CN109072012A - 导电性粘接剂 - Google Patents

导电性粘接剂 Download PDF

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Publication number
CN109072012A
CN109072012A CN201780024674.7A CN201780024674A CN109072012A CN 109072012 A CN109072012 A CN 109072012A CN 201780024674 A CN201780024674 A CN 201780024674A CN 109072012 A CN109072012 A CN 109072012A
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CN
China
Prior art keywords
amine
metal microparticle
conductive adhesive
protective layer
carbon atom
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201780024674.7A
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English (en)
Inventor
森崇充
三并淳郎
三并淳一郎
岩佐成人
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cao Da Osaka
Osaka Soda Co Ltd
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Cao Da Osaka
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Filing date
Publication date
Application filed by Cao Da Osaka filed Critical Cao Da Osaka
Priority to CN202311099183.2A priority Critical patent/CN117285876A/zh
Publication of CN109072012A publication Critical patent/CN109072012A/zh
Pending legal-status Critical Current

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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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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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    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
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    • 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
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Abstract

本发明提供一种导电性粘接剂，其可获得不易产生烧结造成的破裂或缺陷等且机械强度优异的烧结体。一种导电性粘接剂，含有金属微粒子A，所述金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，NH2‑R2‑O‑R1…(1)[式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基]，所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。

Description

导电性粘接剂
技术领域
本发明涉及导电性粘接剂、其制造方法、该导电性粘接剂的烧结体及部件间具备该烧结体的电路或装置。
背景技术
以芯片接合(die bond)或芯片贴装(die attach)剂等为主的导电性粘接剂是用于半导体、LED、功率半导体等的接合材料。作为接合方式，一般已知有利用加压与加热的接合，或利用无加压的加热等的烧结而与基材接合的方式。近年来，从制造工艺的简便性或效率的观点出发，无加压方式的接合材料的开发正在进展。
作为无加压方式的接合材料，可举出一个是含有环氧树脂的导电性粘接剂。该接合材料是以低温处理使环氧树脂固化而使用的材料，可以抑制孔洞的发生或提高与基材的接合强度(专利文献1)。然而，因为环氧树脂本身成为电阻体，所以得到的导电性或热传导性会变低。
另一方面，作为不含有环氧树脂等热固化性树脂的接合材料，可举出仅由银构成的导电性粘接剂。该接合材料使用微米银、或次微米银(粒径300～900nm)(专利文献2)，但容易产生孔洞，作为通常的烧结反应，需要在200～250℃下进行1小时的处理。因此，需要开发可以在更低温且短时间的处理来获得高抗剪强度(接合性高的材料)，且可抑制孔洞的发生的接合材料。
近年来，银纳米微粒子的开发正在进展，银纳米微粒子有在低温且短时间的热处理下易于烧结的特征。特别是在使用粒径在20nm左右的银纳米微粒子的情况下，可以在较低温(200℃)下易于烧结，形成致密的膜。
然而，接合材料中混入较多20nm左右的粒子的情况下，随着膜厚度变厚而涂膜产生应力，其结果产生破裂或缺陷。因此，寻求开发涂膜的应力少的材料。
作为满足该要求的材料，提出有含有纳米尺寸的金属纳米微粒子的导电性粘接剂(例如参照专利文献3)。
现有技术文献
专利文献
专利文献1：国际公开2010/18712
专利文献2：国际公开2014/104046
专利文献3：日本特开2006-83377号公报
发明内容
发明要解决的技术问题
含有纳米尺寸的金属纳米微粒子的导电性粘接剂，在配置于部件间的状态下，可以一边利用加热至高温(例如200℃以上)而烧结的烧结体将部件间粘接，一边发挥高的导电性。
然而，本发明者进行检讨时发现，用含有纳米尺寸的银微粒子的现有的导电性粘接剂获得的烧结体中发生破裂、缺陷等，机械性强度降低。特别是从进一步提高导电性的观点出发，发现在延长烧结时的加热时间或提高加热温度时，烧结体的破裂或缺陷的问题更显著地发生。
在这样的状态下，本发明的主要目的在于，提供一种导电性粘接剂，其可获得不易产生烧结造成的破裂或缺陷等且机械性强度优异的烧结体。进而，本发明目的在于，提供导电性粘接剂的制造方法、导电性粘接剂的烧结体及部件间具备该烧结体的电路或装置。
用于解决问题的技术方案
本发明者为了解决上述课题而进行了深入研究。其结果发现，包含具备含特定胺的保护层且具有特定范围平均粒径的金属微粒子的导电性粘接剂，可以获得导电性粘接剂烧结体的破裂或缺陷被有效抑制且机械性强度优异的烧结体。更具体而言，发现导电性粘接剂具备含胺的保护层且含有平均粒径为30nm～300nm的金属微粒子A，所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，进而，所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内的导电性粘接剂，可以获得导电性粘接剂的烧结体破裂或缺陷被有效抑制且机械性强度优异的烧结体。
NH2-R2-O-R1…(1)
[式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基。]
进而发现，这种烧结体具备高的导电性且粘接性优异。本发明是基于这样的见解，进一步反复检讨而完成的发明。
即，本发明提供下述公开方式的发明。
项1.一种导电性粘接剂，其含有金属微粒子A，所述金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，
所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，
NH2-R2-O-R1…(1)
[式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基。]
所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。
项2.根据项1所述的导电性粘接剂，其中，所述保护层还含有脂肪酸。
项3.根据项1或2所述的导电性粘接剂，其中，所述导电性粘接剂还含有溶剂。
项4.一种烧结体，其为项1～3中任一项所述的导电性粘接剂的烧结体。
项5.一种电路或装置，其具备部件间通过项4所述的烧结体粘接的部分。
项6.一种导电性粘接剂的制造方法，其中，使用金属微粒子A，所述导电性粘接剂的制造方法具备混合所述金属微粒子A的工序，所述金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，其中，
所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，
NH2-R2-O-R1…(1)
[式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基。]
所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100：0～10：90的范围内。
项7.根据项6所述的导电性粘接剂的制造方法，其还具备：
准备金属微粒子的工序，所述金属微粒子具备含胺的保护层，且平均粒径为30nm～300nm；
制备所述金属微粒子A的工序，将该金属微粒子的保护层中所含的胺与碳原子数5～7的单烷基胺及通式(1)所示的烷氧基胺进行置换，将碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率调整成为在100:0～10:90的范围内，制备所述金属微粒子A。
项8.一种部件的粘接方法，其具备：
将项1～6中任一项所述的导电性粘接剂配置于部件间的工序、
将所述导电性粘接剂加热而烧结的工序。
发明效果
根据本发明，可以提供一种导电性粘接剂，其可以获得不易产生烧结所致的破裂或缺陷，且机械性强度(抗剪强度)优异的烧结体。进而，根据本发明，可以提供该导电性粘接剂的制造方法、该导电性粘接剂的烧结体及部件间具备该烧结体的电路或装置。
具体实施方式
本发明的导电性粘接剂的特征在于，含有金属微粒子A，该金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，上述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，上述保护层中，上述碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。
NH2-R2-O-R1…(1)
[式中，R1是表示碳原子数1～4的烷基，R2是表示碳原子数1～4的亚烷基。]
以下详述本发明的导电性粘接剂、该导电性粘接剂的制造方法、该导电性粘接剂的烧结体及部件间具备该烧结体的电路或装置。
1.导电性粘接剂
本发明的导电性粘接剂以规定比率含有上述金属微粒子A。
金属微粒子A
本发明的金属微粒子A具备含胺的保护层，平均粒径在30nm～300nm。如后所述，金属微粒子A在由金属构成的粒子(金属粒子)的表层上具有该保护层。
另外，金属微粒子A的保护层中所含的胺包含碳原子数5～7的单烷基胺(以下有时候称为“C5-7的单烷基胺”)及上述通式(1)所示的烷氧基胺(以下有时候称为“烷氧基胺(1)”)中的至少一方。进而，保护层中，碳原子数5～7的单烷基胺和/或通式(1)所示的烷氧基胺与不同于这些胺的胺的比率(C5-7的单烷基胺和/或烷氧基胺(1)的合计:不同于C5-7的单烷基胺和/或烷氧基胺(1)的胺的合计)在100:0～10:90的范围内。
本发明的金属微粒子A的平均粒径只要在30nm～300nm范围内，则可无特别限制地使用，优选为30nm～250nm范围，更优选为30nm～230nm范围。在平均粒径小于30nm时，不能得到充分的机械性强度(抗剪强度)，在大于300nm时，不能得到充分的导电性。此外，本发明中的金属微粒子A的平均粒径不只是单独使用具有上述范围的平均粒径的金属微粒子，或使用组合多个具有上述范围的平均粒径的金属微粒子的情况，也可包含混合上述范围外的平均粒径的金属微粒子，而成为上述范围的平均粒径的情况。
进而，特别是从发挥高的机械强度(抗剪强度)的观点来看，金属微粒子A中，保护层中所含的胺包含碳原子数5～7的单烷基胺(特别优选正己胺)，且包含平均粒径180nm～210nm范围的金属微粒子S。该金属微粒子S的保护层中所含的胺优选包含80％以上碳原子数5～7的单烷基胺，更优选包含90％以上。另外，金属微粒子A中的该金属微粒子S的比率优选为20质量％以上。
此外，本发明的金属微粒子中的保护层中所含的胺的量可通过后述测定方法求得。
进而，金属微粒子A实质上也可以只由金属微粒子S构成(金属微粒子S的比率为99质量％以上)，也可以包含其它金属微粒子。作为与该金属微粒子S一同含有的金属微粒子，优选保护层中所含的胺包含碳原子数5～7的单烷基胺(特别优选为正己胺)，且平均粒径50nm～100nm范围的金属微粒子P。该金属微粒子P的保护层中所含的胺优选包含80％以上的碳原子数5～7的单烷基胺，更优选包含90％以上。另外，金属微粒子A中的该金属微粒子P的比率优选为20质量％～80质量％的程度。
将具有上述范围的平均粒径的金属微粒子组合多个而使用时，可任意选择具有上述范围的平均粒径的金属微粒子，可以组合不同的平均粒径的金属微粒子而构成金属微粒子A。作为不同的平均粒径的组合，例如，可以例示平均粒径为30nm以上、小于100nm(优选平均粒径为30nm以上、小于100nm的范围，更优选平均粒径为50nm以上、小于100nm的范围)的平均粒径的金属微粒子(例如平均粒径小的金属微粒子(I))与平均粒径为100nm以上、300nm以下(优选平均粒径为100nm以上、250nm以下的范围，更优选平均粒径为100nm以上、230nm以下的范围)的金属微粒子(例如平均粒径大的金属微粒子(Ⅱ))的组合。组合不同的平均粒径的金属微粒子使用时的比率可适当选择，但只要平均粒径小的金属微粒子(I)与平均粒径大的金属微粒子(Ⅱ)的质量比(I:Ⅱ)在99:1～1:99的范围即可，优选为90:10～10:90的范围，更优选为90:10～20:80的范围，进一步优选为90:10～40:60的范围。
进而，作为金属微粒子，可以组合上述平均粒径范围外(30nm～300nm范围外，例如小于30nm、1～25nm、超过300nm、超过300nm且500nm以下程度)的金属微粒子使用。组合上述平均粒径范围外的金属微粒子使用时，只要混合金属微粒子后的平均粒径在上述平均粒径范围内，就不特别限制上述平均粒径范围外的金属微粒子的添加量，例如，相对于金属微粒子总量，只要为15质量％以下即可，优选为10质量％以下，更优选为5质量％以下。
上述平均粒径范围外的金属微粒子优选具有保护层。该金属微粒子的保护层中，可以使用上述C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率在100:0～10:90的范围内的材料，也可使用该范围外的材料。此外，上述平均粒径范围外的金属微粒子的保护层也可以由后述可以用作金属微粒子A保护层的成分构成。
在本发明中，金属微粒子A的平均粒径是用扫描型电子显微镜观察的图像中所含30个以上粒子的长边的长度的平均值。此外，关于本发明的金属微粒子A，在使用单独平均粒径的金属微粒子时，可以设为用扫描型电子显微镜观察的图像中所含任意30个以上粒子的长边的长度的平均值。另外，组合不同平均粒径的金属微粒子使用时的平均粒径可以通过用扫描型电子显微镜观察的图像中所含的各金属微粒子30个以上的粒子的长边的长度的平均值和各金属微粒子的混合比率而求得。
更具体而言，例如在组合2种不同的平均粒径的金属微粒子使用时，可以假设金属微粒子的真密度为一定，通过下式(A)来求得。
已混合的金属微粒子的平均粒径＝2×((A/R1 2+B/R2 2)/(A/R1 3+B/R2 3))…(A)
[式中，平均粒径小的金属微粒子:平均粒径大的金属微粒子的比率以A:B表示，平均粒径小的金属微粒子的半径以R1表示，平均粒径大的金属微粒子的半径以R2表示。]
另外，例如组合3种不同的平均粒径的金属微粒子使用时，可假设金属微粒子的真密度为一定，通过下式(B)来求得。
已混合的金属微粒子的平均粒径＝2×((A/R1 2+B/R2 2+C/R3 2)/(A/R1 3+B/R2 3+C/R3 3))…(B)
[式中，平均粒径小的金属微粒子:中间的平均粒径的金属微粒子:平均粒径大的金属微粒子的比率以A:B:C表示，平均粒径小的金属微粒子的半径以R1表示，中间的平均粒径的金属微粒子的半径以R2表示，平均粒径大的金属微粒子的半径以R3表示。]
在本发明的导电性粘接剂中，作为金属微粒子的含量，没有特别限制，但可举出优选为80质量％以上，更优选为85质量％～95质量％的程度。
作为本发明的金属微粒子A的金属种类，可例示金、银、铜、铂、钯、镍、铝等。其中，从导电性的观点出发，优选为金、银、铂，从成本及低温烧结性的观点出发，优选为银、铜、镍，特别优选为银。
本发明的金属微粒子A在由金属构成的粒子(金属粒子)表层具有保护层。作为形成保护层的材料，只要是可形成金属粒子表层且可作为保护层发挥功能的材料(例如抑制金属微粒子A之间的聚集的层)即可，没有特别限制，但从提高导电性粘接剂烧结体的机械性强度的效果的观点出发，优选可举出脂肪酸、胺、羟基脂肪酸等。保护层可以由1种材料构成，也可由2种以上的材料构成。
脂肪酸
作为保护层中的脂肪酸，没有特别限制，可举出优选为烷基的碳原子数为3以上18以下的脂肪酸，更优选为烷基的碳原子数在4以上18以下的脂肪酸。作为脂肪酸的优选的具体例，可举出：醋酸、丙酸、丁酸、戊酸、己酸、辛酸、2-乙基己酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、油酸、亚油酸、α-亚麻酸等。另外，作为脂肪酸的具体例，也可举出如环己烷甲酸这样的环状烷基羧酸等。这些中，从提高导电性粘接剂烧结体的机械性强度的效果出发，优选为己酸、2-乙基己酸、油酸、亚油酸、α-亚麻酸。保护层中的脂肪酸可以由1种脂肪酸构成，也可由2种以上的脂肪酸构成。
胺
金属微粒子A的保护层中所含的胺的特征在于，包含C5-7的单烷基胺及烷氧基胺(1)中的至少一方。作为保护层中所含的胺，只要是包含C5-7单烷基胺(特别优选碳原子数6的单烷基胺)及烷氧基胺(1)的至少一方，就可以没有特别问题地使用。此外，保护层中的胺可以只由C5-7的单烷基胺及烷氧基胺(1)的至少一方形成，也可包含这些以外的胺。
保护层中，C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率只要在100:0～10:90的范围内即可，优选在100:0～20:80的范围内，更优选在100:0～30:70的范围内，进一步优选在100:0～40:60的范围内，特别优选在100:0～50:50的范围内。如果在上述范围，则烧结时可获得机械性强度(抗剪强度)优异的烧结体。
此外，保护层中所含的各胺的比率可以根据气相色谱计算。具体而言，使金属微粒子1g分散于4g的甲醇后，加入数滴浓盐酸并充分搅拌使保护层中的胺游离于甲醇中，用氢氧化钠中和处理该溶液后，将其导入至气相色谱仪。可以根据由色谱法得到的胺的峰面积来定量各胺比率。保护层中所含的胺的量根据上述测定方法得到的峰面积的值，以含量(％)表示。
作为碳原子数5～7的单烷基胺，可例示：正戊胺、正己胺、正庚胺、环己胺、环庚胺等。其中，优选正戊胺、正己胺、正庚胺，特别优选正己胺。保护层中C5-7的单烷基胺可以由1种单烷基胺构成，也可由2种以上的单烷基胺构成。
另外，上述通式(1)中，如果R1是碳原子数1～4的烷基，则可以是直链或支链任一方，且优选为碳原子数1～3的烷基，更优选为甲基、乙基、丙基、异丙基。如果R2是碳原子数1～4的烷基，则可以是直链或支链任一方，且优选为碳原子数1～3的烷基，更优选为甲基、乙基、丙基、异丙基。上述通式(1)表示的烷氧基胺可以由1种烷氧基胺构成，也可由2种以上的烷氧基胺构成。
作为上述通式(1)表示的烷氧基胺的具体例，可例示：1-甲氧基甲胺、1-乙氧基甲胺、1-丙氧基甲胺、1-异丙氧基甲胺、1-丁氧基甲胺、2-甲氧基乙胺、2-乙氧基乙胺、2-丙氧基乙胺、2-异丙氧基乙胺、2-丁氧基乙胺、3-甲氧基丙胺、3-乙氧基丙胺、3-丙氧基丙胺、3-异丙氧基丙胺、3-丁氧基丙胺、4-甲氧基丁胺、4-乙氧基丁胺、4-丙氧基丁胺、4-异丙氧基丁胺、4-丁氧基丁胺等。其中，优选2-乙氧基乙胺、2-丙氧基乙胺、2-异丙氧基乙胺、2-丁氧基乙胺、3-甲氧基丙胺、3-乙氧基丙胺、3-丙氧基丙胺、3-异丙氧基丙胺。
保护层中所含的胺可以仅为C5-7的单烷基胺及烷氧基胺(1)中的任意一方，也可以包含两方。包含两方时的比率没有特别限制，可以以任意比率包含，作为比率例如可举出70:30～30:70等。
如上述，保护层中所含的胺中也可以包含与C5-7的单烷基胺和/或烷氧基胺(1)不同的胺。此外，本发明的导电性粘接剂中，金属微粒子A的保护层中所含的胺因为在导电性粘接剂烧结时从金属微粒子A的表面脱离，所以不会对获得的烧结体的导电性带来实质的影响。
保护层中所含的胺中，作为与C5-7的单烷基胺和/或烷氧基胺(1)不同的胺的具体例，没有特别限制，可例示伯胺、仲胺、叔胺，进而可例示一个化合物中有2个氨基的二胺化合物等。
作为伯胺，可例示：乙胺、正丙胺、异丙胺、1,2-二甲基丙胺、正丁胺、异丁胺、仲丁胺、叔丁胺胺、异戊胺、正辛胺、2-辛胺、叔辛胺、2-乙基己胺、正壬胺、正癸胺、正十一烷胺、正十二烷胺、正十三烷胺、2-十三烷胺、正十四烷胺、正十五烷胺、正十六烷胺、正十七烷胺、正十八烷胺、正油基胺、3-甲氧基丙胺、3-乙氧基丙胺、3-丙氧基丙胺、3-异丙氧基丙胺、3-丁氧基丙胺、N-乙基-1,3-二氨基丙烷、N,N-二异丙基乙胺、N,N-二甲基-1,3-二氨基丙烷、N,N-二丁基-1,3-二氨基丙烷、N,N-二异丁基-1,3-二氨基丙烷、N-月桂基二氨基丙烷等具有直链或支链烃基的胺等。
另外，也可以例示作为脂环胺的环丙胺、环丁胺、环丙胺、环己胺、环庚胺、环辛胺或作为芳族胺的苯胺等。
另外，也可以例示3-异丙氧基丙胺、异丁氧基丙胺等醚胺。
作为仲胺，可例示：N,N-二丙基胺、N,N-二丁基胺、N,N-二戊基胺、N,N-二己基胺、N,N-二庚基胺、N,N-二辛基胺、N,N-二壬基胺、N,N-二癸基胺、N,N-二(十一烷基)胺、N,N-二(十二烷)基胺、N,N-二硬脂基胺、N-甲基-N-丙胺、N-乙基-N-丙胺、N-丙基-N-丁胺等二烷基单胺及哌啶等环状胺。
作为叔胺，可例示：三乙胺、三丁胺、三己胺、二甲基辛胺、二甲基癸基胺、二甲基月桂基胺、二甲基肉豆蔻基胺、二甲基棕榈基胺、二甲基硬脂酰基胺、二月桂基单甲基胺等。
进而，作为不同的胺，可使用一个化合物中有两个氨基的二胺化合物。作为二胺化合物，可例示：乙二胺、N,N-二甲基乙二胺、N,N'-二甲基乙二胺、N,N-二乙基乙二胺、N,N'-二乙基乙二胺、1,3-丙二胺、2,2-二甲基-1,3-丙二胺、N,N-二甲基-1,3-丙二胺、N,N'-二甲基-1,3-丙二胺、N,N-二乙基-1,3-丙二胺、N,N'-二乙基-1,3-丙二胺、1,4-丁二胺、N,N-二甲基-1,4-丁二胺、N,N'-二甲基-1,4-丁二胺、N,N-二乙基-1,4-丁二胺、N,N'-二乙基-1,4-丁二胺、1,5-戊二胺、1,5-二氨基-2-甲基戊烷、1,6-己二胺、N,N-二甲基-1,6-己二胺、N,N'-二甲基-1,6-己二胺、1,7-庚二胺、1,8-辛二胺等。
其中，从有效提高导电性粘接剂烧结体的机械性强度的观点出发，优选为正丁胺、正辛胺、N,N-二甲基-1,3-二氨基丙烷、N,N-二乙基-1,3-二氨基丙烷等。保护层中的不同的胺可以包含上述的1种胺，也可包含2种以上的胺。
保护层中，在并用胺与脂肪酸时，作为胺与脂肪酸的摩尔比(胺:脂肪酸)，优选为约90:10～约99.9:0.1的范围，更优选为约95:5～约99.5:0.5的范围。
进而，本发明中的金属微粒子A的保护层中可以含有羟基脂肪酸，作为保护层中可含有的羟基脂肪酸，作为羟基脂肪酸，可使用碳原子数3～24，且具有1个以上(例如1个)羟基的化合物。作为羟基脂肪酸，例如可举出：2-羟基癸酸、2-羟基十二烷酸、2-羟基十四烷酸、2-羟基十六烷酸、2-羟基十八烷酸、2-羟基二十烷酸、2-羟基二十二烷酸、2-羟基二十三烷酸、2-羟基二十四烷酸、3-羟基己酸、3-羟基辛酸、3-羟基壬酸、3-羟基癸酸、3-羟基十一烷酸、3-羟基十二烷酸、3-羟基十三烷酸、3-羟基十四烷酸、3-羟基十六烷酸、3-羟基十七烷酸、3-羟基十八烷酸、ω-羟基-2-癸烯酸、ω-羟基十五烷酸、ω-羟基十七烷酸、ω-羟基二十烷酸、ω-羟基二十二烷酸、6-羟基十八烷酸、蓖麻油酸、12-羟基硬脂酸、[R-(E)]-12-羟基-9-十八碳烯酸等。其中，优选为碳原子数4～18且在ω位以外(特别是12位)具有1个羟基的羟基脂肪酸，更优选为蓖麻油酸、12-羟基硬脂酸。第2保护层中所含的羟基脂肪酸可以为1种类，也可以为2种以上。
保护层中，含有羟基脂肪酸时，羟基脂肪酸的含量相对于1摩尔的胺，只要在0.1～10摩尔的范围即可，优选为0.2～5摩尔的范围。
作为金属微粒子A中的保护层的比率(质量％)，没有特别限制，但从保护金属微粒子A的表面并有效提高导电性粘接剂烧结体的机械性强度的观点出发，优选为0.1质量％～10质量％的程度，更优选为0.2质量％～8质量％的程度，特别优选为0.2质量％～5质量％的程度。
本发明中使用的金属微粒子A只要是具有上述特征的金属微粒子，则也可以购买市售的金属微粒子使用，通常，也可以使用根据所使用的金属微粒子(例如银微粒子)的制造方法(例如特开2015-40319号公报)所制造的金属微粒子。此外，关于金属微粒子的制造方法，之后详细描述。另外，本发明的金属微粒子A也可以使用下述金属微粒子：利用保护层中的C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率在100:0～10:90范围外的金属微粒子，并通过后述方法将该比率调整在100:0～10:90范围内的金属微粒子。
溶剂
本发明的导电性粘接剂，除金属微粒子A之外，优选还含有溶剂。通过含有溶剂，流动性提高，易于将本发明的导电性粘接剂配置于期望的场所。
作为溶剂，只要可以分散金属微粒子A，就没有特别限制，但优选含有极性有机溶剂。作为极性有机溶剂，可举出：丙酮、乙酰丙酮、甲基乙基酮等酮类；二乙基醚、二丙基醚、二丁基醚、四氢呋喃、1,4-二噁烷等醚类；1,2-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、1,2-己二醇、1,6-己二醇、1,2-戊二醇、1,5-戊二醇、2-甲基-2,4-戊二醇、3-甲基-1,5-戊二醇、1,2-辛二醇、1,8-辛二醇、2-乙基-1,3-己二醇等二元醇类；甘油；碳原子数1～5的直链或支链的醇、环己醇、3-甲氧基-3-甲基-1-丁醇、3-甲氧基-1-丁醇等醇类；醋酸乙酯、醋酸丁酯、丁酸乙酯、甲酸乙酯等脂肪酸酯类；聚乙二醇、三乙二醇单甲醚、四乙二醇单甲醚、乙二醇单乙醚、二乙二醇单乙醚、二乙二醇二甲醚、三乙二醇二甲醚、四乙二醇二甲醚、3-甲氧基丁基乙酸酯、乙二醇单丁醚、乙二醇单丁醚乙酸酯、乙二醇单己醚、乙二醇单辛醚、乙二醇单-2-乙基己基醚、乙二醇单芐醚、二乙二醇单甲醚、二乙二醇单甲醚乙酸酯、二乙二醇单乙醚、二乙二醇单乙醚乙酸酯、二乙二醇单丁醚、二乙二醇单丁醚乙酸酯、聚丙二醇、丙二醇单丙醚、丙二醇单丁醚、二丙二醇单甲醚、二丙二醇单乙醚、二丙二醇单丙醚、二丙二醇单丁醚、三丙二醇单甲醚、三丙二醇单乙醚、三丙二醇单丙醚、三丙二醇单丁醚等二醇类或二醇醚类；N,N-二甲基甲酰胺、二甲亚砜；萜品醇等萜类；乙腈；γ-丁内酯；2-吡咯烷酮；N-甲基吡咯烷酮；N-(2-氨基乙基)哌嗪等。这些中，从进一步提高导电性粘接剂烧结体的机械性强度的观点出发，优选碳原子数3～5的直链或支链的醇、3-甲氧基-3-甲基-1-丁醇、3-甲氧基-1-丁醇、二乙二醇单丁醚、二乙二醇单丁醚乙酸酯、萜品醇。
溶剂除极性有机溶剂之外，还可以含有非极性或疏水性溶剂。作为非极性有机溶剂，可举出：己烷、庚烷、辛烷、壬烷、癸烷、2-乙基己烷、环已烷等直链、分枝或环状的饱和碳烃化合物；碳原子数6以上的直链或支链的醇等醇类；苯、甲苯、苯甲腈等芳香族化合物；二氯甲烷、氯仿、二氯乙烷等卤化烃化合物类；甲基-正戊基酮；甲基乙基酮肟；三乙酸甘油酯等。这些中，优选为饱和烃化合物及碳原子数6以上的直链或支链的醇类，更优选为己烷、辛烷、癸烷、辛醇、癸醇、十二醇。溶剂可以单独使用1种或混合2种以上使用。
在含有极性有机溶剂与非极性有机溶剂双方的情况下，极性有机溶剂的比率相对于溶剂总量，优选为5容量％以上，更优选为10容量％以上，进一步优选为15容量％以上。另外，可设为60容量％以下，也可以设为55容量％以下，也可以设为50容量％以下。溶剂也可以仅由极性有机溶剂构成。本发明的导电性粘接剂如上述含有较多极性有机溶剂的情况下，金属微粒子A的分散性良好。
本发明的导电性粘接剂中，作为溶剂的比率，没有特别限制，优选为20质量％以下，更优选为5质量％～15质量％的程度。
本发明的导电性粘接剂可以通过具备混合金属微粒子A(更具体而言，混合金属微粒子A与溶剂)的工序的方法来制造，该金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm。本发明的导电性粘接剂的制造方法中，使用上述金属微粒子A，该金属微粒子A中，上述胺包含碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺，在上述保护层中，上述碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。
另外，在本发明的导电性粘接剂的制造方法中，还可以具备：准备具备含胺的保护层且平均粒径在30nm～300nm的金属微粒子，将该金属微粒子的保护层中所含的胺置换成碳原子数5～7的单烷基胺和/或通式(1)所示的烷氧基胺，并将碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率调整成在100:0～10:90的范围内，制备上述金属微粒子A的工序。作为将胺置换而制备金属微粒子A的方法，例如可以采用后述的方法。
2.金属微粒子A的制造方法
以下示出本发明中使用的金属微粒子A(例如银微粒子)的制造方法的一例。
首先，准备用于制造金属微粒子A的组合物(银微粒子制备用组合物)。具体而言，准备成为银微粒子原料的银化合物(优选为硝酸银、草酸银等)、构成保护层的成分(上述脂肪酸、胺、羟基脂肪酸等)及有机溶剂。接着，混合这些各成分而获得银微粒子制备用组合物。该组合物中的各成分的比率只要适当调整成上述金属微粒子A的构成即可。例如，组合物中的草酸银的含量优选相对于组合物总量为20～70质量％的程度。另外，保护层中含有脂肪酸时，作为脂肪酸的含量，优选相对于组合物总量为0.1质量％～20质量％的程度。作为保护层中胺的含量，优选相对于组合物总量为在5质量％～55质量％的程度。保护层中含有羟基脂肪酸时，作为羟基脂肪酸的含量，优选相对于组合物总量为0.1质量％～15质量％的程度。
此外，胺只要调整成C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率在上述范围内使用即可。另外，保护层中的该比率也可以使用调整成在上述范围外的银微粒子制备用组合物来合成银微粒子，且通过后述方法将该比率调整(将胺置换)至上述范围内。
另外，各成分的混合方法也没有特别限制，例如，可以利用机械搅拌器、磁力搅拌器、涡旋混合器、行星式磨机、球磨机、三辊磨机、管路型混合器、行星式混合器、溶解器等通用的装置来混合。为了避免因混合时的溶解热、摩擦热等的影响使组合物温度上升，银微粒子的热分解反应开始，优选将组合物的温度抑制在例如60℃以下，特别是40℃以下混合。
接着，将银微粒子制备用组合物在反应容器内反应，通常通过供给利用加热进行的反应，由此引起银化合物的热分解反应，生成银微粒子。在进行反应时，可以在已预热的反应容器内导入组合物，也可以将组合物导入反应容器后加热。
反应温度只要是进行热分解反应且生成银微粒子的温度即可，例如可举出50～250℃左右。另外，反应时间可按照期望的平均粒径大小或与其相应的组合物的组成适当地选择。作为反应时间，可举出例如1分钟～100小时。
通过热分解反应生成的银微粒子，由于以包含未反应原料的混合物形式获得，所以优选精制银微粒子。作为精制方法，可举出：固液分离方法、利用银微粒子与有机溶剂等未反应原料的比重差的沉淀方法等。作为固液分离方法，可举出：过滤器过滤、离心分离、旋风式或倾析器等方法。为了易于进行精制时的处理，也可以用丙酮、甲醇等低沸点溶剂来稀释含有银微粒子的混合物，调整其粘度。
通过调整银微粒子制备用组合物的组成或反应条件，可以调整获得的银微粒子的平均粒径。
3.调整(置换)保护层中的各胺的比率的方法
下面对“2.金属微粒子A的制造方法”栏中描述的保护层中的各胺的上述比率(C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率)调整成在上述范围外而获得的金属微粒子的该比率调整(置换)成为上述范围内的方法进行叙述。
在保护层中所含的胺中，C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率可通过交付至以下工序而将保护层中的各胺的比率调整(置换)成上述范围，使上述范围外的金属微粒子分散于溶剂中，且将C5-7的单烷基胺及烷氧基胺(1)的至少一方以相对于金属微粒子的质量在0.1～5倍量的范围添加，且在室温～80℃下进行1分钟～24小时搅拌的工序。另外，通过在预先将各胺的比率调整成特定比率的溶剂中添加金属微粒子，可以将金属微粒子的保护层中的C5-7的单烷基胺和/或烷氧基胺(1)与和不同于这些胺的胺的比率调整成期望的比率。
使金属微粒子分散的溶剂可以使用可用于金属微粒子合成的溶剂，也可以使用可用于导电性粘接剂的溶剂。将保护层中的各胺的比率调整(置换)成上述范围的金属微粒子可通过“2.金属微粒子A的制造方法”栏中描述的固液分离方法回收。此外，将本保护层中的各胺的比率调整(置换)的方法在平均粒径在上述范围外的金属微粒子中，也可以将保护层中C5-7的单烷基胺和/或烷氧基胺(1)与不同于这些胺的胺的比率调整成期望的比率。
4.导电性粘接剂的烧结体
本发明的导电性粘接剂的烧结体通过将上述“1.导电性粘接剂”中详述的本发明导电性粘接剂烧结而获得。本发明的导电性粘接剂的烧结体中，构成导电性粘接剂的保护层的成分因烧结时的高热而几乎脱离，烧结体实质上由金属构成。
作为烧结温度，没有特别限制，从获得的烧结体发挥高的导电性与高的粘接力，并同时有效地提高机械性强度的观点出发，可举出优选为150℃～200℃的程度，更优选为150℃～185℃的程度。从同样的观点出发，作为烧结时间，可举出优选为0.4小时～2.0小时的程度，更优选为0.5小时～1.2小时的程度。烧结可以在大气、惰性气体(氮气、氩气)等气氛下进行。作为烧结装置，没有特别限制，可举出烘箱、热风式干燥炉、红外线干燥炉、激光照射、闪光灯照射、微波等。
5.电路或装置
本发明的电路或装置分别具备部件间通过本发明烧结体粘接的部分。即，本发明的电路或装置是将上述的“1.导电性粘接剂”中详述的本发明的导电性粘接剂配置于电路或装置的部件间，且使导电性粘接剂烧结来粘接部件之间而成的电路或装置。
如上述，本发明的烧结体因为发挥高的导电性与高的粘接力，同时可有效地提高机械性强度，所以具备其的电路或装置中，部件间的导电性与粘接力也优异，且机械性强度也优异。
实施例
在以下的实施例中，更具体地说明本发明，但本发明不限定于这些实施例。
实施例及比较例中使用的各成分的详情如下。
·草酸银((COOAg)2)以专利文献1(特许第5574761号公报)记载的方法合成。
·油酸(和光纯药工业株式会社制)
·N,N-二甲基-1,3-二氨基丙烷(和光纯药工业株式会社制)
·N,N-二乙基-1,3-二氨基丙烷(和光纯药工业株式会社制)
·正己胺(碳原子数6，和光纯药工业株式会社制)
·正丙胺(碳原子数3，和光纯药工业株式会社制)
·正丁胺(碳原子数4，和光纯药工业株式会社制)
·3-甲氧基丙胺(碳原子数4，和光纯药工业株式会社制)
·2-(2-乙基己氧基)乙醇(和光纯药工业株式会社制)
·丁醇(和光纯药工业株式会社制)
·戊醇(和光纯药工业株式会社制)
在以下实施例及比较例中，合成的银微粒子的保护层中的胺的测定是通过以下方法进行。
(银微粒子的保护层中所含的各胺的比率的测定方法)
相对于银微粒子1g，添加甲醇4g，搅拌1分钟。之后，边搅拌边添加浓盐酸100mg，进一步持续搅拌10分钟，使保护层游离。进而一边继续搅拌一边添加48％氢氧化钠水溶液150mg，使pH＞7。通过将该固液混合物过滤，由此获得提取了保护层中所含的胺的甲醇溶液，作为气相色谱用的样品。将该样品用气相色谱仪(岛津制作所制，GC-2010，管柱：RESTEK制，Rtx-5Amine)进行分析，根据得到的峰面积比进行保护层中所含的胺的比率(GC％)的定量。将结果示于表1～3。
此外，表1～3中，HA是正己胺，MP是甲氧基丙胺，DA是N,N-二乙基-1,3-二氨基丙烷或N,N-二甲基-1,3-二氨基丙烷，BuNH2是正丁胺，PrNH2是正丙胺。
在以下的实施例及比较例中，机械性强度及涂膜的破裂或缺陷分别如下进行评价，其结果示于表1～3。
(机械性强度的评价)
各实施例及比较例中获得的各涂膜的抗剪强度用粘合强度试验机(西进商事制SS30-WD)实施芯片剪切试验而测定。
(涂膜的破裂或缺陷的评价)
目视观察各实施例及比较例中获得的各涂膜的表面，评价有无涂膜的破裂或缺陷。
＜合成例1＞平均粒径200nm的金属微粒子的合成例
在放入了磁力搅拌子的50mL玻璃制离心管中加入油酸(0.1g)、N,N-二乙基-1,3-二氨基丙烷(3.25g)及戊醇(4.0g)，搅拌约1分钟后，加入草酸银(4.0g)，搅拌约10分钟，由此获得银微粒子制备用组合物。之后，在具备铝块的热搅拌器(小池精密机器制作所制HHE-19G-U)上将这些的玻璃制离心管直立设置，在40℃下搅拌30分钟后，进一步在90℃下搅拌30分钟。放置冷却后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟的离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收制造的银微粒子1。将合成例1中获得的银微粒子1用扫描型电子显微镜(日立ハイテク制S-4500)观察，测定图像中所含的任意30个粒子的长边的长度，求得平均值。平均粒径为200nm。
调整(置换)银微粒子1的保护层中所含的胺的比率的方法
使用合成例1中获得的银微粒子1的分散液(甲醇溶液)，添加银微粒子1的质量3倍量的正己胺(使用于银微粒子1A的制备)、甲氧基丙胺(使用于银微粒子1B的制备)的各胺，在室温下搅拌4小时。搅拌后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟的离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收调整(置换)了保护层中胺的比率的银微粒子1A、1B。另外，平均粒径没有变化。
(实施例1、2)
实施例1中使用银微粒子1A、实施例2使用银微粒子1B，分别添加相当于总质量10％的萜品醇获得各分散液。将该液体用クラボウ社制的行星式搅拌脱泡机(マゼルスター)，以2次搅拌优先模式混合，制备各导电性粘接剂。
接着，准备在铜板上施加了0.5μm化学镀银的基材，在其上将各导电性粘接剂均匀地进行涂膜成厚度成为50μm的涂膜，且将背面(与导电性粘接剂接触的面)施加了镀金或溅射金处理的硅晶片(尺寸2mm×2mm)置于其上。将其通过干燥器(循环式)在规定温度(150℃)下加热60分钟，获得各导电性粘接剂已烧结的涂膜。
＜合成例2＞平均粒径75nm的金属微粒子的合成例
在放入了磁力搅拌子的50mL玻璃制离心管中加入油酸(0.1g)、N,N-二乙基-1,3-二氨基丙烷(3.25g)及丁醇(6.0g)，搅拌约1分钟后，加入草酸银(4.0g)，搅拌约10分钟，获得银微粒子制备用组合物。之后，在具备铝块的热搅拌器(小池精密机器制作所制HHE-19G-U)上将这些的玻璃制离心管直立设置，在40℃下搅拌30分钟后，进而在90℃下搅拌30分钟。放置冷却后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟的离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收制造的银微粒子2。将合成例2中获得的银微粒子2用扫描型电子显微镜(日立ハイテク制S-4500)观察，测定图像中所含任意30个粒子的长边的长度，求得平均值。平均粒径为75nm。另外，合成例2中获得的银微粒子2作为银微粒子2C用于实施例。
调整(置换)银微粒子2的保护层中所含的胺的比率的方法
使用合成例2中获得的银微粒子2的分散液(甲醇溶液)，添加银微粒子2的质量3倍量的正己胺(使用于银微粒子2A的制备)、甲氧基丙胺(使用于银微粒子2B的制备)、正丁胺(使用于银微粒子2D的制备)、正丙胺(使用于银微粒子2E的制备)，在室温下搅拌4小时。搅拌后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌之后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收调整(置换)了保护层中各胺的比率的银微粒子2A～2E。另外，平均粒径没有变化。
(实施例3、4及比较例1～3)
使用上述获得的各银微粒子2A～2E，分别添加相当于总质量10％的萜品醇，获得各分散液。在实施例3中使用银微粒子2A、实施例4中使用银微粒子2B、比较例1中使用银微粒子2C、比较例2中使用银微粒子2D、比较例3中使用银微粒子2E。将这些的液体分别用クラボウ社制的行星式搅拌脱泡机(マゼルスター)，以2次搅拌优先模式混合，制备各导电性粘接剂。
接着，准备在铜板上施加了0.5μm化学镀银的基材，在其上将各导电性粘接剂均匀地进行涂膜成厚度成为50μm的涂膜，且将背面(与导电性粘接剂接触的面)施加了镀金或溅射金处理的硅晶片(尺寸2mm×2mm)置于其上。将其通过干燥器(循环式)在规定温度(150℃)下加热60分钟，获得各导电性粘接剂已烧结的涂膜。
＜合成例3＞平均粒径20nm的金属微粒子的合成例
在放入了磁力搅拌器的50mL玻璃制离心管中加入油酸(0.06g)、己胺(1.4g)、N,N-二甲基-1,3-二氨基丙烷(0.3g)、丁胺(0.6g)及2-(2-乙基己氧基)乙醇(4.0g)，搅拌约1分钟后，加入草酸银(4.0g)，搅拌约10分钟，获得银微粒子制备用组合物。之后，在具备铝块的热搅拌器(小池精密机器制作所制HHE-19G-U)上将这些的玻璃制离心管直立设置，在40℃下搅拌30分钟，进而在90℃下搅拌30分钟。放置冷却后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟的离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收制造的银微粒子6。将合成例3中获得的银微粒子3用扫描型电子显微镜(日立ハイテク制S-4500)观察，测定图像中所含任意30个粒子的长边的长度，求得平均值。平均粒径为20nm。
调整(置换)银微粒子3的保护层中所含的胺的比率的方法
使用合成例3中获得的银微粒子3的分散液(甲醇溶液)，添加银微粒子的质量3倍量的正己胺，在室温下搅拌4小时。搅拌后，取出磁力搅拌子，对各组合物添加甲醇15g用涡旋混合器搅拌之后，用离心分离机(日立工机制CF7D2)以3000rpm(约1600×G)实施1分钟的离心沉积操作，通过倾斜离心管除去上清液。添加甲醇15g、搅拌、离心分离及除去上清液的工序重复2次，回收调整(置换)了保护层中所含的胺的比率的银微粒子3A。另外，平均粒径没有变化。
(比较例4)
使用上述获得的银微粒子3A，添加相当于总质量10％的萜品醇，获得各分散液。将该液体使用クラボウ社制的行星式搅拌脱泡机(マゼルスター)，以2次搅拌优先模式混合，制备导电性粘接剂。
接着，准备在铜板上施加了0.5μm化学镀银的基材，在其上将各导电性粘接剂均匀地进行涂膜成厚度成为50μm的涂膜，且将背面(与导电性粘接剂接触的面)施加了镀金或溅射金处理的硅晶片(尺寸2mm×2mm)置于其上。将其通过干燥器(循环式)在规定温度(150℃)下加热60分钟，获得各导电性粘接剂已烧结的涂膜。
[表1]
从表1所示的结果明显可知，金属微粒子的平均粒径为30nm～300nm范围内，且保护层中的胺包含碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺，进而，碳原子数5～7的单烷基胺和/或通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内的实施例1～4的导电性粘接剂，涂膜的抗剪强度高，也没有涂膜的破裂或缺陷。另一方面，保护层中所含的胺中，N,N-二乙基-1,3-二氨基丙烷、正丁胺或正丙胺的比率为100％的比较例1～3的导电性粘接剂，涂膜的剪应力低。另外，金属微粒子的平均粒径为20nm的比较例4的导电性粘接剂也是涂膜的剪应力低。
(实施例5～11)
将上述获得的各银微粒子1A、1B、2A、2B、2C以表2所示的比率混合，添加相当于总质量10％的萜品醇，获得各分散液。将该液体用クラボウ社制的行星式搅拌脱泡机(マゼルスター)，以2次搅拌优先模式混合，制备各导电性粘接剂。此外，混合后的平均粒径通过上述方法求得。
接着，准备在铜板上施加了0.5μm化学镀银的基材，在其上将各导电性粘接剂均匀地进行涂膜成厚度成为50μm的涂膜，且将背面(与导电性粘接剂接触的面)施加了镀金或溅射金处理的硅晶片(尺寸2mm×2mm)置于其上。将其通过干燥器(循环式)在规定温度(150℃)下加热60分钟，获得各导电性粘接剂已烧结的涂膜。
[表2]
从表2所示的结果明显可知，实施例5～11的导电性粘接剂为混合平均粒径或保护层中所含的胺是不同的金属微粒子的材料，但因为金属微粒子的平均粒径为30nm～300nm范围内，且保护层中的胺包含碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺，进而碳原子数5～7的单烷基胺和/或通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内，因此，在烧结温度150℃中，涂膜的抗剪强度高，也没有涂膜的破裂或缺陷。
(实施例12、比较例5、6)
将上述获得的各银微粒子1A、1B、2A、2B、2C、3A以表3所示的比率混合，添加相当于总质量10％的萜品醇获得各分散液。将该液体用クラボウ社制的行星式搅拌脱泡机(マゼルスター)，以2次搅拌优先模式混合，制备各导电性粘接剂。此外，混合后的平均粒径是通过上述的方法求得。
接着，准备在铜板上施加了0.5μm化学镀银的基材，在其上将各导电性粘接剂均匀地进行涂膜成厚度成为50μm的涂膜，且将背面(与导电性粘接剂接触的面)施加了镀金或溅射金处理的硅晶片(尺寸2mm×2mm)置于其上。将其通过干燥器(循环式)在规定温度(150℃)下加热60分钟，获得各导电性粘接剂已烧结的涂膜。
[表3]
从表3所示的结果明显可知，实施例12的导电性粘接剂是混合了3种类平均粒径及保护层中所含的胺为不同的金属微粒子的材料，但因为金属微粒子的平均粒径在30nm～300nm范围内，且保护层中的胺包含碳原子数5～7的单烷基胺和/或上述通式(1)所示的烷氧基胺，进而碳原子数5～7单烷基胺和/或通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内，因此，在烧结温度150℃中，涂膜的抗剪强度高，也没有涂膜的破裂或缺陷。另一方面，平均粒径低于30μm的比较例5、6中，涂膜的抗剪强度低。

Claims (8)

1.一种导电性粘接剂，其含有金属微粒子A，所述金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，
所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，
NH2-R2-O-R1…(1)
式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基，
所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。
2.根据权利要求1所述的导电性粘接剂，其中，
所述保护层还含有脂肪酸。
3.根据权利要求1或2所述的导电性粘接剂，其中，
所述导电性粘接剂还含有溶剂。
4.一种烧结体，其为权利要求1～3中任一项所述的导电性粘接剂的烧结体。
5.一种电路或装置，其具备部件间通过权利要求4所述的烧结体粘接的部分。
6.一种导电性粘接剂的制造方法，其中，使用金属微粒子A，所述导电性粘接剂的制造方法具备混合所述金属微粒子A的工序，所述金属微粒子A具备含胺的保护层，且平均粒径为30nm～300nm，其中，
所述胺包含碳原子数5～7的单烷基胺和/或下述通式(1)所示的烷氧基胺，
NH2-R2-O-R1…(1)
式中，R1表示碳原子数1～4的烷基，R2表示碳原子数1～4的亚烷基，
所述保护层中，所述碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率在100:0～10:90的范围内。
7.根据权利要求6所述的导电性粘接剂的制造方法，其还具备：
准备金属微粒子的工序，所述金属微粒子具备含胺的保护层，且平均粒径为30nm～300nm；
制备所述金属微粒子A的工序，将该金属微粒子的保护层中所含的胺与碳原子数5～7的单烷基胺及通式(1)所示的烷氧基胺进行置换，将碳原子数5～7的单烷基胺和/或所述通式(1)所示的烷氧基胺与不同于这些胺的胺的比率调整成为在100:0～10:90的范围内，制备所述金属微粒子A。
8.一种部件的粘接方法，其具备：
将权利要求1～6中任一项所述的导电性粘接剂配置于部件间的工序、
将所述导电性粘接剂加热而烧结的工序。
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