峰,且在粒径为1μm以上且10μm以下的区域具有至少一个峰。
详细而言,构成铜粉的第1铜颗粒和第2铜颗粒的粒径是在通过扫描型电子显微镜对导电性组合物中的铜粉进行测定而得到的粒度分布中,分为粒径小于1μm的区域和粒径为1μm以上的区域,由各个区域中的累积体积50容量%的体积累积粒径D50计算的。
具体而言,对于成为测定对象的导电性组合物,添加10倍等量(质量)的2-丙醇并充分搅拌后,一边残留固体成分(滤饼)一边重复仅去除上清液的清洗操作。接下来,将得到的滤饼在常温下静置使其充分干燥后,用扫描型电子显微镜确认该干燥物。
在扫描型电子显微镜的确认中,从倍率1000倍~10万倍的各粉末的扫描型电子显微镜图像中,随机选择观察到颗粒的轮廓的颗粒来测定粒径(投影面积圆相当径),计算粒度分布。接下来,将得到的粒度分布分为粒径小于1μm的区域和粒径为1μm以上的区域,由粒径小于1μm的区域的粒度分布测定累积体积50容量%的体积累积粒径D50,作为第1铜颗粒的粒径。另外,由粒径为1μm以上的区域的粒度分布测定累积体积50容量%的体积累积粒径D50,作为第2铜颗粒的粒径。上述的成为测定对象的颗粒的粒径是在小于1μm和1μm以上的各个区域中测定至少50点以上而计算的。
从防止导电性组合物中的第1铜颗粒的凝聚、使颗粒分散性适当的观点出发,通过扫描型电子显微镜测定的粒度分布中小于1μm的区域中的累积体积50容量%的第1铜颗粒的体积累积粒径D50优选为0.11μm以上。另外,从提高导电性组合物的低温烧结性的观点出发,第1铜颗粒的体积累积粒径D50优选小于1μm,更优选为0.8μm以下,进一步优选为0.6μm以下,更进一步优选为0.4μm以下。
从将导电性组合物烧结时成为致密的接合结构、接合强度容易提高的观点出发,通过扫描型电子显微镜测定的粒度分布中的1μm以上的区域中的累积体积50容量%的第2铜颗粒的体积累积粒径D50优选为1μm以上。另外,从提高将导电性组合物涂布于电子部件用材料时的涂布性的观点出发,第2铜颗粒的体积累积粒径D50优选为10μm以下,更优选为8μm以下,进一步优选为6μm以下。
第1铜颗粒和第2铜颗粒的各形状没有特别限制,能够分别独立地采用例如球状、薄片状(鳞片状)、多面体状、枝晶状(树枝状)、柱状等各种形状。从提高颗粒的填充性、即使在无加压下的接合中也充分显现出接合强度的观点出发,优选第1铜颗粒和第2铜颗粒均为球状。
关于铜颗粒是否为球状,由通过上述粒径的测定方法随机选择的各颗粒的面积S和周长L计算圆形度系数4πS/L2,进而计算其算术平均值。在圆形度系数的算术平均值为0.85以上的情况下,定义为铜颗粒是球状。
导电性组合物中的第1铜颗粒相对于第1铜颗粒和第2铜颗粒的总质量的比例优选为20质量%以上且95质量%以下,更优选为25质量%以上且90质量%以下,进一步优选为30质量%以上且80质量%以下。
同样地,第2铜颗粒相对于第1铜颗粒和第2铜颗粒的总质量的比例优选为5质量%以上且80质量%以下,更优选为10质量%以上且75质量%以下,进一步优选为20质量%以上且70质量%以下。
通过成为这样的配混比例,能够提高颗粒的填充性,即使在无加压下的接合中也能够充分地显现出接合强度。
导电性组合物包含羧酸。羧酸是在1个大气压、20℃下为液体或固体的有机酸。通过使导电性组合物中含有羧酸,构成铜粉的各铜颗粒的表面被蚀刻,能够去除在颗粒表面不可避免地形成的氧化物层、氢氧化物层,使金属铜暴露而使颗粒表面活化。另外,通过来自铜颗粒的铜与羧酸的化学反应而生成的羧酸铜能够促进铜颗粒彼此的烧结性。其结果,将导电性组合物烧结而得到的接合层能够充分地显现出金属铜所具有的导电性,并且即使在无加压下的接合中也能够充分地显现出接合强度。
作为导电性组合物所含的羧酸,可列举出具有直链碳链或支链碳链(以下,也将其简称为支链)的脂肪族或芳香族羧酸。
其中,导电性组合物所含的羧酸优选为支链的脂肪族羧酸。由此,通过由羧酸所具有的支链引起的空间位阻,铜颗粒彼此能够取得适度的距离,因此导电性组合物中的颗粒的分散性提高,并且该组合物的印刷性也提高。
作为导电性组合物所含的羧酸,可列举出具有支链的伯羧酸、仲羧酸以及叔羧酸,优选为仲羧酸或叔羧酸,进一步优选为叔羧酸。
通过使用这样的羧酸,通过羧酸的分子结构的体积大,能够适度地维持颗粒彼此的分散性,能够使导电性组合物的操作性良好。除此之外,能够充分地提高导电性组合物的烧结性,容易地得到以高水平兼顾导电性和其他构件彼此的接合强度的接合层。
另外,羧酸既可以是一元的,也可以是多元的。另外,羧酸既可以是饱和羧酸,也可以是不饱和羧酸。
作为导电性组合物所含的羧酸,从提高操作性的观点出发,优选碳原子数为4以上且18以下,更优选碳原子数为5以上且15以下,进一步优选碳原子数为6以上且13以下。
详细而言,作为适于本发明的羧酸,例如可列举出异丁酸、新戊酸、2,2-甲基丁酸、异戊酸、异己酸、异庚酸、异辛酸、异壬酸、异癸酸、新癸酸、异十三烷酸、异十四烷酸、异棕榈酸、异硬脂酸等支链且脂肪族饱和单羧酸;甲基丙烯酸等支链的脂肪族不饱和单羧酸;乌头酸等不饱和三羧酸等中的一种以上。它们能够单独使用或组合使用。
羧酸优选使用在1个大气压、20℃下为液体的羧酸。通过使用这样的羧酸,即使不另外使用后述的分散介质,羧酸本身也作为分散介质发挥功能,因此能够以高生产率得到各铜颗粒均匀分散的导电性组合物。另外,即使不使用可能成为烧结后的空隙的原因的分散介质等其他挥发成分,也能够使各铜颗粒容易地分散且维持该状态,因此能够提高导电性,并且容易地得到兼顾了其他构件彼此的高接合强度的接合层。
作为在1个大气压、20℃下为液体的羧酸,例如可列举出碳原子数为4以上且18以下的支链且脂肪族饱和单羧酸。
从以高水平兼具导电性和接合强度的观点出发,进一步优选为在1个大气压、20℃下为液体的叔饱和脂肪族单羧酸。作为这样的羧酸,可列举出2,2-二甲基丁酸、新癸酸,特别优选新癸酸。通过将这样的羧酸用于导电性组合物,即使在无加压下的接合中也能够显现出更高的接合强度。
导电性组合物中的羧酸的含量相对于铜粉100质量份优选为6质量份以上且24质量份以下,更优选为6质量份以上且20质量份以下。通过使羧酸含量在该范围内,能够使导电性组合物中的颗粒的分散性和该组合物的印刷性良好,并且能够得到制成接合结构时的高接合强度。在含有两种以上羧酸的情况下,羧酸的含量只要其总量满足上述范围即可。
作为上述导电性组合物的形态,例如为导电性浆料、导电性墨或导电性糊剂。
在含有在1个大气压、20℃下为固体的羧酸作为羧酸的情况下,从提高铜颗粒和羧酸的均匀分散性、并且提高铜颗粒彼此的分散性的观点出发,优选进一步含有分散介质。
作为能够在导电性组合物中使用的分散介质,例如可列举出水、醇、酮、酯、醚和烃、粘结剂树脂等。作为粘结剂树脂,例如可列举出丙烯酸类树脂、环氧树脂、聚酯树脂、聚碳酸酯树脂以及纤维素树脂等中的至少一种。
其中,优选丙二醇、乙二醇、己二醇、二甘醇、1,3-丁二醇、1,4-丁二醇、双丙甘醇、三丙二醇、萜品醇及二氢萜品醇等醇、以及乙基卡必醇和丁基卡必醇等醚中的至少一种。
在导电性组合物中还包含分散介质的情况下,导电性组合物中的分散介质的含量相对于铜粉100质量份优选为20质量份以下,更优选为15质量份以下,进一步优选为10质量份以下。通过使分散介质的含量为该范围,能够在导电性组合物的烧结时将空隙抑制得较少,能够提高制成接合结构时的填充性而提高接合强度。
以提高导电性组合物的填充性而得到致密的接合层、或通过高还原作用防止烧结时的铜颗粒的不希望的氧化为目的,导电性组合物还优选进一步含有烧结助剂。烧结助剂既可以单独使用,也可以多种组合使用。
作为提高导电性组合物的填充性的烧结助剂,可列举出硼硅酸玻璃、硼硅酸钡玻璃、硼硅酸锌玻璃等无机材料等。
作为具有高还原作用的烧结助剂,可列举出聚乙二醇和聚丙二醇等聚醚。这些聚醚从上述分散介质中排除。在上述有机高分子化合物中,在使用聚乙二醇的情况下,其数均分子量优选为120以上且400以下,更优选为180以上且400以下。
在导电性组合物中还包含烧结助剂的情况下,导电性组合物中的烧结助剂的含量相对于铜粉100质量份优选为20质量份以下,更优选为15质量份以下,进一步优选为10质量份以下。在含有两种以上烧结助剂的情况下,烧结助剂的含量只要其总量满足上述范围即可。通过使烧结助剂的含量为该范围,能够防止使导电性组合物烧结时的接合结构的接合强度降低。
上述各铜颗粒也可以不进行特别的表面处理。代替于此,只要发挥本发明的效果,则构成铜粉的各铜颗粒也可以实施利用有机物、无机物的覆盖或表面处理。
接下来,对导电性组合物的优选的制造方法进行说明。本制造方法具有如下工序:在包含第1铜颗粒、第2铜颗粒以及羧酸时,分别单独地制造第1铜颗粒和第2铜颗粒,然后,将第1铜颗粒、第2铜颗粒和羧酸、以及根据需要使用的分散介质和烧结助剂同时混合,或者将它们以任意的顺序添加并混合。在各原料的混合中,能够使用辊式粉碎机等公知的混合装置。
作为各铜颗粒的制造方法,能够采用湿式还原法、雾化法、电解还原法等各种方法。在使用湿式还原法、雾化法的情况下,容易得到球状的颗粒。在使用电解还原法的情况下,容易得到枝晶状、柱状的颗粒。薄片状的颗粒例如通过对球状的颗粒施加机械外力使其塑性变形而得到。
第1铜颗粒和第2铜颗粒的制造均从兼顾粒径的控制的容易性和球状的颗粒的获得容易性的观点出发,优选采用湿式还原法。湿式还原法能够采用例如日本特开2003-34802号公报、日本特开2015-168878号公报或日本特开2017-179555号公报中记载的方法。
湿式还原法是在含有例如水和优选碳原子数为1以上且5以下的一元醇的液体介质中制备含有氯化铜、乙酸铜、氢氧化铜、硫酸铜、氧化铜或氧化亚铜等一价或二价铜源的反应液。将该反应液和肼以相对于1摩尔铜优选为0.5摩尔以上且50摩尔以下的比例混合,将来自该铜源的铜离子还原,得到作为目标的第1铜颗粒或第2铜颗粒。所得到的铜颗粒根据需要也可以通过倾析法、旋转过滤法等清洗方法进行清洗。通过该方法得到的各铜颗粒是包含颗粒的集合体的浆料,或者是由该集合体构成的干燥粉末。也可以对得到的铜颗粒进一步实施上述表面处理或覆盖处理。
在湿式还原法中,为了控制铜颗粒的平均一次粒径,例如能够通过变更反应液中所含的铜离子浓度、反应液的温度等条件来容易地进行调整。由此,能够分别得到粒径互不相同的第1铜颗粒和第2铜颗粒。之后,以作为目标的铜粉具有上述粒度分布和质量比例的方式混合第1铜颗粒和第2铜颗粒即可。
从容易得到制成导电性组合物时的铜粉的粒度分布、以及第1铜颗粒和第2铜颗粒的期望的粒径的观点出发,导电性组合物的制造中使用的第1铜颗粒的平均一次粒径优选为0.11μm以上且小于1μm,更优选为0.11μm以上且0.8μm以下。
从同样的观点出发,导电性组合物的制造中使用的第2铜颗粒的平均一次粒径优选为1μm以上且10μm以下,更优选为1μm以上且8μm以下。
关于导电性组合物的制造中使用的第1铜颗粒和第2铜颗粒的平均一次粒径,例如从倍率1000倍~10万倍下的铜颗粒的扫描型电子显微镜图像中随机选择50个以上颗粒彼此不重合的颗粒来测定粒径(投影面积圆相当径),由这些测定值计算换算成球的体积平均粒径。
经过以上工序而得到的导电性组合物例如也可以将其通过预定的手段涂布于应用对象物的表面等而形成涂膜,然后,将该涂膜在无加压下或加压下加热而制成导电膜。
本发明的导电性组合物适合用作用于将各种导电体等电子部件用材料彼此接合的芯片接合用材料等这样的导电性的接合用材料。另外,除此之外,也能够用作印刷布线基板中的通孔填充用材料、将电子器件表面安装于印刷布线基板时的粘接剂。特别是,本发明的导电性组合物在无加压下的接合中能够显现出充分的接合强度。
作为接合对象物的电子部件用材料,例如可优选列举出由金、银或铜等导电性的各种金属构成的间隔件、散热板、金属线、在表面具有该金属的基板、半导体芯片等导电体。
以下对使用导电性组合物作为用于将导电体彼此接合的接合用材料的方法的一例进行说明。本方法包括如下工序:将导电性组合物配置在2个导电体之间,使所述接合用导电性组合物烧结。
首先,在第1导电体的表面涂布导电性组合物而形成涂膜。接合用组合物的涂布的手段没有特别限制,能够使用公知的涂布手段。所形成的涂膜既可以形成于第1导电体的表面的整个区域,或者也可以不连续地形成于第1导电体的表面。从更高地显现出接合强度的观点出发,优选在后述的第2导电体的配置预定区域的整个区域形成涂膜。
从形成稳定地具有高接合强度的接合结构的观点出发,所形成的涂膜的厚度在刚涂布后优选设定为1μm以上且500μm以下,更优选设定为5μm以上且300μm以下。
接下来,在涂膜上层叠第2导电体。由此,得到第1导电体和第2导电体、以及在它们之间隔着作为导电性组合物的涂膜而配置的导电性构件。
第1导电体和第2导电体分别可以是同种材料,或者也可以是种类不同的材料。
最后,在无加压下或加压下对导电性构件进行加热处理,对涂膜进行加热而使所含的铜粉烧结,由此将第1导电体与第2导电体接合。由此,能够得到形成有来自导电性组合物的接合部位的导电性的接合结构。
烧结时的气氛优选为氢、甲酸等还原气体气氛、氮、氩等非活性气体气氛。烧结温度优选低于300℃,更优选为150℃以上且低于300℃,进一步优选为200℃以上且低于300℃,更进一步优选为230℃以上且低于300℃。
烧结时间以烧结温度为所述范围为条件,优选为20分钟以上,更优选为20分钟以上且60分钟以下,进一步优选为30分钟以上且60分钟以下。
在烧结时赋予压力的情况下,优选为0.001MPa以上,更优选为0.001MPa以上且20MPa以下,进一步优选为0.01MPa以上且15MPa以下。
设为非活性气体气氛且采用了上述烧结温度条件的烧结条件是在现有技术中颗粒彼此的烧结未良好地进行且接合强度也难以显现的平缓的条件。另外,在无加压下进行接合时,铜颗粒的熔融性、颗粒彼此的缩颈的形成难以变得充分,其结果,接合强度未充分显现,或者在得到的烧结体中容易产生空隙。
关于这一点,通过使用本发明的导电性组合物,即使在上述平缓的烧结条件下,由于具有支链的羧酸的存在,铜颗粒彼此的分散性也高,另外,各铜颗粒的表面活性维持得高,因此铜颗粒彼此的烧结良好地进行,能够显现出高接合强度。另外,即使在无加压下进行接合的情况下,粒径大的第2铜颗粒也起到骨料那样的作用,且粒径小的第1铜颗粒起到填埋铜颗粒间的间隙的填料那样的作用,因此能够提高填充性。其结果,得到的烧结体的结构变得致密,不易产生空隙,能够显现出高接合强度。另外,涂膜的厚度变得均匀,不易产生接合对象物的不希望的倾斜、接合不良。除此之外,在无加压下进行接合具有能够同时接合高度不同的多个接合对象物的优点、不需要另外设置加压装置而能够降低制造成本的优点。
进而,在不含有分散介质的情况下,能够进一步减少由来自分散介质的挥发成分引起的空隙的产生,因此在烧结良好地进行、并且能够显现出更高的接合强度的方面也是有利的。
经过以上工序而形成的接合部位通过导电性组合物的烧结而形成。详细而言,接合部位是构成导电性组合物的各铜颗粒的烧结体,具有导电性。
具有这样的接合部位的接合结构有效利用其高接合强度、导电性等特性,适合用于各种电子电路、在暴露于高温的环境下使用的电子电路、例如车载用电子电路、安装有功率器件的电子电路。
实施例
以下,通过实施例对本发明进行更详细的说明。然而,本发明的范围并不限定于该实施例。在以下的表中,用“-”表示的栏表示不含有,或不实施评价。另外,“平均一次粒径”表示对于作为原料使用的各铜颗粒,通过上述方法测定的粒径。本发明的发明人确认了该值与制成导电性组合物时的各铜颗粒的体积累积粒径D50相同。
〔实施例1〕
作为铜粉,使用平均一次粒径为0.14μm的球状的第1铜颗粒(CH-0200L1,三井金属矿业株式会社制)和平均一次粒径为2.2μm的球状的第2铜颗粒(CS20,三井金属矿业株式会社制),作为质量比,使用以第1铜颗粒:第2铜颗粒=90:10的比例混合而成的铜粉。作为羧酸,使用新癸酸(瀚森公司制Versatic 10;1个大气压、20℃下为液体的支链且叔饱和脂肪族单羧酸,碳原子数10)。
相对于铜粉100质量份添加新癸酸12.99质量份,用刮刀预混炼后,使用株式会社日新基制的自转/公转真空混合器ARE-500,将以搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒)为1个循环的处理进行2个循环,进行糊剂化。将该糊剂进一步使用3根辊式粉碎机进行处理,由此进一步进行分散混合,制备糊剂状的接合用导电性组合物。
〔实施例2〕
在实施例1中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转·公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本实施例的糊剂状的接合用导电性组合物。
〔实施例3〕
将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=70:30的比例,将新癸酸的添加量相对于铜粉100质量份设为11.11质量份。除此以外,与实施例1同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔实施例4〕
在实施例3中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本实施例的糊剂状的接合用导电性组合物。
〔实施例5〕
将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=50:50的比例,将新癸酸的添加量相对于铜粉100质量份设为11.11质量份。除此以外,与实施例1同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔实施例6〕
在实施例5中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本实施例的糊剂状的接合用导电性组合物。
〔实施例7〕
将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=30:70的比例,将新癸酸的添加量相对于铜粉100质量份设为8.11质量份。除此以外,与实施例1同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔实施例8〕
在实施例7中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本实施例的糊剂状的接合用导电性组合物。
〔比较例1〕
除了将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=10:90的比例以外,与实施例3同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔比较例2〕
除了将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=10:90的比例以外,与实施例4同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔比较例3〕
不含有羧酸,将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=50:50的比例,相对于铜粉100质量份,添加11.11质量份的萜品醇作为分散介质。除此以外,与实施例1同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔比较例4〕
在比较例3中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本比较例的糊剂状的接合用导电性组合物。
〔比较例5〕
相对于铜粉100质量份添加11.11质量份的癸酸(直链碳链的伯饱和羧酸,碳原子数10,富士胶片和光纯药公司制)作为羧酸,相对于铜粉100质量份添加7.41质量份的萜品醇作为分散介质,除此以外,与实施例5同样地制备糊剂状的导电性组合物。
〔实施例9~11和比较例6〕
相对于铜粉100质量份,以以下表1所示的量添加新癸酸的添加量,除此以外,与实施例5同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔实施例12〕
代替实施例5中使用的第1铜颗粒,使用平均一次粒径为0.16μm的球状的第1铜颗粒(CH-0200,三井金属矿业株式会社制),除此以外,与实施例5同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔实施例13〕
在实施例12中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本实施例的糊剂状的接合用导电性组合物。
〔比较例7〕
不含有羧酸,将第1铜颗粒与第2铜颗粒的质量比设为第1铜颗粒:第2铜颗粒=50:50的比例,相对于铜粉100质量份,添加11.11质量份的萜品醇作为分散介质。除此以外,与实施例12同样地进行预混炼、糊剂化以及分散混合,制备糊剂状的接合用导电性组合物。
〔比较例8〕
在比较例7中制作的导电性组合物中,相对于铜粉100质量份进一步添加1质量份的烧结助剂(聚乙二醇300(PEG300)),使用株式会社日新基制的自转/公转真空混合器ARE-500,实施1个循环的搅拌模式(1000rpm×1分钟)和脱泡模式(2000rpm×30秒),制备本比较例的糊剂状的接合用导电性组合物。
〔导电性的评价〕
将实施例和比较例的导电性组合物分别以10mm×20mm的尺寸涂布在玻璃板上,接下来,在260℃下进行30分钟烧结,制造作为导电性组合物的烧结体的导电膜。对于该导电膜,使用Mitsubishi Chemical Analytech Co.,Ltd.制的四探针法电阻率测定装置即Loresta MCP-T600,测定电阻率(μΩ·cm)。需要说明的是,关于比较例5的导电性组合物,由于经时变化而固体化,无法对玻璃板进行印刷,因此未实施导电性的评价。将结果示于以下的表1。
〔接合强度的评价〕
在铜制的引线框(厚度2.0mm)的芯片搭载部上,通过丝网印刷涂布实施例或比较例的导电性组合物而形成涂膜。涂膜形成为5mm见方的正方形。涂膜的厚度为100μm。
接下来,在涂膜上载置2mm见方的正方形的SiC芯片(厚度0.37mm),以涂膜的厚度成为50μm的方式用数显指示器(三丰公司制)进行调整。然后,在氮气氛下在260℃下进行30分钟烧结,制造在铜板与SiC芯片之间形成有导电性组合物的烧结体的接合结构。
对于通过上述方法得到的接合结构,分别测定断裂强度。测定中使用XYZTEC公司制的Bond Tester Condor Sigma。断裂强度(MPa)是由断裂载荷(N)/接合面积(mm2)定义的值。需要说明的是,关于比较例5的导电性组合物,如上所述发生了固体化,因此未实施接合强度的评价。将结果示于以下的表1。
[表1]
产业上的可利用性
根据本发明,提供一种能够同时显现出高导电性和高接合强度的接合用导电性组合物。
Claims (7)
1.一种接合用导电性组合物,其是铜粉与羧酸混合而成的,
所述羧酸在其结构中具有支链碳链,
所述铜粉包含第1铜颗粒以及第2铜颗粒,所述第1铜颗粒通过扫描型电子显微镜测定的粒度分布中小于1μm的区域中的累积体积50容量%的体积累积粒径D50为0.11μm以上且小于1μm,所述第2铜颗粒通过扫描型电子显微镜测定的粒度分布中1μm以上的区域中的累积体积50容量%的体积累积粒径D50为1μm以上且10μm以下,
所述羧酸的含量相对于所述铜粉100质量份为6质量份以上且24质量份以下。
2.根据权利要求1所述的接合用导电性组合物,其中,所述羧酸为碳原子数4以上且18以下的脂肪族一元羧酸。
3.根据权利要求1或2所述的接合用导电性组合物,其中,所述羧酸为叔羧酸。
4.根据权利要求1~3中任一项所述的接合用导电性组合物,其中,所述羧酸在1个大气压、20℃下为液体。
5.根据权利要求1~4中任一项所述的接合用导电性组合物,其中,所述羧酸为新癸酸。
6.一种接合结构,其具备第1导电体、第2导电体以及将第1导电体与第2导电体接合的接合部位,
所述接合部位由权利要求1~5中任一项所述的接合用导电性组合物的烧结体构成。
7.一种接合结构的制造方法,其包括如下工序:将权利要求1~5中任一项所述的接合用导电性组合物配置于2个导电体之间,使所述接合用导电性组合物烧结。
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