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KR102095823B1 - Conductive particle, conductive material and connecting structure - Google Patents

Conductive particle, conductive material and connecting structure Download PDF

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Publication number
KR102095823B1
KR102095823B1 KR1020147033188A KR20147033188A KR102095823B1 KR 102095823 B1 KR102095823 B1 KR 102095823B1 KR 1020147033188 A KR1020147033188 A KR 1020147033188A KR 20147033188 A KR20147033188 A KR 20147033188A KR 102095823 B1 KR102095823 B1 KR 102095823B1
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KR
South Korea
Prior art keywords
conductive
particles
conductive layer
layer
particle
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KR1020147033188A
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Korean (ko)
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KR20150063962A (en
Inventor
게이조 니시오까
Original Assignee
세키스이가가쿠 고교가부시키가이샤
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Publication of KR20150063962A publication Critical patent/KR20150063962A/en
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Publication of KR102095823B1 publication Critical patent/KR102095823B1/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • 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
    • B22F1/18—Non-metallic particles coated with metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • H—ELECTRICITY
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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Abstract

본 발명은 전극 간을 접속한 경우에, 접속 저항을 낮게 할 수 있는 도전성 입자, 및 상기 도전성 입자를 사용한 도전 재료를 제공한다. 본 발명에 따른 도전성 입자(1)는, 기재 입자(2)와, 기재 입자(2)의 표면 상의 일부의 영역에 배치된 도전재(4)를 구비하고, 도전재(4)의 재질이 니켈보다도 모스 경도가 높은 재질이다.The present invention provides conductive particles capable of lowering the connection resistance when connecting between electrodes, and conductive materials using the conductive particles. The electroconductive particle 1 which concerns on this invention is equipped with the base material particle 2 and the electroconductive material 4 arrange | positioned in a partial area | region on the surface of the base material particle 2, and the material of the electroconductive material 4 is nickel It is a material with a higher Mohs hardness.

Description

도전성 입자, 도전 재료 및 접속 구조체{CONDUCTIVE PARTICLE, CONDUCTIVE MATERIAL AND CONNECTING STRUCTURE}CONDUCTIVE PARTICLE, CONDUCTIVE MATERIAL AND CONNECTING STRUCTURE

본 발명은, 기재 입자의 표면 상에 도전재가 배치되어 있는 도전성 입자에 관한 것이다. 보다 상세하게는, 본 발명은 예를 들어 전극 간의 전기적인 접속에 사용할 수 있는 도전성 입자에 관한 것이다. 또한, 본 발명은, 상기 도전성 입자를 사용한 도전 재료 및 접속 구조체에 관한 것이다.The present invention relates to conductive particles in which a conductive material is disposed on the surface of the substrate particles. More specifically, the present invention relates to conductive particles that can be used, for example, for electrical connection between electrodes. Further, the present invention relates to a conductive material and a connecting structure using the conductive particles.

이방성 도전 페이스트 및 이방성 도전 필름 등의 도전 재료가 널리 알려져 있다. 이 이방성 도전 재료에서는, 결합제 수지 중에 도전성 입자가 분산되어 있다.Conductive materials such as anisotropic conductive pastes and anisotropic conductive films are widely known. In this anisotropic conductive material, conductive particles are dispersed in the binder resin.

상기 이방성 도전 재료는, 각종 접속 구조체를 얻기 위해서, 예를 들어 플렉시블 프린트 기판과 유리 기판과의 접속(FOG(Film on Glass)), 반도체칩과 플렉시블 프린트 기판과의 접속(COF(Chip on Film)), 반도체칩과 유리 기판과의 접속(COG(Chip on Glass)), 및 플렉시블 프린트 기판과 유리 에폭시 기판과의 접속(FOB(Film on Board)) 등에 사용되고 있다.In order to obtain various connection structures, the anisotropic conductive material is, for example, a connection between a flexible printed circuit board and a glass substrate (FOG (Film on Glass)), a connection between a semiconductor chip and a flexible printed circuit board (Chip on Film (COF)) ), Semiconductor chip and glass substrate (COG (Chip on Glass)), and flexible printed substrate and glass epoxy substrate (FOB (Film on Board)).

상기 도전성 입자의 일례로서, 하기의 특허문헌 1에는, 복합 입자와, 해당 복합 입자를 덮는 금속 도금층을 구비하는 도전성 입자가 개시되어 있다. 상기 복합 입자는, 플라스틱 핵체와, 해당 플라스틱 핵체에 화학 결합에 의해 흡착한 비도전성 무기 입자를 갖는다.As an example of the conductive particles, Patent Document 1 below discloses conductive particles comprising composite particles and a metal plating layer covering the composite particles. The composite particle has a plastic nucleus and non-conductive inorganic particles adsorbed on the plastic nucleus by chemical bonding.

하기의 특허문헌 2에는, 플라스틱 핵체와, 해당 플라스틱 핵체를 덮는 고분자 전해질층과, 해당 고분자 전해질층을 통해 상기 플라스틱 핵체에 흡착한 금속 입자와, 해당 금속 입자를 덮도록 상기 플라스틱 핵체의 주위에 형성된 무전해 금속 도금층을 구비하는 도전성 입자가 개시되어 있다. 특허문헌 2에서는, 상기 플라스틱 핵체에 흡착시키는 금속 입자가, 예를 들어 금, 은, 구리, 팔라듐 및 니켈로부터 선택되는 금속의 입자인 것이 기재되어 있다.In Patent Document 2, a plastic nucleus, a polymer electrolyte layer covering the plastic nucleus, metal particles adsorbed on the plastic nucleus through the polymer electrolyte layer, and formed around the plastic nucleus to cover the metal particles Conductive particles having an electroless metal plating layer are disclosed. Patent Document 2 discloses that the metal particles adsorbed on the plastic nucleus are metal particles selected from gold, silver, copper, palladium and nickel, for example.

하기의 특허문헌 3에는, 기재 입자의 표면에, 니켈 및 인을 함유하는 금속 도금 피막층과 금층과의 다층의 도전층이 형성되어 있는 도전성 입자가 개시되어 있다. 상기 도전성 입자에서는, 기재 입자의 표면 상에 코어 물질이 배치되어 있고, 해당 코어 물질은 도전층에 의해 피복되어 있다. 코어 물질에 의해 도전층이 융기되어 있고, 도전층의 표면에 돌기가 형성되어 있다. 특허문헌 3에서는, 상기 코어 물질을 구성하는 도전성 물질이 금속인 경우에, 해당 금속으로서는, 예를 들어 니켈, 구리, 금, 은, 백금, 아연, 철, 납, 주석, 알루미늄, 코발트, 인듐, 크롬, 티타늄, 안티몬, 비스무트, 게르마늄 및 카드뮴 등의 금속, 및 주석-납 합금, 주석-구리 합금, 주석-은 합금 및 주석-납-은 합금 등의 2종류 이상의 금속으로 구성되는 합금 등이 예시되어 있다.In the following patent document 3, the electroconductive particle in which the multilayered conductive layer of the metal plating film layer containing nickel and phosphorus and a gold layer is formed on the surface of a base material particle is disclosed. In the said electroconductive particle, a core material is arrange | positioned on the surface of a base material particle, and this core material is covered with the electroconductive layer. The conductive layer is raised by the core material, and protrusions are formed on the surface of the conductive layer. In Patent Document 3, when the conductive material constituting the core material is a metal, as the metal, for example, nickel, copper, gold, silver, platinum, zinc, iron, lead, tin, aluminum, cobalt, indium, Examples include metals such as chromium, titanium, antimony, bismuth, germanium, and cadmium, and alloys composed of two or more metals such as tin-lead alloy, tin-copper alloy, tin-silver alloy, and tin-lead-silver alloy. It is done.

일본 특허 공개 제2011-29179호 공보Japanese Patent Publication No. 2011-29179 일본 특허 공개 제2011-108446호 공보Japanese Patent Publication No. 2011-108446 일본 특허 공개 제2006-228475호 공보Japanese Patent Publication No. 2006-228475

상술한 특허문헌 1 내지 3에는, 도전층의 외측 표면에 돌기를 갖는 도전성 입자가 개시되어 있다. 도전성 입자에 의해 접속되는 전극, 및 도전성 입자의 도전층 표면에는, 산화 피막이 형성되어 있는 경우가 많다. 상기 도전층의 돌기는, 도전성 입자를 통해 전극 간을 압착할 때에, 전극 및 도전성 입자의 표면 산화 피막을 배제하여, 도전층과 전극을 접촉시키기 위해서 형성되어 있다.In the above-mentioned Patent Documents 1 to 3, conductive particles having projections on the outer surface of the conductive layer are disclosed. In many cases, an oxide film is formed on the surfaces of the electrodes connected by the conductive particles and the conductive layer of the conductive particles. The projections of the conductive layer are formed to exclude the surface oxide film of the electrode and the conductive particles and make the conductive layer and the electrode contact each other when the electrode is pressed through the conductive particles.

그러나, 특허문헌 1 내지 3에 기재와 같은 종래의 도전성 입자를 사용하여 전극 간을 접속한 경우에는, 접속 저항이 높아지는 경우가 있다. 또한, 전극 및 도전성 입자의 표면 산화 피막을 충분히 배제할 수 없고, 접속 저항이 비교적 높아지기 쉽다.However, when connecting between electrodes using the conventional electroconductive particle as described in patent documents 1-3, connection resistance may increase. In addition, the surface oxide film of the electrode and the conductive particles cannot be sufficiently removed, and the connection resistance tends to be relatively high.

또한, 최근 들어, 전극 간의 접속 저항을 보다 한층 낮게 하는 것을 가능하게 하는 도전성 입자가 요망되고 있다.Moreover, in recent years, the electroconductive particle which makes it possible to further lower the connection resistance between electrodes is calculated | required.

본 발명의 목적은, 전극 간을 접속한 경우에, 전극 간의 접속 저항을 낮게 할 수 있는 도전성 입자, 및 상기 도전성 입자를 사용한 도전 재료 및 접속 구조체를 제공하는 것이다.An object of the present invention is to provide conductive particles capable of reducing the connection resistance between electrodes when connecting between electrodes, and conductive materials and connection structures using the conductive particles.

본 발명의 넓은 국면에 의하면, 기재 입자와, 상기 기재 입자의 표면 상의 일부 영역에 배치된 도전재를 구비하고, 상기 도전재의 재질이 니켈보다도 모스 경도가 높은 재질인 도전성 입자가 제공된다.According to the broad aspect of the present invention, there is provided a conductive particle comprising a substrate particle and a conductive material disposed in a partial region on the surface of the substrate particle, the material of the conductive material having a higher Mohs hardness than nickel.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전성 입자는 상기 기재 입자와, 상기 기재 입자의 표면 상의 일부의 영역에 배치된 상기 도전재를 구비하고, 상기 도전재의 재질이 몰리브덴, 탄화텅스텐, 텅스텐, 탄화티타늄 또는 탄화탄탈이다.In a specific aspect of the conductive particle according to the present invention, the conductive particle includes the substrate particle and the conductive material disposed in a partial region on the surface of the substrate particle, and the material of the conductive material is molybdenum, tungsten carbide, Tungsten, titanium carbide or tantalum carbide.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전성 입자는 복수의 상기 도전재를 구비한다.In a specific aspect of the conductive particles according to the present invention, the conductive particles include a plurality of the conductive materials.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전성 입자는 상기 기재 입자와, 상기 기재 입자의 표면 상에 배치되어 있는 도전층과, 상기 기재 입자의 표면 상의 일부의 영역에 배치되어 있는 상기 도전재를 구비하고, 상기 도전재가 상기 도전층 내에 매입(

Figure 112014114395923-pct00001
)되어 있다.In a specific aspect of the conductive particles according to the present invention, the conductive particles are the substrate particles, the conductive layer disposed on the surface of the substrate particles, and the conductive layer disposed in a partial region on the surface of the substrate particles Provided with the ash, and the conductive material is embedded in the conductive layer (
Figure 112014114395923-pct00001
).

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전층이 외측의 표면에 돌기를 갖고, 상기 도전층의 상기 돌기의 내측에 상기 도전재가 배치되어 있다.In a specific aspect of the conductive particles according to the present invention, the conductive layer has a projection on the outer surface, and the conductive material is disposed inside the projection of the conductive layer.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전층이 니켈층을 갖는다.In a specific aspect of the conductive particles according to the present invention, the conductive layer has a nickel layer.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전층이 상기 기재 입자측에 니켈층과, 상기 기재 입자측과는 반대측에 팔라듐층을 갖는다.In a specific aspect of the conductive particles according to the present invention, the conductive layer has a nickel layer on the substrate particle side and a palladium layer on the opposite side to the substrate particle side.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전성 입자는 상기 도전층의 표면에 부착되어 있는 절연성 물질을 더 구비한다.In a specific aspect of the conductive particles according to the present invention, the conductive particles further include an insulating material attached to the surface of the conductive layer.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전재가 입자이다.In a specific aspect of the conductive particles according to the present invention, the conductive material is particles.

본 발명에 따른 도전성 입자의 어느 특정한 국면에서는, 상기 도전성 입자는 상기 기재 입자와, 상기 기재 입자의 표면 상의 일부의 영역에 배치된 상기 도전재를 구비하고, 상기 도전재의 재질이 몰리브덴, 탄화텅스텐, 텅스텐 또는 탄화탄탈이다.In a specific aspect of the conductive particle according to the present invention, the conductive particle includes the substrate particle and the conductive material disposed in a partial region on the surface of the substrate particle, and the material of the conductive material is molybdenum, tungsten carbide, Tungsten or tantalum carbide.

본 발명의 넓은 국면에 의하면, 상술한 도전성 입자와, 결합제 수지를 포함하는 도전 재료가 제공된다.According to the wide aspect of this invention, the conductive material containing the above-mentioned electroconductive particle and binder resin is provided.

본 발명의 넓은 국면에 의하면, 제1 전극을 표면에 갖는 제1 접속 대상 부재와, 제2 전극을 표면에 갖는 제2 접속 대상 부재와, 상기 제1 접속 대상 부재와 상기 제2 접속 대상 부재를 접속하고 있는 접속부를 구비하고, 상기 접속부가 상술한 도전성 입자에 의해 형성되어 있거나, 또는 상기 도전성 입자와 결합제 수지를 포함하는 도전 재료에 의해 형성되어 있고, 상기 제1 전극과 상기 제2 전극이 상기 도전성 입자에 의해 전기적으로 접속되어 있는, 접속 구조체가 제공된다.According to the broad aspect of the present invention, the first connection target member having the first electrode on the surface, the second connection target member having the second electrode on the surface, the first connection target member and the second connection target member It is provided with the connecting part which is connected, the said connecting part is formed of the above-mentioned electroconductive particle, or is formed of the electroconductive material containing the said electroconductive particle and binder resin, and the said 1st electrode and said 2nd electrode are said. A connection structure is provided, which is electrically connected by conductive particles.

본 발명에 따른 도전성 입자는, 기재 입자의 표면 상의 일부의 영역에 도전 재가 배치되어 있고, 상기 도전재의 재질이 니켈보다도 모스 경도가 높은 재질이므로, 본 발명에 따른 도전성 입자를 사용하여 전극 간을 접속한 경우에 접속 저항을 낮게 할 수 있다.In the conductive particles according to the present invention, since a conductive material is disposed in a part of the surface of the substrate particle, and the material of the conductive material has a higher Mohs hardness than nickel, the conductive particles according to the present invention are used to connect between electrodes. In one case, the connection resistance can be made low.

도 1은, 본 발명의 제1 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.
도 2는, 본 발명의 제2 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.
도 3은, 본 발명의 제3 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.
도 4는, 본 발명의 제1 실시 형태에 따른 도전성 입자를 사용한 접속 구조체를 모식적으로 나타내는 정면 단면도이다.1 is a cross-sectional view showing conductive particles according to a first embodiment of the present invention.
2 is a cross-sectional view showing conductive particles according to a second embodiment of the present invention.
3 is a cross-sectional view showing conductive particles according to a third embodiment of the present invention.
4 is a front sectional view schematically showing a connection structure using conductive particles according to a first embodiment of the present invention.

이하, 본 발명의 상세를 설명한다.Hereinafter, the details of the present invention will be described.

(도전성 입자)(Conductive particles)

본 발명에 따른 도전성 입자는, 기재 입자와, 해당 기재 입자의 표면 상의 일부의 영역에 배치된 도전재를 구비한다. 상기 도전재의 재질이 니켈보다도 모스 경도가 높은 재질이다.The electroconductive particle which concerns on this invention is equipped with a base material particle and the electrically conductive material arrange | positioned in a partial area | region on the surface of this base material particle. The material of the conductive material is a material having a higher Mohs hardness than nickel.

본 발명에 따른 도전성 입자에 있어서의 상술한 구성의 채용에 의해, 본 발명에 따른 도전성 입자를 사용하여 전극 간을 접속한 경우에, 전극 간의 접속 불량이 발생하기 어려워지고, 또한 전극 간의 접속 저항을 효과적으로 낮게 할 수 있다.By adopting the above-described configuration in the conductive particles according to the present invention, when the electrodes are connected using the conductive particles according to the present invention, connection failures between the electrodes are less likely to occur, and connection resistances between the electrodes are also reduced. It can be effectively lowered.

상기 도전재의 재질은 몰리브덴, 텅스텐, 탄화텅스텐, 탄화티타늄 또는 탄화탄탈인 것이 바람직하고, 몰리브덴, 텅스텐, 탄화텅스텐, 또는 탄화탄탈인 것도 바람직하다. 이들 재질의 모스 경도는 높다. 이들 재질의 도전재를 구비하는 도전성 입자를 사용하여 전극 간을 접속한 경우에는, 전극 간의 접속 불량이 발생하기 어려워지고, 또한 전극 간의 접속 저항을 효과적으로 낮게 할 수 있다.The material of the conductive material is preferably molybdenum, tungsten, tungsten carbide, titanium carbide or tantalum carbide, and also preferably molybdenum, tungsten, tungsten carbide, or tantalum carbide. The Mohs hardness of these materials is high. When the electrodes are connected using conductive particles having a conductive material made of these materials, connection failure between the electrodes is less likely to occur, and connection resistance between the electrodes can be effectively lowered.

본 발명에 따른 도전성 입자는, 상기 기재 입자와, 상기 기재 입자의 표면 상에 배치되어 있는 도전층과, 상기 기재 입자의 표면 상의 일부의 영역에 배치되어 있는 상기 도전재를 구비하는 것이 바람직하다. 이 경우에, 상기 도전재는 상기 도전층 내에 매입되어 있는 것이 바람직하다. 상기 도전층의 일부 영역이 상기 기재 입자와 접하고 있는 것이 바람직하다.It is preferable that the electroconductive particle which concerns on this invention is equipped with the said substrate particle, the conductive layer arrange | positioned on the surface of the said substrate particle, and the said electrically conductive material arrange | positioned in a partial area | region on the surface of the said substrate particle. In this case, it is preferable that the conductive material is embedded in the conductive layer. It is preferable that some regions of the conductive layer are in contact with the substrate particles.

상기 도전층 내에 상기 도전재가 매입되어 있는 도전성 입자를 사용함으로써, 도전성 입자를 사용하여 전극 간을 접속한 경우에, 전극 간의 접속 불량이 보다 한층 발생하기 어려워지고, 또한 전극 간의 접속 저항을 보다 한층 낮게 할 수 있다.By using the conductive particles in which the conductive material is embedded in the conductive layer, when the electrodes are connected using the conductive particles, connection defects between the electrodes are less likely to occur, and the connection resistance between the electrodes is further lowered. can do.

본 발명에 따른 도전성 입자에서는, 상기 도전층이 외측의 표면에 돌기를 갖고, 상기 도전층의 상기 돌기의 내측에 상기 도전재가 배치되어 있는 것이 바람직하다. 상기 도전재에 의해 상기 돌기가 형성되어 있는 것이 바람직하다.In the conductive particles according to the present invention, it is preferable that the conductive layer has a projection on the outer surface, and the conductive material is disposed inside the projection of the conductive layer. It is preferable that the protrusion is formed of the conductive material.

도전성 입자에 의해 접속되는 전극의 표면에는 산화 피막이 형성되어 있는 경우가 많다. 또한, 상기 도전층의 외측 표면에는 산화 피막이 형성되어 있는 경우가 많다. 상기 도전층이 외측의 표면에 복수의 돌기를 가짐으로써, 전극 간에 도전성 입자를 배치한 후, 압착시킴으로써, 돌기에 의해 산화 피막이 배제된다. 이로 인해, 전극과 도전성 입자를 보다 한층 확실하게 접촉시킬 수 있고, 전극 간의 접속 저항을 더욱 한층 낮게 할 수 있다.In many cases, an oxide film is formed on the surface of the electrode connected by the conductive particles. In addition, an oxide film is often formed on the outer surface of the conductive layer. The conductive layer has a plurality of protrusions on the outer surface, whereby the conductive particles are disposed between the electrodes, and then compressed, whereby the oxide film is excluded by the protrusions. For this reason, the electrode and the conductive particles can be more reliably brought into contact, and the connection resistance between the electrodes can be further lowered.

이하, 도면을 참조하면서 본 발명의 구체적인 실시 형태 및 실시예를 설명함으로써, 본 발명을 분명하게 한다.Hereinafter, the present invention will be clarified by explaining specific embodiments and examples of the present invention with reference to the drawings.

도 1은, 본 발명의 제1 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.1 is a cross-sectional view showing conductive particles according to a first embodiment of the present invention.

도 1에 나타내는 도전성 입자(1)는, 기재 입자(2)와, 도전층(3)과, 복수의 도전재(4)와, 복수의 절연성 물질(5)을 구비한다. 도전층(3)은 기재 입자(2)의 표면 상에 배치되어 있다. 도전성 입자(1)에서는 단층의 도전층(3)이 형성되어 있다. 도전층(3)은 기재 입자(2)를 피복하고 있다. 도전층(3)은 도전재(4)도 피복하고 있다. 도전층(3)은 외측의 표면에 복수의 돌기(3a)를 갖는다.The electroconductive particle 1 shown in FIG. 1 is provided with the base material particle 2, the conductive layer 3, the some conductive material 4, and the some insulating material 5. The conductive layer 3 is disposed on the surface of the substrate particles 2. In the conductive particles 1, a single-layer conductive layer 3 is formed. The conductive layer 3 covers the substrate particles 2. The conductive layer 3 also covers the conductive material 4. The conductive layer 3 has a plurality of protrusions 3a on its outer surface.

도전성 입자(1)는 복수의 도전재(4)를 구비한다. 복수의 도전재(4)가 기재 입자(2)의 표면 상의 일부의 영역에 배치되어 있고, 도전층(3) 내에 매입되어 있다. 도전재(4)는 기재 입자(2)의 표면 상의 모든 영역에 배치되어 있지 않다. 도전재(4)는 기재 입자(2)의 표면 전체를 피복하고 있지 않다. 도전재(4)가 기재 입자(2)의 표면 상의 일부의 영역에 배치되어 있으므로, 기재 입자(2)는 도전재(4)에 접하고 있지 않은 표면의 영역을 갖는다. 도전재(4)는 돌기(3a)의 내측에 배치되어 있다. 1개의 돌기(3a)의 내측에 1개의 도전재(4)가 배치되어 있다. 복수의 도전재(4)에 의해 도전층(3)의 외측 표면이 융기되어 있고, 복수의 돌기(3a)가 형성되어 있다. 도전성 입자가 복수의 도전재를 구비함으로써, 도전성 입자의 외측 표면에 복수의 돌기를 형성하는 것이 용이하다.The conductive particles 1 include a plurality of conductive materials 4. A plurality of conductive materials 4 are arranged in a part of the region on the surface of the substrate particles 2 and embedded in the conductive layer 3. The conductive material 4 is not disposed in any area on the surface of the substrate particles 2. The conductive material 4 does not cover the entire surface of the substrate particles 2. Since the conductive material 4 is disposed in a part of the area on the surface of the substrate particle 2, the substrate particle 2 has an area of the surface that is not in contact with the conductive material 4. The conductive material 4 is disposed inside the projection 3a. One conductive material 4 is disposed inside one projection 3a. The outer surface of the conductive layer 3 is raised by the plurality of conductive materials 4, and a plurality of protrusions 3a are formed. When the conductive particles are provided with a plurality of conductive materials, it is easy to form a plurality of protrusions on the outer surface of the conductive particles.

도전재(4)는 입자이다. 도전재(4)가 입자이기 때문에, 기재 입자(2)의 표면 상의 일부의 영역에 도전재(4)가 배치되어 있다.The conductive material 4 is a particle. Since the conductive material 4 is a particle, the conductive material 4 is disposed in a partial region on the surface of the substrate particle 2.

도전재(4)는 기재 입자(2)에 접하고 있다. 기재 입자의 표면과 도전재의 표면 사이에, 도전층이 배치되어 있을 수도 있다. 도전재가 기재 입자에 접하고 있지 않고, 기재 입자의 표면과 도전재의 표면이 거리를 이격하고 있을 수도 있다.The conductive material 4 is in contact with the substrate particles 2. A conductive layer may be disposed between the surface of the substrate particle and the surface of the conductive material. The conductive material is not in contact with the substrate particles, and the surface of the substrate particles and the surface of the conductive material may be spaced apart.

절연성 물질(5)은 도전층(3)의 표면 상에 배치되어 있다. 절연성 물질(5)은 절연성 입자이다. 절연성 물질(5)은 절연성을 갖는 재료에 의해 형성되어 있다. 도전성 입자는 절연성 물질을 반드시 구비하고 있지 않아도 된다. 또한, 도전성 입자는 절연성 물질로서, 절연 입자 대신에 도전층의 외측 표면을 피복하고 있는 절연층을 구비하고 있을 수도 있다.The insulating material 5 is disposed on the surface of the conductive layer 3. The insulating material 5 is insulating particles. The insulating material 5 is formed of an insulating material. The conductive particles are not necessarily provided with an insulating material. Further, the conductive particles are insulating materials, and may include an insulating layer covering the outer surface of the conductive layer instead of the insulating particles.

도 2는, 본 발명의 제2 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.2 is a cross-sectional view showing conductive particles according to a second embodiment of the present invention.

도 2에 나타내는 도전성 입자(11)는, 기재 입자(2)와, 제1 도전층(12)과, 제2 도전층(13)과, 복수의 도전재(4)와, 복수의 절연성 물질(5)을 구비한다.The electroconductive particle 11 shown in FIG. 2 includes the substrate particle 2, the first conductive layer 12, the second conductive layer 13, the plurality of conductive materials 4, and the plurality of insulating materials ( 5) is provided.

도전성 입자(1)와 도전성 입자(11)는 도전층만이 상이하다. 즉, 도전성 입자(1)에서는 1층 구조의 도전층이 형성되어 있는 것에 반해, 도전성 입자(11)에서는 2층 구조의 제1 도전층(12) 및 제2 도전층(13)이 형성되어 있다. 도전재(4)는 제1 도전층(11) 및 도전층(13) 내에 매입되어 있다.The conductive particles 1 and the conductive particles 11 differ only in the conductive layer. That is, the conductive particles 1 are formed with a single-layered conductive layer, whereas the conductive particles 11 are formed with a two-layered first conductive layer 12 and a second conductive layer 13. . The conductive material 4 is embedded in the first conductive layer 11 and the conductive layer 13.

제1 도전층(12)은 기재 입자(2)의 표면 상에 배치되어 있다. 기재 입자(2)와 제2 도전층(13) 사이에 제1 도전층(12)이 배치되어 있다. 제1 도전층(12)은 기재 입자(2)측에 위치하고 있고, 기재 입자(2)에 접하는 도전층이다. 제2 도전층(13)은 기재 입자(2)측과는 반대측에 위치하고 있고, 기재 입자(2)에 접하고 있지 않다. 따라서, 기재 입자(2)의 표면 상에 제1 도전층(12)이 배치되어 있고, 제1 도전층(12)의 표면 상에 제2 도전층(13)이 배치되어 있다. 제2 도전층(13)은 외표면에 복수의 돌기(13a)를 갖는다. 도전성 입자(11)는 도전성의 표면에 복수의 돌기(11a)를 갖는다.The first conductive layer 12 is disposed on the surface of the substrate particles 2. The first conductive layer 12 is disposed between the substrate particles 2 and the second conductive layer 13. The first conductive layer 12 is located on the substrate particle 2 side and is a conductive layer in contact with the substrate particle 2. The second conductive layer 13 is located on the opposite side to the substrate particle 2 side, and is not in contact with the substrate particle 2. Therefore, the 1st conductive layer 12 is arrange | positioned on the surface of the base material particle 2, and the 2nd conductive layer 13 is arrange | positioned on the surface of the 1st conductive layer 12. The second conductive layer 13 has a plurality of protrusions 13a on its outer surface. The conductive particles 11 have a plurality of protrusions 11a on the conductive surface.

도 3은, 본 발명의 제3 실시 형태에 따른 도전성 입자를 나타내는 단면도이다.3 is a cross-sectional view showing conductive particles according to a third embodiment of the present invention.

도 3에 나타내는 도전성 입자(21)는, 기재 입자(2)와, 도전층(22)과, 복수의 도전재(4)를 구비한다. 도전층(22)은 기재 입자(2)의 표면 상에 배치되어 있다. 도전재(4)는 도전층(22) 내에 매입되어 있다.The electroconductive particle 21 shown in FIG. 3 is provided with the base material particle 2, the electroconductive layer 22, and the some electrically conductive material 4. The conductive layer 22 is disposed on the surface of the substrate particles 2. The conductive material 4 is embedded in the conductive layer 22.

도전성 입자(21)는 표면에 돌기를 갖지 않는다. 도전성 입자(21)는 구상이다. 도전층(22)은 외측의 표면에 돌기를 갖지 않는다. 이와 같이, 본 발명에 따른 도전성 입자는 돌기를 갖고 있지 않을 수도 있고, 구상일 수도 있다. 또한, 도전성 입자(21)는 절연성 물질을 갖지 않는다. 단, 도전성 입자(21)는 도전층(22)의 표면 상에 배치된 절연성 물질을 구비하고 있을 수도 있다.The conductive particles 21 do not have protrusions on the surface. The conductive particles 21 are spherical. The conductive layer 22 does not have protrusions on the outer surface. As described above, the conductive particles according to the present invention may not have projections or may be spherical. Further, the conductive particles 21 do not have an insulating material. However, the conductive particles 21 may be provided with an insulating material disposed on the surface of the conductive layer 22.

이하, 도전성 입자를 보다 상세하게 설명한다.Hereinafter, the conductive particles will be described in more detail.

[기재 입자][Substrate particles]

상기 기재 입자로서는, 수지 입자, 금속 입자를 제외한 무기 입자, 유기 무기 하이브리드 입자 및 금속 입자 등을 들 수 있다. 그 중에서도, 금속 입자를 제외한 기재 입자가 바람직하고, 수지 입자, 금속 입자를 제외한 무기 입자 또는 유기 무기 하이브리드 입자가 보다 바람직하다.Examples of the substrate particles include resin particles, inorganic particles other than metal particles, organic-inorganic hybrid particles, and metal particles. Among them, base particles excluding metal particles are preferred, and inorganic particles excluding resin particles and metal particles or organic-inorganic hybrid particles are more preferable.

상기 수지 입자를 형성하기 위한 수지로서 다양한 유기물이 적절하게 사용된다. 상기 수지 입자를 형성하기 위한 수지로서는, 예를 들어 폴리에틸렌, 폴리프로필렌, 폴리스티렌, 폴리염화비닐, 폴리염화비닐리덴, 폴리이소부틸렌, 폴리부타디엔 등의 폴리올레핀 수지; 폴리메틸메타크릴레이트 및 폴리메틸아크릴레이트 등의 아크릴 수지; 폴리알킬렌테레프탈레이트, 폴리카르보네이트, 폴리아미드, 페놀 포름알데히드 수지, 멜라민 포름알데히드 수지, 벤조구아나민 포름알데히드 수지, 요소 포름알데히드 수지, 페놀 수지, 멜라민 수지, 벤조구아나민 수지, 요소 수지, 에폭시 수지, 불포화 폴리에스테르 수지, 포화 폴리에스테르 수지, 폴리에틸렌테레프탈레이트, 폴리술폰, 폴리페닐렌옥시드, 폴리아세탈, 폴리이미드, 폴리아미드이미드, 폴리에테르에테르케톤, 폴리에테르술폰, 디비닐벤젠 중합체, 및 디비닐벤젠계 공중합체 등을 들 수 있다. 상기 디비닐벤젠계 공중합체 등으로서는, 디비닐벤젠-스티렌 공중합체 및 디비닐벤젠-(메트)아크릴산 에스테르 공중합체 등을 들 수 있다. 상기 수지 입자의 경도를 적합한 범위로 용이하게 제어할 수 있으므로, 상기 수지 입자를 형성하기 위한 수지는 에틸렌성 불포화기를 갖는 중합성 단량체를 1종 또는 2종 이상 중합시킨 중합체인 것이 바람직하다.Various organic materials are suitably used as a resin for forming the resin particles. Examples of the resin for forming the resin particles include polyolefin resins such as polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyvinylidene chloride, polyisobutylene, and polybutadiene; Acrylic resins such as polymethyl methacrylate and polymethyl acrylate; Polyalkylene terephthalate, polycarbonate, polyamide, phenol formaldehyde resin, melamine formaldehyde resin, benzoguanamine formaldehyde resin, urea formaldehyde resin, phenol resin, melamine resin, benzoguanamine resin, urea resin, Epoxy resin, unsaturated polyester resin, saturated polyester resin, polyethylene terephthalate, polysulfone, polyphenylene oxide, polyacetal, polyimide, polyamideimide, polyether ether ketone, polyether sulfone, divinylbenzene polymer, and And divinylbenzene-based copolymers. Examples of the divinylbenzene-based copolymers include divinylbenzene-styrene copolymers and divinylbenzene- (meth) acrylic acid ester copolymers. Since the hardness of the resin particles can be easily controlled within a suitable range, the resin for forming the resin particles is preferably a polymer obtained by polymerizing one or two or more polymerizable monomers having an ethylenically unsaturated group.

상기 수지 입자를 에틸렌성 불포화기를 갖는 단량체를 중합시켜 얻는 경우에는, 해당 에틸렌성 불포화기를 갖는 단량체로서는, 비가교성의 단량체와 가교성의 단량체를 들 수 있다.When the resin particles are obtained by polymerizing a monomer having an ethylenically unsaturated group, examples of the monomer having the ethylenically unsaturated group include a non-crosslinkable monomer and a crosslinkable monomer.

상기 비가교성의 단량체로서는, 예를 들어 스티렌, α-메틸스티렌 등의 스티렌계 단량체; (메트)아크릴산, 말레산, 무수 말레산 등의 카르복실기 함유 단량체; 메틸(메트)아크릴레이트, 에틸(메트)아크릴레이트, 프로필(메트)아크릴레이트, 부틸(메트)아크릴레이트, 2-에틸헥실(메트)아크릴레이트, 라우릴(메트)아크릴레이트, 세틸(메트)아크릴레이트, 스테아릴(메트)아크릴레이트, 시클로헥실(메트)아크릴레이트, 이소보르닐(메트)아크릴레이트 등의 알킬(메트)아크릴레이트류; 2-히드록시에틸(메트)아크릴레이트, 글리세롤(메트)아크릴레이트, 폴리옥시에틸렌(메트)아크릴레이트, 글리시딜(메트)아크릴레이트 등의 산소 원자 함유 (메트)아크릴레이트류; (메트)아크릴로니트릴 등의 니트릴 함유 단량체; 메틸비닐에테르, 에틸비닐에테르, 프로필비닐에테르 등의 비닐에테르류; 아세트산 비닐, 부티르산 비닐, 라우르산 비닐, 스테아르산 비닐 등의 산 비닐에스테르류; 에틸렌, 프로필렌, 이소프렌, 부타디엔 등의 불포화 탄화수소; 트리플루오로메틸 (메트)아크릴레이트, 펜타플루오로에틸(메트)아크릴레이트, 염화비닐, 불화비닐, 클로로스티렌 등의 할로겐 함유 단량체 등을 들 수 있다.Examples of the non-crosslinkable monomers include styrene-based monomers such as styrene and α-methylstyrene; Carboxyl group-containing monomers such as (meth) acrylic acid, maleic acid, and maleic anhydride; Methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, lauryl (meth) acrylate, cetyl (meth) Alkyl (meth) acrylates such as acrylate, stearyl (meth) acrylate, cyclohexyl (meth) acrylate, and isobornyl (meth) acrylate; Oxygen atom-containing (meth) acrylates such as 2-hydroxyethyl (meth) acrylate, glycerol (meth) acrylate, polyoxyethylene (meth) acrylate, and glycidyl (meth) acrylate; Nitrile-containing monomers such as (meth) acrylonitrile; Vinyl ethers such as methyl vinyl ether, ethyl vinyl ether, and propyl vinyl ether; Acid vinyl esters such as vinyl acetate, vinyl butyrate, vinyl laurate, and vinyl stearate; Unsaturated hydrocarbons such as ethylene, propylene, isoprene, and butadiene; And halogen-containing monomers such as trifluoromethyl (meth) acrylate, pentafluoroethyl (meth) acrylate, vinyl chloride, vinyl fluoride, and chlorostyrene.

상기 가교성의 단량체로서는, 예를 들어 테트라메틸올메탄테트라(메트)아크릴레이트, 테트라메틸올메탄트리(메트)아크릴레이트, 테트라메틸올메탄디(메트)아크릴레이트, 트리메틸올프로판트리(메트)아크릴레이트, 디펜타에리트리톨헥사(메트)아크릴레이트, 디펜타에리트리톨펜타(메트)아크릴레이트, 글리세롤트리(메트)아크릴레이트, 글리세롤디(메트)아크릴레이트, (폴리)에틸렌글리콜디(메트)아크릴레이트, (폴리)프로필렌글리콜디(메트)아크릴레이트, (폴리)테트라메틸렌글리콜디(메트)아크릴레이트, 1,4-부탄디올디(메트)아크릴레이트 등의 다관능 (메트)아크릴레이트류; 트리알릴(이소)시아누레이트, 트리알릴트리멜리테이트, 디비닐벤젠, 디알릴프탈레이트, 디알릴아크릴아미드, 디알릴에테르, γ-(메트)아크릴옥시프로필트리메톡시실란, 트리메톡시실릴스티렌, 비닐트리메톡시실란 등의 실란 함유 단량체 등을 들 수 있다.Examples of the crosslinkable monomer include tetramethylolmethanetetra (meth) acrylate, tetramethylolmethanetri (meth) acrylate, tetramethylolmethanedi (meth) acrylate, and trimethylolpropanetri (meth) acrylic. Rate, dipentaerythritol hexa (meth) acrylate, dipentaerythritol penta (meth) acrylate, glycerol tri (meth) acrylate, glycerol di (meth) acrylate, (poly) ethylene glycol di (meth) acrylic Polyfunctional (meth) acrylates such as acrylate, (poly) propylene glycol di (meth) acrylate, (poly) tetramethylene glycol di (meth) acrylate, and 1,4-butanediol di (meth) acrylate; Triallyl (iso) cyanurate, triallyl trimellitate, divinylbenzene, diallyl phthalate, diallyl acrylamide, diallyl ether, γ- (meth) acryloxypropyl trimethoxysilane, trimethoxysilylstyrene And silane-containing monomers such as vinyl trimethoxysilane.

상기 에틸렌성 불포화기를 갖는 중합성 단량체를 공지된 방법에 의해 중합 시킴으로써, 상기 수지 입자를 얻을 수 있다. 이 방법으로서는, 예를 들어 라디칼 중합 개시제의 존재 하에서 현탁 중합하는 방법, 및 비가교의 종 입자를 사용하여 라디칼 중합 개시제와 함께 단량체를 팽윤시켜 중합하는 방법 등을 들 수 있다.The resin particles can be obtained by polymerizing the polymerizable monomer having the ethylenically unsaturated group by a known method. Examples of the method include suspension polymerization in the presence of a radical polymerization initiator, and polymerization of a monomer by swelling the monomer together with a radical polymerization initiator using non-crosslinked seed particles.

상기 기재 입자가 금속을 제외한 무기 입자 또는 유기 무기 하이브리드 입자인 경우에는, 기재 입자를 형성하기 위한 무기물로서는, 실리카 및 카본 블랙 등을 들 수 있다. 상기 실리카에 의해 형성된 입자로서는 특별히 한정되지 않지만, 예를 들어 가수분해성의 알콕시실릴기를 2개 이상 갖는 규소 화합물을 가수분해하여 가교 중합체 입자를 형성한 후에, 필요에 따라 소성을 행함으로써 얻어지는 입자를 들 수 있다. 상기 유기 무기 하이브리드 입자로서는, 예를 들어 가교한 알콕시실릴 중합체와 아크릴 수지에 의해 형성된 유기 무기 하이브리드 입자 등을 들 수 있다.When the base particles are inorganic particles or organic-inorganic hybrid particles other than metals, silica and carbon black may be mentioned as inorganic substances for forming the base particles. The particles formed by the silica are not particularly limited, but, for example, particles obtained by hydrolysis of a silicon compound having two or more hydrolyzable alkoxysilyl groups to form crosslinked polymer particles, followed by firing as necessary. You can. Examples of the organic-inorganic hybrid particles include organic-inorganic hybrid particles formed of a crosslinked alkoxysilyl polymer and an acrylic resin.

상기 기재 입자가 금속 입자인 경우에, 해당 금속 입자를 형성하기 위한 금속으로서는, 은, 구리, 니켈, 규소, 금 및 티타늄 등을 들 수 있다. 상기 기재 입자가 금속 입자인 경우에, 해당 금속 입자는 구리 입자인 것이 바람직하다. 단, 상기 기재 입자는 금속 입자가 아닌 것이 바람직하다.When the base particle is a metal particle, silver, copper, nickel, silicon, gold, titanium, etc. are mentioned as a metal for forming the metal particle. When the base particle is a metal particle, it is preferable that the metal particle is a copper particle. However, it is preferable that the said substrate particle is not a metal particle.

상기 기재 입자의 입자 직경은, 바람직하게는 0.1㎛ 이상, 보다 바람직하게는 1㎛ 이상, 더욱 바람직하게는 1.5㎛ 이상, 특히 바람직하게는 2㎛ 이상, 바람직하게는 1000㎛ 이하, 보다 바람직하게는 500㎛ 이하, 보다 한층 바람직하게는 300㎛ 이하, 더욱 바람직하게는 50㎛ 이하, 특히 바람직하게는 30㎛ 이하, 가장 바람직하게는 5㎛ 이하이다. 기재 입자의 입자 직경이 상기 하한 이상이면 도전성 입자와 전극과의 접촉 면적이 커지기 때문에, 전극 간의 도통 신뢰성이 보다 한층 높아지고, 도전성 입자를 통해 접속된 전극 간의 접속 저항이 보다 한층 낮아진다. 또한, 기재 입자의 표면에 도전층을 무전해 도금에 의해 형성할 때에 응집하기 어려워지고, 응집한 도전성 입자가 형성되기 어려워진다. 입자 직경이 상기 상한 이하이면, 도전성 입자가 충분히 압축되기 쉽고, 전극 간의 접속 저항이 보다 한층 낮아지고, 또한 전극 간의 간격이 작아진다. 상기 기재 입자의 입자 직경은, 기재 입자가 진구상인 경우에는 직경을 나타내고, 기재 입자가 진구상이 아닌 경우에는 최대 직경을 나타낸다.The particle diameter of the substrate particles is preferably 0.1 µm or more, more preferably 1 µm or more, further preferably 1.5 µm or more, particularly preferably 2 µm or more, preferably 1000 µm or less, more preferably 500 µm or less, more preferably 300 µm or less, still more preferably 50 µm or less, particularly preferably 30 µm or less, and most preferably 5 µm or less. When the particle diameter of the substrate particles is greater than or equal to the above lower limit, the contact area between the conductive particles and the electrode increases, so that the conduction reliability between the electrodes is further increased, and the connection resistance between the electrodes connected through the conductive particles is further lowered. In addition, when the conductive layer is formed on the surface of the substrate particles by electroless plating, it becomes difficult to aggregate, and it is difficult to form aggregated conductive particles. When the particle diameter is equal to or less than the above upper limit, the conductive particles are easily compressed, the connection resistance between the electrodes is further lowered, and the interval between the electrodes is smaller. The particle diameter of the base particles represents the diameter when the base particles are spherical, and represents the maximum diameter when the base particles are not spherical.

상기 기재 입자의 입자 직경은 2㎛ 이상, 5㎛ 이하인 것이 특히 바람직하다. 상기 기재 입자의 입자 직경이 2 내지 5㎛의 범위 내이면, 전극 간의 간격이 작아지며, 도전층의 두께를 두껍게 해도 작은 도전성 입자가 얻어진다. 상기 기재 입자의 입자 직경은 3㎛ 이하인 것도 바람직하다.It is particularly preferable that the particle diameter of the base particles is 2 μm or more and 5 μm or less. When the particle diameter of the substrate particles is in the range of 2 to 5 µm, the distance between the electrodes becomes small, and even when the thickness of the conductive layer is thick, small conductive particles are obtained. It is also preferable that the particle diameter of the substrate particles is 3 μm or less.

[도전층][Challenge layer]

본 발명에 따른 도전성 입자는, 기재 입자의 표면 상에 배치되어 있는 도전층을 갖는다.The electroconductive particle which concerns on this invention has a conductive layer arrange | positioned on the surface of a base material particle.

상기 도전층을 형성하기 위한 금속은 특별히 한정되지 않는다. 해당 금속으로서는, 예를 들어 금, 은, 팔라듐, 구리, 백금, 아연, 철, 주석, 납, 알루미늄, 코발트, 인듐, 니켈, 크롬, 티타늄, 안티몬, 비스무트, 탈륨, 게르마늄, 카드뮴, 규소 및 이들의 합금 등을 들 수 있다. 또한, 상기 금속으로서는, 주석 도프 산화인듐(ITO) 및 땜납 등을 들 수 있다. 그 중에서도, 전극 간의 접속 저항을 보다 한층 낮게 할 수 있으므로, 주석을 포함하는 합금, 니켈, 팔라듐, 구리 또는 금이 바람직하고, 니켈 또는 팔라듐이 바람직하다.The metal for forming the conductive layer is not particularly limited. Examples of the metal include gold, silver, palladium, copper, platinum, zinc, iron, tin, lead, aluminum, cobalt, indium, nickel, chromium, titanium, antimony, bismuth, thallium, germanium, cadmium, silicon and these And alloys thereof. In addition, tin-doped indium oxide (ITO), solder, etc. are mentioned as said metal. Among them, an alloy containing tin, nickel, palladium, copper or gold is preferable, and nickel or palladium is preferable because the connection resistance between the electrodes can be further lowered.

도전성 입자(1, 21)와 같이, 상기 도전층은 1개의 층에 의해 형성되어 있을 수도 있다. 도전성 입자(11)와 같이 도전층은 복수의 층에 의해 형성되어 있을 수도 있다. 즉, 도전층은, 2층 이상의 적층 구조를 가질 수도 있다. 도전층이 복수의 층에 의해 형성되어 있는 경우에는, 최외층(제2 도전층 등)은 금층, 니켈층, 팔라듐층, 구리층 또는 주석과 은을 포함하는 합금층인 것이 바람직하고, 팔라듐층 또는 금층인 것이 보다 바람직하다. 최외층은 팔라듐층인 것이 바람직하고, 금층인 것도 바람직하다. 최외층이 이들의 바람직한 도전층인 경우에는, 전극 간의 접속 저항이 보다 한층 낮아진다. 또한, 최외층이 금층인 경우에는, 내부식성이 보다 한층 높아진다. 니켈층은 니켈을 50중량％ 이상 포함한다. 팔라듐층 또는 금층은 팔라듐 또는 금을 50중량％ 이상 포함한다.Like the conductive particles 1 and 21, the conductive layer may be formed of one layer. Like the conductive particles 11, the conductive layer may be formed of a plurality of layers. That is, the conductive layer may have a laminated structure of two or more layers. When the conductive layer is formed of a plurality of layers, the outermost layer (such as the second conductive layer) is preferably a gold layer, a nickel layer, a palladium layer, a copper layer, or an alloy layer containing tin and silver, and the palladium layer Or it is more preferable that it is a gold layer. The outermost layer is preferably a palladium layer, and also preferably a gold layer. When the outermost layers are these preferred conductive layers, the connection resistance between the electrodes is further lowered. Moreover, when the outermost layer is a gold layer, corrosion resistance becomes higher. The nickel layer contains 50% by weight or more of nickel. The palladium layer or gold layer contains at least 50% by weight of palladium or gold.

상기 기재 입자에 접하는 도전층이 니켈을 포함하는 것이 바람직하다. 도전성 입자(1, 21)와 같이 상기 도전층이 단층인 경우에, 상기 도전층은 니켈을 포함하는 것이 바람직하다. 도전성 입자(11)와 같이 도전층이 기재 입자측의 제1 도전층과, 기재 입자측과는 반대측인 제2 도전층을 갖는 경우에, 상기 제1 도전층(기재 입자에 접하는 도전층)이 니켈을 포함하는 것이 바람직하다. 상기 도전층 및 상기 제1 도전층은 니켈을 주성분으로서 포함하는 것이 바람직하다. 니켈을 포함하는 도전층의 도전성은 비교적 높다. 따라서, 니켈을 포함하는 도전층을 구비하는 도전성 입자에 의해 전극 간을 접속한 경우에, 전극 간의 접속 저항이 보다 한층 낮아진다.It is preferable that the conductive layer in contact with the substrate particles contains nickel. When the conductive layer is a single layer like the conductive particles 1 and 21, it is preferable that the conductive layer contains nickel. When the conductive layer like the conductive particles 11 has a first conductive layer on the substrate particle side and a second conductive layer opposite to the substrate particle side, the first conductive layer (conductive layer in contact with the substrate particle) is It is preferred to include nickel. It is preferable that the said conductive layer and said 1st conductive layer contain nickel as a main component. The conductivity of the conductive layer containing nickel is relatively high. Therefore, when the electrodes are connected by conductive particles having a conductive layer containing nickel, the connection resistance between the electrodes is further lowered.

상기 기재 입자에 접하는 도전층 100중량％ 중, 니켈의 함유량은 50중량％ 이상인 것이 바람직하다. 상기 도전층이 단층인 경우에, 상기 도전층 100중량％ 중, 니켈의 함유량은 50중량％ 이상인 것이 바람직하다. 상기 도전층이 상기 제1, 제2 도전층을 구비하는 경우에, 상기 제1 도전층 100중량％ 중의 니켈의 함유량은 50중량％ 이상인 것이 바람직하다. 니켈의 함유량이 50중량％ 이상이면 전극 간의 접속 저항이 상당히 낮아진다. 상기 도전층 또는 상기 제1 도전층 100중량％ 중, 니켈의 함유량은 보다 바람직하게는 60중량％ 이상, 더욱 바람직하게는 70중량％ 이상, 특히 바람직하게는 90중량％ 이상이다. 상기 도전층 또는 상기 제1 도전층 100중량％ 중의 니켈의 함유량은 97중량％ 이상일 수도 있고, 97.5중량％ 이상일 수도 있고, 98중량％ 이상일 수도 있다. 상기 도전층 또는 상기 제1 도전층 100중량％ 중의 니켈의 함유량은, 바람직하게는 99.85중량％ 이하, 보다 바람직하게는 99.7중량％ 이하, 더욱 바람직하게는 99.45중량％ 미만이다. 상기 니켈의 함유량이 상기 하한 이상이면 전극 간의 접속 저항이 보다 한층 낮아진다. 또한, 전극이나 도전층의 표면에 있어서의 산화 피막이 적은 경우에는, 상기 니켈의 함유량이 많을수록 전극 간의 접속 저항이 낮아지는 경향이 있다.It is preferable that the content of nickel in 100% by weight of the conductive layer contacting the substrate particles is 50% by weight or more. When the conductive layer is a single layer, the content of nickel in 100% by weight of the conductive layer is preferably 50% by weight or more. When the said conductive layer is provided with said 1st, 2nd conductive layer, it is preferable that content of nickel in 100 weight% of the said 1st conductive layer is 50 weight% or more. When the content of nickel is 50% by weight or more, the connection resistance between the electrodes is considerably lowered. In 100% by weight of the conductive layer or the first conductive layer, the content of nickel is more preferably 60% by weight or more, still more preferably 70% by weight or more, particularly preferably 90% by weight or more. The content of nickel in 100% by weight of the conductive layer or the first conductive layer may be 97% by weight or more, 97.5% by weight or more, or 98% by weight or more. The content of nickel in 100% by weight of the conductive layer or the first conductive layer is preferably 99.85% by weight or less, more preferably 99.7% by weight or less, and even more preferably less than 99.45% by weight. When the content of the nickel is more than the lower limit, the connection resistance between the electrodes is further lowered. Moreover, when there are few oxide films on the surface of an electrode or a conductive layer, the connection resistance between electrodes tends to become low, so that the said nickel content is large.

상기 도전층 또는 상기 제1 도전층은 니켈과, 붕소 및 인 중 적어도 1종을 포함하는 것이 바람직하다. 상기 도전층 또는 상기 제1 도전층에서는, 니켈과 붕소 및 인 중 적어도 1종과는 합금화하고 있을 수도 있다. 또한, 상기 도전층 또는 상기 제1 도전층에서는, 니켈, 붕소 및 인 이외의 성분을 사용할 수도 있다.It is preferable that the conductive layer or the first conductive layer contains at least one of nickel, boron, and phosphorus. The conductive layer or the first conductive layer may be alloyed with at least one of nickel, boron, and phosphorus. Moreover, in the said conductive layer or said 1st conductive layer, components other than nickel, boron, and phosphorus can also be used.

또한, 접속 구조체가 산의 존재 하에 노출되었을 때에, 전극 간의 접속 저항이 상승하는 경우가 있다. 이로 인해, 상기 도전층 또는 상기 제1 도전층은, 기재 입자측에서 니켈층 중의 인의 함유량이 높고, 기재 입자와는 반대측으로 니켈층 중의 인의 함유량이 낮은 쪽이 좋은 경우가 있다.Further, when the connection structure is exposed in the presence of an acid, the connection resistance between the electrodes may increase. For this reason, the conductive layer or the first conductive layer may have a higher phosphorus content in the nickel layer on the substrate particle side and a lower phosphorus content in the nickel layer on the opposite side to the substrate particle.

상기 도전층 또는 상기 제1 도전층 100중량％ 중의 붕소와 인과의 합계의 함유량은, 바람직하게는 0.01중량％ 이상, 보다 바람직하게는 0.05중량％ 이상, 더욱 바람직하게는 0.1중량％ 이상, 바람직하게는 5중량％ 이하, 보다 바람직하게는 4중량％ 이하, 더욱 바람직하게는 3중량％ 이하, 특히 바람직하게는 2.5중량％ 이하, 가장 바람직하게는 2중량％ 이하이다. 붕소와 인과의 합계의 함유량이 상기 하한 이상이면, 상기 도전층 또는 상기 제1 도전층이 보다 한층 단단해지고, 전극 및 도전성 입자의 표면 산화 피막을 보다 한층 효과적으로 제거할 수 있고, 전극 간의 접속 저항을 보다 한층 낮게 할 수 있다. 붕소와 인과의 합계의 함유량이 상기 상한 이하이면, 니켈의 함유량이 상대적으로 많아지므로, 전극 간의 접속 저항이 낮아진다.The total content of boron and phosphorus in 100% by weight of the conductive layer or the first conductive layer is preferably 0.01% by weight or more, more preferably 0.05% by weight or more, still more preferably 0.1% by weight or more, preferably Is 5% by weight or less, more preferably 4% by weight or less, still more preferably 3% by weight or less, particularly preferably 2.5% by weight or less, and most preferably 2% by weight or less. When the total content of boron and phosphorus is greater than or equal to the above lower limit, the conductive layer or the first conductive layer becomes harder, and the surface oxide film of the electrode and the conductive particles can be more effectively removed, and the connection resistance between electrodes is improved. It can be made lower. When the total content of boron and phosphorus is less than or equal to the above upper limit, the content of nickel is relatively high, and the connection resistance between the electrodes is lowered.

상기 도전층 또는 상기 제1 도전층 100중량％ 중의 붕소의 함유량은, 바람직하게는 0.01중량％ 이상, 보다 바람직하게는 0.05중량％ 이상, 더욱 바람직하게는 0.1중량％ 이상, 바람직하게는 5중량％ 이하, 보다 바람직하게는 4중량％ 이하, 더욱 바람직하게는 3중량％ 이하, 특히 바람직하게는 2.5중량％ 이하, 가장 바람직하게는 2중량％ 이하이다. 붕소의 함유량이 상기 하한 이상이면 상기 도전층 또는 상기 제1 도전층이 보다 한층 단단해지고, 전극 및 도전성 입자의 표면 산화 피막을 보다 한층 효과적으로 제거할 수 있고, 전극 간의 접속 저항을 보다 한층 낮게 할 수 있다. 붕소의 함유량이 상기 상한 이하이면, 니켈의 함유량이 상대적으로 많아지므로, 전극 간의 접속 저항이 낮아진다.The content of boron in 100% by weight of the conductive layer or the first conductive layer is preferably 0.01% by weight or more, more preferably 0.05% by weight or more, still more preferably 0.1% by weight or more, preferably 5% by weight Below, it is more preferably 4% by weight or less, still more preferably 3% by weight or less, particularly preferably 2.5% by weight or less, and most preferably 2% by weight or less. When the content of boron is greater than or equal to the above lower limit, the conductive layer or the first conductive layer becomes harder, the surface oxide film of the electrode and the conductive particles can be more effectively removed, and the connection resistance between the electrodes can be further lowered. have. When the content of boron is less than or equal to the above upper limit, the content of nickel is relatively high, so the connection resistance between the electrodes is lowered.

상기 도전층 또는 상기 제1 도전층은, 인을 포함하지 않거나 또는 포함하며, 상기 도전층 또는 상기 제1 도전층 100중량％ 중의 인의 함유량이 10.0중량％ 미만인 것이 바람직하다. 상기 도전층 100중량％ 중의 인의 함유량은, 보다 바람직하게는 0.5중량％ 미만, 더욱 바람직하게는 0.3중량％ 이하, 특히 바람직하게는 0.1중량％ 이하이다. 상기 도전층 또는 상기 제1 도전층은 인을 포함하지 않는 것이 특히 바람직하다.It is preferable that the said conductive layer or said 1st conductive layer does not contain or contains phosphorus, and the content of phosphorus in 100 weight% of said conductive layer or said 1st conductive layer is less than 10.0 weight%. The content of phosphorus in 100% by weight of the conductive layer is more preferably less than 0.5% by weight, still more preferably 0.3% by weight or less, and particularly preferably 0.1% by weight or less. It is particularly preferable that the conductive layer or the first conductive layer does not contain phosphorus.

상기 도전층 또는 상기 제1 도전층에 있어서의 니켈, 붕소 및 인 등의 각 함유량의 측정 방법은, 기지의 다양한 분석법을 사용할 수 있고 특별히 한정되지 않는다. 이 측정 방법으로서, 흡광 분석법 또는 스펙트럼 분석법 등을 들 수 있다. 상기 흡광 분석법에서는, 프레임 흡광 광도계 및 전기 가열로 흡광 광도계 등을 사용할 수 있다. 상기 스펙트럼 분석법으로서는, 플라즈마 발광 분석법 및 플라즈마 이온원 질량 분석법 등을 들 수 있다.As for the measurement method of each content, such as nickel, boron, and phosphorus, in the said conductive layer or said 1st conductive layer, various known analytical methods can be used and are not specifically limited. As this measurement method, an absorbance analysis method or a spectrum analysis method can be mentioned. In the absorbance analysis method, a frame absorbance photometer, an electric heating furnace absorbance photometer, or the like can be used. Examples of the spectrum analysis method include a plasma emission analysis method and a plasma ion source mass spectrometry method.

상기 도전층 또는 상기 제1 도전층에 있어서의 니켈, 붕소 및 인 등의 각 함유량을 측정할 때에는, ICP 발광 분석 장치를 사용하는 것이 바람직하다. ICP 발광 분석 장치의 시판품으로서는, 호리바(HORIBA)사 제조의 ICP 발광 분석 장치 등을 들 수 있다.When measuring respective contents of nickel, boron and phosphorus in the conductive layer or the first conductive layer, it is preferable to use an ICP emission analyzer. As a commercial item of the ICP emission analysis device, an ICP emission analysis device manufactured by Horiba (HORIBA) and the like can be mentioned.

전극 간의 접속 저항을 보다 한층 낮게 하는 관점에서는, 상기 도전층이 상기 기재 입자측에 니켈층과, 상기 기재 입자측과는 반대측에 제2 도전층을 갖는 것이 바람직하다. 이 경우에, 제2 도전층이 팔라듐층 또는 금층인 것이 바람직하고, 팔라듐층인 것이 보다 바람직하고, 금층인 것이 보다 바람직하다.From the viewpoint of further lowering the connection resistance between the electrodes, it is preferable that the conductive layer has a nickel layer on the substrate particle side and a second conductive layer on the opposite side to the substrate particle side. In this case, the second conductive layer is preferably a palladium layer or a gold layer, more preferably a palladium layer, and more preferably a gold layer.

상기 기재 입자의 표면 상에 상기 도전층 또는 상기 제1 도전층을 형성하는 방법 및 상기 제1 도전층의 표면 상에 상기 제2 도전층을 형성하는 방법은 특별히 한정되지 않는다. 도전층을 형성하는 방법으로서는, 예를 들어 무전해 도금에 의한 방법, 전기 도금에 의한 방법, 물리적 증착에 의한 방법, 및 금속 분말 또는 금속 분말과 결합제를 포함하는 페이스트를 기재 입자 또는 다른 도전층의 표면에 코팅하는 방법 등을 들 수 있다. 그 중에서도, 도전층의 형성이 간편하므로, 무전해 도금에 의한 방법이 바람직하다. 상기 물리적 증착에 의한 방법으로서는, 진공 증착, 이온 플레이팅 및 이온 스퍼터링 등의 방법을 들 수 있다.The method of forming the conductive layer or the first conductive layer on the surface of the substrate particle and the method of forming the second conductive layer on the surface of the first conductive layer are not particularly limited. As a method for forming the conductive layer, for example, a method by electroless plating, a method by electroplating, a method by physical vapor deposition, and a paste containing a metal powder or a metal powder and a binder may be used as a base particle or other conductive layer. And a method of coating on the surface. Especially, since the formation of a conductive layer is easy, the method by electroless plating is preferable. Examples of the method by physical vapor deposition include vacuum vapor deposition, ion plating and ion sputtering.

상기 도전성 입자의 입자 직경은, 바람직하게는 0.5㎛ 이상, 보다 바람직하게는 1㎛ 이상, 바람직하게는 100㎛ 이하, 보다 바람직하게는 20㎛ 이하이다. 도전성 입자의 입자 직경이 상기 하한 이상 및 상한 이하이면, 도전성 입자를 사용하여 전극 간을 접속한 경우에, 도전성 입자와 전극과의 접촉 면적이 충분히 커지며, 도전층을 형성할 때에 응집한 도전성 입자가 형성되기 어려워진다. 또한, 도전성 입자를 통해 접속된 전극 간의 간격이 너무 커지지 않으며, 도전층이 기재 입자의 표면으로부터 박리하기 어려워진다.The particle diameter of the conductive particles is preferably 0.5 μm or more, more preferably 1 μm or more, preferably 100 μm or less, and more preferably 20 μm or less. When the particle diameter of the conductive particles is greater than or equal to the above lower limit and less than or equal to the upper limit, when the electrodes are connected using conductive particles, the contact area between the conductive particles and the electrode is sufficiently large, and the conductive particles aggregated when forming the conductive layer It becomes difficult to form. In addition, the gap between the electrodes connected through the conductive particles is not too large, and the conductive layer is difficult to peel off from the surface of the substrate particles.

상기 도전성 입자의 입자 직경은, 도전성 입자가 진구상인 경우에는 직경을 나타내고, 도전성 입자가 진구상이 아닌 경우에는 최대 직경을 나타낸다.The particle diameter of the said electroconductive particle shows the diameter when electroconductive particle is spherical shape, and shows the largest diameter when electroconductive particle is not spherical shape.

도전성 입자에 있어서의 도전층 전체의 두께 및 도전층이 단층인 경우의 도전층 두께는, 바람직하게는 0.005㎛ 이상, 보다 바람직하게는 0.01㎛ 이상, 더욱 바람직하게는 0.05㎛ 이상, 바람직하게는 1㎛ 이하, 보다 바람직하게는 0.3㎛ 이하이다. 상기 도전층의 두께가 상기 하한 이상 및 상기 상한 이하이면, 충분한 도전성이 얻어지며, 도전성 입자가 너무 단단해지지 않고, 전극 간의 접속시에 도전성 입자가 충분히 변형된다.The thickness of the entire conductive layer in the conductive particles and the thickness of the conductive layer when the conductive layer is a single layer are preferably 0.005 µm or more, more preferably 0.01 µm or more, still more preferably 0.05 µm or more, and preferably 1 Μm or less, more preferably 0.3 µm or less. When the thickness of the conductive layer is greater than or equal to the lower limit and less than or equal to the upper limit, sufficient conductivity is obtained, the conductive particles are not too hard, and the conductive particles are sufficiently deformed during connection between the electrodes.

도전층이 2층 이상의 적층 구조인 경우에, 기재 입자에 접하는 도전층(제1 도전층)의 두께는, 바람직하게는 0.001㎛ 이상, 보다 바람직하게는 0.01㎛ 이상, 더욱 바람직하게는 0.05㎛ 이상, 바람직하게는 0.5㎛ 이하, 보다 바람직하게는 0.3㎛ 이하, 더욱 바람직하게는 0.1㎛ 이하이다. 기재 입자에 접하는 도전층의 두께가 상기 하한 이상 및 상기 상한 이하이면, 도전층에 의한 피복을 균일하게 할 수 있으며, 전극 간의 접속 저항이 충분히 낮아진다.When the conductive layer has a laminated structure of two or more layers, the thickness of the conductive layer (first conductive layer) in contact with the substrate particles is preferably 0.001 μm or more, more preferably 0.01 μm or more, still more preferably 0.05 μm or more , Preferably 0.5 μm or less, more preferably 0.3 μm or less, still more preferably 0.1 μm or less. When the thickness of the conductive layer in contact with the substrate particles is greater than or equal to the above lower limit and less than or equal to the upper limit, the coating by the conductive layer can be made uniform, and the connection resistance between the electrodes is sufficiently low.

도전성 입자에 있어서의 도전층 전체의 두께 및 도전층이 단층인 경우의 도전층 두께는 0.05㎛ 이상, 0.3㎛ 이하인 것이 특히 바람직하다. 또한, 기재 입자의 입자 직경이 2㎛ 이상, 5㎛ 이하이며, 도전성 입자에 있어서의 도전층 전체의 두께 및 도전층이 단층인 경우의 도전층 두께가 0.05㎛ 이상, 0.3㎛ 이하인 것이 특히 바람직하다. 이 경우에는, 도전성 입자를 큰 전류가 흐르는 용도에 보다 적합하게 사용할 수 있다. 또한, 도전성 입자를 압축하여 전극 간을 접속한 경우에, 전극이 손상하는 것을 보다 한층 억제할 수 있다.The thickness of the entire conductive layer in the conductive particles and the thickness of the conductive layer when the conductive layer is a single layer are particularly preferably 0.05 µm or more and 0.3 µm or less. Moreover, it is particularly preferable that the particle diameter of the substrate particles is 2 μm or more and 5 μm or less, and the thickness of the entire conductive layer in the conductive particles and the thickness of the conductive layer when the conductive layer is a single layer is 0.05 μm or more and 0.3 μm or less. . In this case, the conductive particles can be more suitably used for applications in which a large current flows. In addition, when the electrodes are connected by compressing the conductive particles, damage to the electrodes can be further suppressed.

상기 도전층의 두께는, 예를 들어 투과형 전자 현미경(TEM)을 사용하여, 도전성 입자의 단면을 관찰함으로써 측정할 수 있다.The thickness of the said conductive layer can be measured by observing the cross section of electroconductive particle, for example using a transmission electron microscope (TEM).

상기 도전층 및 상기 제1 도전층에 있어서의 니켈, 붕소 및 인의 함유량을 제어하는 방법으로서는, 예를 들어 무전해 니켈 도금에 의해 도전층을 형성할 때에 니켈 도금액의 pH를 제어하는 방법, 무전해 니켈 도금에 의해 도전층을 형성할 때에 붕소 함유 환원제의 농도를 조정하는 방법, 무전해 니켈 도금에 의해 도전층을 형성할 때에 인 함유 환원제의 농도를 조정하는 방법, 및 니켈 도금액 중의 니켈 농도를 조정하는 방법 등을 들 수 있다.As a method of controlling the content of nickel, boron and phosphorus in the conductive layer and the first conductive layer, for example, a method of controlling the pH of a nickel plating solution when forming a conductive layer by electroless nickel plating, electroless Method for adjusting the concentration of the boron-containing reducing agent when forming the conductive layer by nickel plating, method for adjusting the concentration of the phosphorus-containing reducing agent when forming the conductive layer by electroless nickel plating, and adjusting the nickel concentration in the nickel plating solution And the like.

무전해 도금에 의해 형성하는 방법에서는, 일반적으로 촉매화 공정과, 무전해 도금 공정이 행해진다. 이하, 무전해 도금에 의해 수지 입자의 표면에 니켈과 붕소를 포함하는 합금 도금층을 형성하는 방법의 일례를 설명한다.In the method of forming by electroless plating, a catalytic process and an electroless plating process are generally performed. Hereinafter, an example of a method of forming an alloy plating layer containing nickel and boron on the surface of resin particles by electroless plating will be described.

상기 촉매화 공정도에서는, 무전해 도금에 의해 도금층을 형성하기 위한 기점이 되는 촉매를 수지 입자의 표면에 형성시킨다.In the catalytic process drawing, a catalyst serving as a starting point for forming a plating layer by electroless plating is formed on the surface of the resin particles.

상기 촉매를 수지 입자의 표면에 형성시키는 방법으로서는, 예를 들어 염화팔라듐과 염화주석을 포함하는 용액에 수지 입자를 첨가한 후, 산 용액 또는 알칼리 용액에 의해 수지 입자의 표면을 활성화시켜, 수지 입자의 표면에 팔라듐을 석출시키는 방법, 및 황산팔라듐과 아미노 피리딘을 함유하는 용액에 수지 입자를 첨가한 후, 환원제를 포함하는 용액에 의해 수지 입자의 표면을 활성화시켜, 수지 입자의 표면에 팔라듐을 석출시키는 방법 등을 들 수 있다. 상기 환원제로서, 붕소 함유 환원제가 적절하게 사용된다. 또한, 상기 환원제로서, 인 함유 환원제를 사용함으로써 인을 포함하는 도전층을 형성할 수 있다.As a method of forming the catalyst on the surface of the resin particles, for example, after adding the resin particles to a solution containing palladium chloride and tin chloride, the surface of the resin particles is activated by an acid solution or an alkali solution, and the resin particles After the method of depositing palladium on the surface of the, and after adding the resin particles to a solution containing palladium sulfate and amino pyridine, the surface of the resin particles is activated by a solution containing a reducing agent to deposit palladium on the surface of the resin particles And a method for prescribing. As the reducing agent, a boron-containing reducing agent is suitably used. Moreover, a conductive layer containing phosphorus can be formed by using a phosphorus-containing reducing agent as the reducing agent.

상기 무전해 도금 공정에서는, 니켈 함유 화합물 및 상기 붕소 함유 환원제를 포함하는 니켈 도금욕이 적절하게 사용된다. 니켈 도금욕 중에 수지 입자를 침지시킴으로써, 촉매가 표면에 형성된 수지 입자의 표면에 니켈을 석출시킬 수 있고, 니켈과 붕소를 포함하는 도전층을 형성할 수 있다.In the electroless plating process, a nickel plating bath containing a nickel-containing compound and the boron-containing reducing agent is suitably used. By immersing the resin particles in a nickel plating bath, the catalyst can deposit nickel on the surface of the resin particles formed on the surface, and a conductive layer containing nickel and boron can be formed.

상기 니켈 함유 화합물로서는, 황산니켈 및 염화니켈 등을 들 수 있다. 상기 니켈 함유 화합물은 니켈염인 것이 바람직하다.Nickel sulfate, nickel chloride, etc. are mentioned as said nickel containing compound. It is preferable that the nickel-containing compound is a nickel salt.

상기 붕소 함유 환원제로서는, 디메틸아민보란, 수소화붕소나트륨 및 수소화붕소칼륨 등을 들 수 있다. 상기 인 함유 환원제로서는, 차아인산나트륨 등을 들 수 있다.Examples of the boron-containing reducing agent include dimethylamine borane, sodium borohydride, and potassium borohydride. Sodium hypophosphite etc. are mentioned as said phosphorus containing reducing agent.

[도전재][Conductive material]

본 발명에 따른 도전성 입자는 기재 입자의 표면 상에 배치된 도전재를 구비한다. 해당 도전재의 재질은, 몰리브덴(Mo)(모스 경도 5.5), 텅스텐(W)(모스 경도 7.5), 탄화텅스텐(WC)(모스 경도 9), 탄화티타늄(TiC)(모스 경도 9), 또는 탄화탄탈(TaC)(모스 경도 9)인 것이 바람직하다. 도전성 입자가, 이 특정한 재질의 도전재를 구비함으로써, 도전성 입자의 도전성 표면이 충분히 단단해져, 전극 간의 접속 저항을 상당히 낮게 할 수 있다. 상기 도전재의 재질 모스 경도는 니켈(Ni)(모스 경도 5.0)의 모스 경도보다도 높다. 상기 도전재의 재질은 탄화텅스텐 또는 탄화탄탈인 것이 바람직하다. 상기 도전재의 재질은 몰리브덴인 것이 바람직하고, 텅스텐인 것이 바람직하고, 탄화텅스텐인 것이 바람직하고, 탄화티타늄인 것이 바람직하고, 탄화탄탈인 것이 바람직하다.The conductive particles according to the present invention include a conductive material disposed on the surface of the substrate particles. The material of the conductive material is molybdenum (Mo) (Mohs hardness 5.5), tungsten (W) (Mohs hardness 7.5), tungsten carbide (WC) (Moss hardness 9), titanium carbide (TiC) (Moss hardness 9), or carbonization It is preferably tantalum (TaC) (Mohs hardness 9). When the electroconductive particle is provided with the conductive material of this specific material, the electroconductive particle becomes sufficiently hard, and the connection resistance between electrodes can be made quite low. The Mohs hardness of the conductive material is higher than the Mohs hardness of nickel (Ni) (Mohs hardness 5.0). The material of the conductive material is preferably tungsten carbide or tantalum carbide. The material of the conductive material is preferably molybdenum, preferably tungsten, preferably tungsten carbide, preferably titanium carbide, and preferably tantalum carbide.

상기 도전재의 분체 저항률의 값은 0.1Ω·cm 이하인 것이 바람직하다.It is preferable that the value of the powder resistivity of the conductive material is 0.1 Ω · cm or less.

본 발명에 따른 도전성 입자는 도전성의 표면에 돌기를 갖는 것이 바람직하다. 상기 도전층은 외측의 표면에 돌기를 갖는 것이 바람직하다. 해당 돌기는 복수인 것이 바람직하다. 도전성 입자에 의해 접속되는 전극의 표면에는, 산화 피막이 형성되어 있는 경우가 많다. 또한, 도전성 입자의 도전층 표면에는, 산화 피막이 형성되어 있는 경우가 많다. 돌기를 갖는 도전성 입자의 사용에 의해, 전극 간에 도전성 입자를 배치한 후, 압착시킴으로써, 돌기에 의해 산화 피막이 효과적으로 배제된다. 상기 돌기의 내측에 특정한 재질의 상기 도전재가 존재함으로써, 돌기에 의해 산화 피막이 상당히 배제되기 쉬워진다. 이로 인해, 전극과 도전성 입자를 보다 한층 확실하게 접촉시킬 수 있고, 전극 간의 접속 저항을 낮게 할 수 있다. 또한, 도전성 입자가 표면에 절연성 물질을 갖는 경우, 또는 도전성 입자가 결합제 수지 중에 분산되어 도전 재료로서 사용할 수 있는 경우에, 도전성 입자의 돌기에 의해 도전성 입자와 전극 사이의 수지를 효과적으로 배제할 수 있다. 이로 인해, 전극 간의 도통 신뢰성을 높일 수 있다.It is preferable that the electroconductive particle which concerns on this invention has a processus | protrusion on the surface of electroconductivity. It is preferable that the said conductive layer has a processus | protrusion on the outer surface. It is preferable that the protrusion is plural. In many cases, an oxide film is formed on the surface of the electrode connected by the conductive particles. In addition, an oxide film is often formed on the surface of the conductive layer of the conductive particles. By using the conductive particles having protrusions, after placing the conductive particles between the electrodes, by pressing, the oxide film is effectively removed by the protrusions. When the conductive material of a specific material is present inside the projection, the oxide film is easily excluded by the projection. For this reason, the electrode and the conductive particles can be brought into contact more reliably, and the connection resistance between the electrodes can be made low. Further, when the conductive particles have an insulating material on the surface, or when the conductive particles are dispersed in a binder resin and can be used as a conductive material, the protrusion between the conductive particles can effectively exclude the resin between the conductive particles and the electrode. . For this reason, the reliability of conduction between electrodes can be improved.

상기 도전재가 상기 도전층 중에 매입되어 있음으로써, 상기 도전층이 외측의 표면에 복수의 돌기를 갖도록 하는 것이 용이하다.When the conductive material is embedded in the conductive layer, it is easy for the conductive layer to have a plurality of protrusions on its outer surface.

상기 도전성 입자가 상기 도전층을 구비하는 경우에, 상기 도전재는, 상기 기재 입자에 접하고 있을 수도 있고, 접하고 있지 않을 수도 있다. 상기 기재 입자와 상기 도전재와의 사이에 상기 도전층의 일부가 배치되어 있을 수도 있다.When the conductive particles include the conductive layer, the conductive material may or may not be in contact with the substrate particles. A part of the conductive layer may be disposed between the substrate particle and the conductive material.

본 발명에 따른 도전성 입자는 복수의 상기 도전재를 구비하는 것이 바람직하다. 이 경우에는, 도전층의 내측에 복수의 상기 도전재가 배치되어 있는 개소에서, 도전성 입자의 도전부를 단단하게 할 수 있다. 또한, 도전성 입자 및 도전층의 표면에 복수의 돌기를 형성하는 것이 용이하다.It is preferable that the conductive particles according to the present invention include a plurality of the conductive materials. In this case, the conductive portion of the conductive particles can be hardened at a location where a plurality of the conductive materials are disposed inside the conductive layer. Further, it is easy to form a plurality of protrusions on the surfaces of the conductive particles and the conductive layer.

상기 도전재는 입자인 것이 바람직하다. 이 경우에는, 도전층의 내측에 배치된 입자인 도전재의 형상에서 유래하여, 도전성 입자의 도전부를 효과적으로 단단하게 할 수 있다. 또한, 도전성 입자 및 도전층의 표면에 복수의 돌기를 형성하는 것이 용이하다.It is preferable that the said conductive material is a particle. In this case, originating from the shape of the conductive material which is the particles disposed inside the conductive layer, it is possible to effectively harden the conductive portion of the conductive particles. Further, it is easy to form a plurality of protrusions on the surfaces of the conductive particles and the conductive layer.

입자인 상기 도전재의 형상은 괴상인 것이 바람직하다. 입자인 상기 도전재로서는, 예를 들어 입자상의 덩어리, 복수의 미소 입자가 응집한 응집 덩어리 및 부정형의 덩어리 등을 들 수 있다.It is preferable that the shape of the said conductive material which is a particle is a mass. Examples of the conductive material that is a particle include, for example, a particle-like lump, agglomeration lumps in which a plurality of microparticles are aggregated, and an amorphous lump.

상기 기재 입자의 입자 직경을 D로 했을 때에, 상기 도전재의 최대 직경은 바람직하게는 0.005D 이상, 보다 바람직하게는 0.015D 이상, 바람직하게는 0.25D 이하, 보다 바람직하게는 0.15D 이하이다.When the particle diameter of the substrate particles is D, the maximum diameter of the conductive material is preferably 0.005D or more, more preferably 0.015D or more, preferably 0.25D or less, and more preferably 0.15D or less.

또한, 상기 기재 입자의 입자 직경을 D로 했을 때에, 상기 도전층의 두께 방향에 있어서의 상기 도전재의 크기는, 바람직하게는 0.005D 이상, 보다 바람직하게는 0.015D 이상, 바람직하게는 0.25D 이하, 보다 바람직하게는 0.15D 이하이다.In addition, when the particle diameter of the substrate particles is D, the size of the conductive material in the thickness direction of the conductive layer is preferably 0.005D or more, more preferably 0.015D or more, preferably 0.25D or less , More preferably, it is 0.15D or less.

상기 돌기를 형성하는 방법으로서는, 기재 입자의 표면에 상기 도전재를 부착시킨 후 무전해 도금에 의해 도전층을 형성하는 방법, 및 기재 입자의 표면에 무전해 도금에 의해 도전층을 형성한 후 상기 도전재를 부착시키고, 추가로 무전해 도금에 의해 도전층을 형성하는 방법 등을 들 수 있다. 상기 돌기를 형성하는 다른 방법으로서는, 기재 입자의 표면 상에 제1 도전층을 형성한 후, 해당 제1 도전층 상에 상기 도전재를 배치하고, 다음으로 제2 도전층을 형성하는 방법, 및 기재 입자의 표면 상에 도전층을 형성하는 도중 단계에서 상기 도전재를 첨가하는 방법 등을 들 수 있다.As a method of forming the protrusions, after attaching the conductive material to the surface of the substrate particles, a method of forming a conductive layer by electroless plating, and after forming a conductive layer by electroless plating on the surface of the substrate particles, And a method in which a conductive material is adhered and a conductive layer is formed by electroless plating. As another method of forming the protrusions, after forming a first conductive layer on the surface of the substrate particles, a method of disposing the conductive material on the first conductive layer, and then forming a second conductive layer, and And a method of adding the conductive material in a step in the middle of forming the conductive layer on the surface of the substrate particle.

상기 도전성 입자 1개당의 상기 도전재의 수 및 상기 돌기의 수는 각각, 바람직하게는 3개 이상, 보다 바람직하게는 5개 이상이다. 상기 도전재의 수 및 상기 돌기의 수의 상한은 특별히 한정되지 않는다. 상기 도전재의 수 및 상기 돌기의 수의 상한은 도전성 입자의 입자 직경 등을 고려하여 적절히 선택할 수 있다.The number of the conductive material and the number of protrusions per one of the conductive particles are preferably 3 or more, and more preferably 5 or more. The upper limit of the number of the conductive materials and the number of the projections is not particularly limited. The upper limit of the number of the conductive materials and the number of the protrusions can be appropriately selected in consideration of the particle diameter of the conductive particles and the like.

[절연성 물질][Insulating material]

본 발명에 따른 도전성 입자는, 상기 도전층의 표면 상에 배치된 절연성 물질을 구비하는 것이 바람직하다. 이 경우에는, 도전성 입자를 전극 간의 접속에 사용하면, 인접하는 전극 간의 단락을 보다 한층 방지할 수 있다. 구체적으로는, 복수의 도전성 입자가 접촉했을 때에, 복수의 전극 간에 절연성 물질이 존재하므로, 상하의 전극 간이 아닌, 가로 방향에 인접하는 전극 간의 단락을 방지할 수 있다. 또한, 전극 간의 접속시에 2개의 전극으로 도전성 입자를 가압함으로써, 도전성 입자의 도전층과 전극과의 사이의 절연성 물질을 용이하게 배제할 수 있다. 도전성 입자가 도전층의 외측 표면에 복수의 돌기를 갖는 경우에는, 도전성 입자의 도전층과 전극 사이의 절연성 물질을 용이하게 배제할 수 있다.It is preferable that the conductive particles according to the present invention include an insulating material disposed on the surface of the conductive layer. In this case, when the conductive particles are used for connection between electrodes, short circuit between adjacent electrodes can be further prevented. Specifically, when a plurality of conductive particles are in contact, an insulating material is present between the plurality of electrodes, so that a short circuit between the electrodes adjacent to the lateral direction rather than between the upper and lower electrodes can be prevented. Further, by pressing the conductive particles with two electrodes at the time of connection between the electrodes, the insulating material between the conductive layer of the conductive particles and the electrode can be easily removed. When the conductive particles have a plurality of protrusions on the outer surface of the conductive layer, the insulating material between the conductive layer of the conductive particles and the electrode can be easily removed.

전극 간의 압착시에 상기 절연성 물질을 보다 한층 용이하게 배제할 수 있는 점에서, 상기 절연성 물질은 절연성 입자인 것이 바람직하다.It is preferable that the insulating material is insulating particles in that the insulating material can be more easily excluded when crimping between electrodes.

상기 절연성 물질의 재료인 절연성 수지의 구체예로서는, 폴리올레핀류, (메트)아크릴레이트 중합체, (메트)아크릴레이트 공중합체, 블록 중합체, 열가소성 수지, 열가소성 수지의 가교물, 열경화성 수지 및 수용성 수지 등을 들 수 있다.Specific examples of the insulating resin as a material for the insulating material include polyolefins, (meth) acrylate polymers, (meth) acrylate copolymers, block polymers, thermoplastic resins, crosslinked products of thermoplastic resins, thermosetting resins, and water-soluble resins. You can.

(도전 재료)(Challenge material)

본 발명에 따른 도전 재료는 상술한 도전성 입자와 결합제 수지를 포함한다. 본 발명에 따른 도전성 입자는, 결합제 수지 중에 분산되어 도전 재료로서 사용할 수 있는 것이 바람직하다. 상기 도전 재료는 이방성 도전 재료인 것이 바람직하다.The conductive material according to the present invention includes the aforementioned conductive particles and a binder resin. It is preferable that the electroconductive particle which concerns on this invention is disperse | distributed in binder resin and can be used as an electroconductive material. It is preferable that the said conductive material is an anisotropic conductive material.

상기 결합제 수지는 특별히 한정되지 않는다. 상기 결합제 수지로서, 공지된 절연성의 수지가 사용된다.The binder resin is not particularly limited. As the binder resin, a known insulating resin is used.

상기 결합제 수지로서는, 예를 들어 비닐 수지, 열가소성 수지, 경화성 수지, 열가소성 블록 공중합체 및 엘라스토머 등을 들 수 있다. 상기 결합제 수지는 1종만이 사용될 수도 있고, 2종 이상이 병용될 수도 있다.As said binder resin, vinyl resin, a thermoplastic resin, curable resin, a thermoplastic block copolymer, an elastomer, etc. are mentioned, for example. As for the said binder resin, only 1 type may be used and 2 or more types may be used together.

상기 비닐 수지로서는, 예를 들어 아세트산 비닐 수지, 아크릴 수지 및 스티렌 수지 등을 들 수 있다. 상기 열가소성 수지로서는, 예를 들어 폴리올레핀 수지, 에틸렌-아세트산 비닐 공중합체 및 폴리아미드 수지 등을 들 수 있다. 상기 경화성 수지로서는, 예를 들어 에폭시 수지, 우레탄 수지, 폴리이미드 수지 및 불포화 폴리에스테르 수지 등을 들 수 있다. 또한, 상기 경화성 수지는, 상온 경화형 수지, 열경화형 수지, 광경화형 수지 또는 습기 경화형 수지일 수도 있다. 상기 경화성 수지는 경화제와 병용될 수도 있다. 상기 열가소성 블록 공중합체로서는, 예를 들어 스티렌-부타디엔-스티렌 블록 공중합체, 스티렌-이소프렌-스티렌 블록 공중합체, 스티렌-부타디엔-스티렌 블록 공중합체의 수소 첨가물 및 스티렌-이소프렌-스티렌 블록 공중합체의 수소 첨가물 등을 들 수 있다. 상기 엘라스토머로서는, 예를 들어 스티렌-부타디엔 공중합 고무 및 아크릴로니트릴-스티렌 블록 공중합 고무 등을 들 수 있다.As said vinyl resin, vinyl acetate resin, acrylic resin, styrene resin, etc. are mentioned, for example. As said thermoplastic resin, polyolefin resin, ethylene-vinyl acetate copolymer, polyamide resin, etc. are mentioned, for example. Examples of the curable resin include epoxy resins, urethane resins, polyimide resins, and unsaturated polyester resins. Further, the curable resin may be a room temperature curable resin, a thermosetting resin, a photocurable resin, or a moisture curable resin. The curable resin may be used in combination with a curing agent. As the thermoplastic block copolymer, for example, styrene-butadiene-styrene block copolymer, styrene-isoprene-styrene block copolymer, hydrogenation of styrene-butadiene-styrene block copolymer and hydrogen of styrene-isoprene-styrene block copolymer And additives. Examples of the elastomers include styrene-butadiene copolymer rubber, acrylonitrile-styrene block copolymer rubber, and the like.

상기 도전 재료는, 상기 도전성 입자 및 상기 결합제 수지 이외에, 예를 들어 충전제, 증량제, 연화제, 가소제, 중합 촉매, 경화 촉매, 착색제, 산화 방지제, 열 안정제, 광 안정제, 자외선 흡수제, 활제, 대전 방지제 및 난연제 등의 각종 첨가제를 포함하고 있을 수도 있다.The conductive material, in addition to the conductive particles and the binder resin, for example, fillers, extenders, softeners, plasticizers, polymerization catalysts, curing catalysts, colorants, antioxidants, heat stabilizers, light stabilizers, ultraviolet absorbers, lubricants, antistatic agents and It may contain various additives such as flame retardants.

상기 결합제 수지 중에 상기 도전성 입자를 분산시키는 방법은 종래 공지된 분산 방법을 사용할 수 있고, 특별히 한정되지 않는다. 상기 결합제 수지 중에 상기 도전성 입자를 분산시키는 방법으로서는, 예를 들어 상기 결합제 수지 중에 상기 도전성 입자를 첨가한 후, 플라너터리 믹서 등에서 혼련하여 분산시키는 방법, 상기 도전성 입자를 물 또는 유기 용제 중에 호모게나이저 등을 사용하여 균일하게 분산시킨 후, 상기 결합제 수지 중에 첨가하고, 플라너터리 믹서 등으로 혼련하여 분산시키는 방법, 및 상기 결합제 수지를 물 또는 유기 용제 등으로 희석한 후, 상기 도전성 입자를 첨가하고, 플라너터리 믹서 등으로 혼련하여 분산시키는 방법 등을 들 수 있다.The method for dispersing the conductive particles in the binder resin can use a conventionally known dispersion method, and is not particularly limited. As a method for dispersing the conductive particles in the binder resin, for example, after adding the conductive particles in the binder resin, kneading and dispersing in a planetary mixer or the like, the conductive particles are homogeneous in water or an organic solvent. After uniformly dispersing using a Niger or the like, adding to the binder resin, kneading and dispersing with a planetary mixer, etc., and after diluting the binder resin with water or an organic solvent, the conductive particles are added. And kneading and dispersing with a planetary mixer or the like.

본 발명에 따른 도전 재료는, 도전 페이스트 및 도전 필름 등으로서 사용될 수 있다. 본 발명에 따른 도전 재료가 도전 필름인 경우에는, 상기 도전성 입자를 포함하는 도전 필름에, 도전성 입자를 포함하지 않는 필름이 적층되어 있을 수도 있다. 상기 도전 페이스트는 이방성 도전 페이스트인 것이 바람직하다. 상기 도전 필름은 이방성 도전 필름인 것이 바람직하다.The conductive material according to the present invention can be used as a conductive paste and a conductive film. When the conductive material according to the present invention is a conductive film, a film not containing conductive particles may be laminated on the conductive film containing the conductive particles. It is preferable that the said conductive paste is an anisotropic conductive paste. It is preferable that the said conductive film is an anisotropic conductive film.

상기 도전 재료 100중량％ 중, 상기 결합제 수지의 함유량은, 바람직하게는 10중량％ 이상, 보다 바람직하게는 30중량％ 이상, 더욱 바람직하게는 50중량％ 이상, 특히 바람직하게는 70중량％ 이상, 바람직하게는 99.99중량％ 이하, 보다 바람직하게는 99.9중량％ 이하이다. 상기 결합제 수지의 함유량이 상기 하한 이상 및 상기 상한 이하이면, 전극 간에 도전성 입자가 효율적으로 배치되어, 도전 재료에 의해 접속된 접속 대상 부재의 접속 신뢰성이 보다 한층 높아진다.The content of the binder resin in 100% by weight of the conductive material is preferably 10% by weight or more, more preferably 30% by weight or more, further preferably 50% by weight or more, particularly preferably 70% by weight or more, Preferably it is 99.99 weight% or less, More preferably, it is 99.9 weight% or less. When the content of the binder resin is greater than or equal to the lower limit and less than or equal to the upper limit, conductive particles are efficiently disposed between the electrodes, and connection reliability of the connection target member connected by the conductive material is further increased.

상기 도전 재료 100중량％ 중, 상기 도전성 입자의 함유량은, 바람직하게는 0.01중량％ 이상, 보다 바람직하게는 0.1중량％ 이상, 바람직하게는 40중량％ 이하, 보다 바람직하게는 20중량％ 이하, 더욱 바람직하게는 10중량％ 이하이다. 상기 도전성 입자의 함유량이 상기 하한 이상 및 상기 상한 이하이면, 전극 간의 도통 신뢰성이 보다 한층 높아진다.The content of the conductive particles in 100% by weight of the conductive material is preferably 0.01% by weight or more, more preferably 0.1% by weight or more, preferably 40% by weight or less, more preferably 20% by weight or less, further It is preferably 10% by weight or less. When the content of the conductive particles is greater than or equal to the lower limit and less than or equal to the upper limit, the reliability of conduction between the electrodes is further increased.

(접속 구조체)(Connection structure)

본 발명의 도전성 입자를 사용하거나, 또는 상기 도전성 입자와 결합제 수지를 포함하는 도전 재료를 사용하여, 접속 대상 부재를 접속함으로써, 접속 구조체를 얻을 수 있다.A connection structure can be obtained by connecting the member to be connected by using the conductive particles of the present invention or by using the conductive particles and the conductive material containing the binder resin.

상기 접속 구조체는 제1 접속 대상 부재와, 제2 접속 대상 부재와, 제1 접속 대상 부재와 제2 접속 대상 부재를 접속하고 있는 접속부를 구비하고, 해당 접속부가 본 발명의 도전성 입자에 의해 형성되어 있거나, 또는 상기 도전성 입자와 결합제 수지를 포함하는 도전 재료에 의해 형성되어 있는 접속 구조체인 것이 바람직하다. 도전성 입자가 사용된 경우에는, 접속부 자체가 도전성 입자이다. 즉, 제1, 제2 접속 대상 부재가 도전성 입자에 의해 접속된다.The connection structure includes a first connection target member, a second connection target member, and a connection portion connecting the first connection target member and the second connection target member, and the connection portion is formed of the conductive particles of the present invention. Or it is preferable that it is a connection structure formed with the conductive material containing the said electroconductive particle and binder resin. When electroconductive particle is used, the connection part itself is electroconductive particle. That is, the 1st, 2nd connection target member is connected by electroconductive particle.

도 4에, 본 발명의 제1 실시 형태에 따른 도전성 입자를 사용한 접속 구조체를 모식적으로 정면 단면도로 나타내었다.4, the connection structure using the electroconductive particle which concerns on 1st Embodiment of this invention is typically shown in front sectional drawing.

도 4에 나타내는 접속 구조체(51)는, 제1 접속 대상 부재(52)와, 제2 접속 대상 부재(53)와, 제1, 제2 접속 대상 부재(52, 53)를 접속하고 있는 접속부(54)를 구비한다. 접속부(54)는, 도전성 입자(1)를 포함하는 도전 재료를 경화시킴으로써 형성되어 있다. 또한, 도 4에서는, 도전성 입자(1)는 도시의 편의상 대략도적으로 나타내고 있다.The connection structure 51 shown in FIG. 4 is a connection part connecting the first connection target member 52, the second connection target member 53, and the first and second connection target members 52, 53. 54). The connecting portion 54 is formed by curing a conductive material containing the conductive particles 1. In Fig. 4, the conductive particles 1 are schematically shown for convenience of illustration.

제1 접속 대상 부재(52)는 표면(상면)에, 복수의 제1 전극(52a)을 갖는다. 제2 접속 대상 부재(53)는 표면(하면)에, 복수의 제2 전극(53a)을 갖는다. 제1 전극(52a)과 제2 전극(53a)이 1개 또는 복수의 도전성 입자(1)에 의해 전기적으로 접속되어 있다. 따라서, 제1, 제2 접속 대상 부재(52, 53)가 도전성 입자(1)에 의해 전기적으로 접속되어 있다.The first connection target member 52 has a plurality of first electrodes 52a on its surface (upper surface). The second connection target member 53 has a plurality of second electrodes 53a on its surface (lower surface). The first electrode 52a and the second electrode 53a are electrically connected by one or a plurality of conductive particles 1. Therefore, the 1st, 2nd connection target members 52 and 53 are electrically connected by the electroconductive particle 1.

상기 접속 구조체의 제조 방법은 특별히 한정되지 않는다. 접속 구조체의 제조 방법 일례로서는, 제1 접속 대상 부재와 제2 접속 대상 부재와의 사이에 상기 도전 재료를 배치하고, 적층체를 얻은 후, 해당 적층체를 가열 및 가압하는 방법 등을 들 수 있다. 상기 가압의 압력은 9.8×104 내지 4.9×106Pa 정도이다. 상기 가열의 온도는 120 내지 220℃ 정도이다.The manufacturing method of the said connection structure is not specifically limited. As an example of the manufacturing method of a connection structure, after arrange | positioning the said electrically-conductive material between a 1st connection object member and a 2nd connection object member, and obtaining a laminated body, the method of heating and pressing the said laminated body, etc. are mentioned. . The pressure of the pressurization is about 9.8 × 10 4 to 4.9 × 10 6 Pa. The temperature of the heating is about 120 to 220 ° C.

상기 접속 대상 부재로서는, 구체적으로는 반도체칩, 콘덴서 및 다이오드 등의 전자 부품, 및 프린트 기판, 플렉시블 프린트 기판, 유리 에폭시 기판 및 유리 기판 등의 회로 기판 등의 전자 부품 등을 들 수 있다. 상기 도전 재료는 전자 부품을 접속하기 위한 도전 재료인 것이 바람직하다. 상기 도전 재료는 페이스트 상태의 도전 페이스트이고, 페이스트상의 상태에서 접속 대상 부재 상에 도포 시공되는 것이 바람직하다.Specific examples of the connection target member include electronic components such as semiconductor chips, capacitors and diodes, and electronic components such as printed circuit boards, flexible printed circuit boards, glass epoxy substrates, and circuit boards such as glass substrates. It is preferable that the said conductive material is a conductive material for connecting an electronic component. It is preferable that the conductive material is a conductive paste in a paste state, and is coated and applied on a member to be connected in a paste form.

상기 접속 대상 부재에 설치되어 있는 전극으로서는 금 전극, 니켈 전극, 주석 전극, 알루미늄 전극, 구리 전극, 몰리브덴 전극 및 텅스텐 전극 등의 금속 전극을 들 수 있다. 상기 접속 대상 부재가 플렉시블 프린트 기판인 경우에는, 상기 전극은 금 전극, 니켈 전극, 주석 전극 또는 구리 전극인 것이 바람직하다. 상기 접속 대상 부재가 유리 기판인 경우에는, 상기 전극은 알루미늄 전극, 구리 전극, 몰리브덴 전극 또는 텅스텐 전극인 것이 바람직하다. 또한, 상기 전극이 알루미늄 전극인 경우에는, 알루미늄만으로 형성된 전극일 수도 있고, 금속 산화물층의 표면에 알루미늄층이 적층된 전극일 수도 있다. 상기 금속 산화물층의 재료로서는, 3가의 금속 원소가 도핑된 산화인듐 및 3가의 금속 원소가 도핑된 산화아연 등을 들 수 있다. 상기 3가의 금속 원소로서는 Sn, Al 및 Ga 등을 들 수 있다.Examples of the electrodes provided on the connection target member include metal electrodes such as gold electrodes, nickel electrodes, tin electrodes, aluminum electrodes, copper electrodes, molybdenum electrodes, and tungsten electrodes. When the member to be connected is a flexible printed circuit board, the electrode is preferably a gold electrode, a nickel electrode, a tin electrode, or a copper electrode. When the member to be connected is a glass substrate, the electrode is preferably an aluminum electrode, a copper electrode, a molybdenum electrode, or a tungsten electrode. Further, when the electrode is an aluminum electrode, it may be an electrode formed of only aluminum, or an electrode in which an aluminum layer is laminated on the surface of a metal oxide layer. Examples of the material of the metal oxide layer include indium oxide doped with a trivalent metal element, zinc oxide doped with a trivalent metal element, and the like. Sn, Al, Ga, etc. are mentioned as said trivalent metal element.

본 발명에 따른 도전성 입자의 다른 사용 형태를 들면, 액정 표시 소자를 구성하는 동시 하부 기판 간의 전기적인 접속을 하기 위한 도통 재료로서 도전성 입자를 사용할 수도 있다. 도전성 입자를 열 경화성 수지 또는 열 UV 병용 경화성 수지에 혼합하여 분산시키고, 편측 기판 상에 점 형상으로 도포하여 대향 기판과 접합하는 방법, 및 도전성 입자를 주변 밀봉제에 혼합하여 분산시켜 선상으로 도포하여 밀봉 시일과 상하 기판의 전기 접속을 겸용하는 방법 등이 있다. 이러한 사용 형태에도 본 발명에 따른 도전성 입자는 적용할 수 있다.For another form of use of the conductive particles according to the present invention, conductive particles may also be used as a conductive material for electrical connection between the lower substrates constituting the liquid crystal display element. The conductive particles are mixed and dispersed in a heat-curable resin or a heat-curable resin used in combination with a heat UV, and a dot-shaped coating is applied on one side of the substrate to bond with the opposing substrate. There is a method of using both the sealing seal and the electrical connection of the upper and lower substrates. The conductive particles according to the present invention can also be applied to these use forms.

이하, 실시예 및 비교예를 들어, 본 발명을 구체적으로 설명한다. 본 발명은 이하의 실시예에만 한정되지 않는다.Hereinafter, the present invention will be specifically described with reference to Examples and Comparative Examples. The present invention is not limited to the following examples.

이하의 실시예에서 사용한 도전재의 분체 저항률은 0.1Ω·cm 이하의 값을 나타내었다. 도전재의 분체 저항률은, 구체적으로는 몰리브덴(Mo)(0.001Ω·cm), 텅스텐(W)(0.001Ω·cm), 탄화텅스텐(WC)(0.005Ω·cm), 탄화티타늄(TiC)(0.005Ω·cm), 탄화탄탈(TaC)(0.003Ω·cm)이었다.The powder resistivity of the conductive material used in the examples below was 0.1 Ω · cm or less. Specifically, the powder resistivity of the conductive material is molybdenum (Mo) (0.001 Ω · cm), tungsten (W) (0.001 Ω · cm), tungsten carbide (WC) (0.005 Ω · cm), titanium carbide (TiC) (0.005 Ω · cm) and tantalum carbide (TaC) (0.003 Ω · cm).

상기 분체 저항률은, 미쯔비시 가가꾸사 제조의 제분체 저항률 측정 시스템 「로레스터 GP」에서, 도전재 2.5g을 사용하여, 23℃에서 하중 20kN일 때의 분체 저항률로 구하였다.The said powder resistivity was calculated | required with the powder resistivity at the load of 20 kN at 23 degreeC using 2.5 g of conductive materials in the milling-resistance measurement system "Lorester GP" manufactured by Mitsubishi Chemical Corporation.

(실시예 1)(Example 1)

(1) 팔라듐 부착 공정(1) Palladium attachment process

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-205」)를 준비하였다. 이 수지 입자를 에칭하고, 수세하였다. 이어서, 팔라듐 촉매를 8중량％ 포함하는 팔라듐 촉매화 액 100mL 중에 수지 입자를 첨가하고, 교반하였다. 그 후, 여과하고, 세정하였다. pH6의 0.5중량％ 디메틸아민보란 액에 수지 입자를 첨가하여, 팔라듐이 부착된 수지 입자를 얻었다.Divinylbenzene resin particles ("Micro Pearl SP-205" manufactured by Sekisui Chemical Co., Ltd.) having a particle diameter of 3.0 µm were prepared. The resin particles were etched and washed with water. Subsequently, resin particles were added to 100 mL of the palladium catalyzed liquid containing 8% by weight of the palladium catalyst, and stirred. After that, it was filtered and washed. Resin particles were added to a 0.5 wt% dimethylamine borane solution at pH 6 to obtain resin particles with palladium attached thereto.

(2) 도전재 부착 공정(2) Conductive material attachment process

팔라듐이 부착된 수지 입자를 이온 교환수 400mL 중에서 3분간 교반하고, 분산시켜, 분산액을 얻었다. 이어서, 탄화텅스텐 입자(평균 입자 직경 100nm)를 5중량％ 포함하는 슬러리 400g을, 얻어진 분산액에 3분간 걸쳐 첨가하여, 도전재가 부착된 수지 입자를 포함하는 현탁액을 얻었다.The resin particles with palladium were stirred in 400 mL of ion-exchanged water for 3 minutes and dispersed to obtain a dispersion. Subsequently, 400 g of a slurry containing 5 wt% of tungsten carbide particles (average particle diameter of 100 nm) was added to the obtained dispersion solution over 3 minutes to obtain a suspension containing resin particles with a conductive material.

(3) 무전해 니켈 도금 공정(3) Electroless nickel plating process

황산니켈 0.23mol/L, 디메틸아민보란 0.92mol/L, 및 시트르산나트륨 0.5mol/L을 포함하는 니켈 도금액(pH8.5)을 준비하였다.A nickel plating solution (pH8.5) containing 0.23 mol / L nickel sulfate, 0.92 mol / L dimethylamine borane, and 0.5 mol / L sodium citrate was prepared.

얻어진 현탁액을 60℃에서 교반하면서, 상기 니켈 도금액을 현탁액에 서서히 적하하고, 무전해 니켈 도금을 행하였다. 그 후, 현탁액을 여과함으로써, 입자를 취출하고, 수세하고, 건조함으로써, 도전재가 부착된 수지 입자의 표면 상에 니켈층(두께 0.1㎛)이 배치된 도전성 입자를 얻었다. 니켈층 100중량％ 중의 니켈의 함유량은 98.9중량％, 붕소의 함유량은 1.1중량％였다. 얻어진 도전성 입자는, 도전층 내에 매입된 복수의 도전재를 구비하고 있고, 도전층의 외측 표면에 복수의 돌기를 갖고, 도전층의 돌기 내측에 도전재가 배치되어 있었다.While stirring the obtained suspension at 60 ° C, the nickel plating solution was slowly added dropwise to the suspension, and electroless nickel plating was performed. Thereafter, by filtering the suspension, particles were taken out, washed with water, and dried to obtain conductive particles in which a nickel layer (0.1 µm thick) was disposed on the surface of the resin particles with the conductive material. The content of nickel in 100% by weight of the nickel layer was 98.9% by weight, and the content of boron was 1.1% by weight. The obtained conductive particles were provided with a plurality of conductive materials embedded in the conductive layer, had a plurality of protrusions on the outer surface of the conductive layer, and a conductive material was disposed inside the protrusions of the conductive layer.

(실시예 2)(Example 2)

탄화텅스텐 입자(평균 입자 직경 100nm)를 텅스텐 입자(평균 입자 직경 100nm)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1, except that the tungsten carbide particles (average particle diameter 100 nm) were changed to tungsten particles (average particle diameter 100 nm).

(실시예 3)(Example 3)

탄화텅스텐 입자(평균 입자 직경 100nm)를 탄화탄탈 입자(평균 입자 직경 100nm)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1 except that the tungsten carbide particles (average particle diameter 100 nm) were changed to tantalum carbide particles (average particle diameter 100 nm).

(실시예 4)(Example 4)

탄화텅스텐 입자(평균 입자 직경 100nm)를 몰리브덴 입자(평균 입자 직경 100nm)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1 except that the tungsten carbide particles (average particle diameter 100 nm) were changed to molybdenum particles (average particle diameter 100 nm).

(실시예 5)(Example 5)

(1) 절연성 입자의 제작(1) Preparation of insulating particles

4구 세퍼러블 커버, 교반 날개, 삼방 코크, 냉각관 및 온도 프로브가 설치된 1000mL의 세퍼러블 플라스크에, 메타크릴산 메틸 100mmol과, N,N,N-트리메틸-N-2-메타크릴로일옥시에틸암모늄클로라이드 1mmol과, 2,2'-아조비스(2-아미디노프로판)이염산염 1mmol을 포함하는 단량체 조성물을 고형분율이 5중량％가 되도록 이온 교환수에 칭량한 후, 200rpm으로 교반하고, 질소 분위기하 70℃에서 24시간 중합을 행하였다. 반응 종료 후, 동결 건조하여, 표면에 암모늄기를 갖고, 평균 입자 직경 220nm 및 CV값 10％의 절연성 입자를 얻었다.100 mL methyl methacrylate and N, N, N-trimethyl-N-2-methacryloyloxy in a 1000 mL separable flask equipped with a 4-neck separable cover, stirring vane, three-way cock, cooling tube, and temperature probe The monomer composition containing 1 mmol of ethyl ammonium chloride and 1 mmol of 2,2'-azobis (2-amidinopropane) hydrochloride was weighed in ion-exchanged water so that the solid content was 5% by weight, and then stirred at 200 rpm. Polymerization was performed at 70 ° C for 24 hours under a nitrogen atmosphere. After completion of the reaction, freeze drying was performed to obtain insulating particles having an ammonium group on the surface and an average particle diameter of 220 nm and a CV value of 10%.

(2) 절연성 입자의 부착 공정(2) Process of attaching insulating particles

절연성 입자를 초음파 조사 하에서 이온 교환수에 분산시키고, 절연성 입자에 10중량％ 수분산액을 얻었다.The insulating particles were dispersed in ion-exchanged water under ultrasonic irradiation, and a 10% by weight aqueous dispersion was obtained on the insulating particles.

실시예 1에서 얻어진 도전성 입자 10g을 이온 교환수 500mL에 분산시켜, 절연성 입자의 수 분산액 4g을 첨가하고, 실온에서 6시간 교반하였다. 3㎛의 메쉬 필터로 여과한 후, 추가로 메탄올에서 세정하고, 건조하여, 절연성 입자가 부착된 도전성 입자를 얻었다.10 g of the conductive particles obtained in Example 1 were dispersed in 500 mL of ion-exchanged water, and 4 g of a water dispersion of insulating particles was added and stirred at room temperature for 6 hours. After filtration through a 3 µm mesh filter, further washed with methanol and dried to obtain conductive particles with insulating particles.

주사형 전자 현미경(SEM)에 의해 관찰한 바, 도전성 입자의 표면에 절연성 입자에 의한 피복층이 1층만 형성되어 있었다. 화상 해석에 의해 도전성 입자의 중심으로부터 2.5㎛의 면적에 대한 절연성 입자의 피복 면적(즉, 절연성 입자의 입자 직경 투영 면적)을 산출한 바, 피복률은 35％였다.As observed with a scanning electron microscope (SEM), only one layer of a coating layer made of insulating particles was formed on the surface of the conductive particles. When the coverage area of the insulating particles with respect to an area of 2.5 µm (that is, the particle diameter projection area of the insulating particles) was calculated from the center of the conductive particles by image analysis, the coverage was 35%.

(실시예 6)(Example 6)

절연성 입자를 부착시키기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 2에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 5와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 5, except that the conductive particles obtained in Example 1 before attaching the insulating particles were changed to those obtained in Example 2.

(실시예 7)(Example 7)

절연성 입자를 부착시키기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 3에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 5와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 5, except that the conductive particles obtained in Example 1 before adhering the insulating particles were replaced with those obtained in Example 3.

(실시예 8)(Example 8)

절연성 입자를 부착시키기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 4에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 5와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 5, except that the conductive particles obtained in Example 1 before attaching the insulating particles were changed to those obtained in Example 4.

(실시예 9)(Example 9)

실시예 1에서 얻어진 도전성 입자 10g을 이온 교환수 500mL에 첨가하고, 초음파 처리기에 의해 충분히 분산시켜, 현탁액을 얻었다. 이 현탁액을 50℃에서 교반하면서, 황산팔라듐 0.02mol/L, 착화제로서 에틸렌디아민 0.04mol/L, 환원제로서 포름산 나트륨 0.06mol/L 및 결정 조정제를 포함하는 pH10.0의 무전해 도금액을 준비하였다.10 g of the conductive particles obtained in Example 1 were added to 500 mL of ion-exchanged water, and sufficiently dispersed by an ultrasonicator to obtain a suspension. While stirring the suspension at 50 ° C, an electroless plating solution of pH 10.0 containing palladium sulfate 0.02 mol / L, ethylenediamine 0.04 mol / L as a complexing agent, sodium formate 0.06 mol / L as a reducing agent, and a crystal modifier was prepared. .

얻어진 현탁액에, 상기 무전해 도금액을 서서히 첨가하고, 무전해 팔라듐 도금을 행하였다. 팔라듐층의 두께가 0.03㎛가 된 시점에서 무전해 팔라듐 도금을 종료하였다. 이어서, 세정하고, 진공 건조함으로써, 니켈층의 표면에 팔라듐층(두께 0.03㎛)이 적층된 도전성 입자를 얻었다.The electroless plating solution was gradually added to the obtained suspension, and electroless palladium plating was performed. Electroless palladium plating was completed when the thickness of the palladium layer became 0.03 µm. Subsequently, by washing and drying under vacuum, conductive particles were obtained in which a palladium layer (0.03 µm thick) was laminated on the surface of the nickel layer.

(실시예 10)(Example 10)

팔라듐층을 형성하기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 2에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 9와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 9, except that the conductive particles obtained in Example 1 before forming the palladium layer were replaced with the conductive particles obtained in Example 2.

(실시예 11)(Example 11)

팔라듐층을 형성하기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 3에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 9와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 9, except that the conductive particles obtained in Example 1 before forming the palladium layer were replaced with the conductive particles obtained in Example 3.

(실시예 12)(Example 12)

팔라듐층을 형성하기 전의 실시예 1에서 얻어진 도전성 입자를 실시예 4에서 얻어진 도전성 입자로 변경한 것 이외에는 실시예 9와 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 9, except that the conductive particles obtained in Example 1 before forming the palladium layer were changed to those obtained in Example 4.

(실시예 13)(Example 13)

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-203」)를 입자 직경이 2.5㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-2025」)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Divinylbenzene resin particles having a particle diameter of 3.0 µm ("Micropearl SP-203" manufactured by Sekisui Chemical Co., Ltd.) and divinylbenzene resin particles having a particle diameter of 2.5 µm ("Micropearl" manufactured by Sekisui Chemical Co., Ltd.) SP-2025 ”), and the same procedure as in Example 1 was carried out to obtain conductive particles.

(실시예 14)(Example 14)

(1) 팔라듐 부착 공정(1) Palladium attachment process

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-203」)를 준비하였다. 이 수지 입자를 에칭하고, 수세하였다. 이어서, 팔라듐 촉매를 8중량％ 포함하는 팔라듐 촉매화 액 100mL 중에 수지 입자를 첨가하여, 교반하였다. 그 후, 여과하고, 세정하였다. pH6의 0.5중량％ 디메틸아민보란 액에 수지 입자를 첨가하여, 팔라듐이 부착된 수지 입자를 얻었다.Divinylbenzene resin particles having a particle diameter of 3.0 µm ("Micropearl SP-203" manufactured by Sekisui Chemical Co., Ltd.) were prepared. The resin particles were etched and washed with water. Subsequently, resin particles were added and stirred in 100 mL of a palladium catalyzed liquid containing 8% by weight of a palladium catalyst. After that, it was filtered and washed. Resin particles were added to a 0.5 wt% dimethylamine borane solution at pH 6 to obtain resin particles with palladium attached thereto.

(2) 도전재 부착 공정(2) Conductive material attachment process

팔라듐이 부착된 수지 입자를 이온 교환수 400mL 중에서 3분간 교반하고, 분산시켜, 분산액을 얻었다. 이어서, 탄화텅스텐 입자(평균 입자 직경 100nm)를 5중량％ 포함하는 슬러리 400g을, 얻어진 분산액에 3분간 걸쳐 첨가하여, 도전재가 부착된 수지 입자를 포함하는 현탁액을 얻었다.The resin particles with palladium were stirred in 400 mL of ion-exchanged water for 3 minutes and dispersed to obtain a dispersion. Subsequently, 400 g of a slurry containing 5 wt% of tungsten carbide particles (average particle diameter of 100 nm) was added to the obtained dispersion solution over 3 minutes to obtain a suspension containing resin particles with a conductive material.

(3) 무전해 니켈 도금 공정(3) Electroless nickel plating process

황산니켈 0.25mol/L, 차아인산나트륨 0.25mol/L 및 시트르산나트륨 0.15mol/L을 포함하는 니켈 도금액(pH9.0)을 준비하였다.A nickel plating solution (pH9.0) containing 0.25 mol / L of nickel sulfate, 0.25 mol / L of sodium hypophosphite, and 0.15 mol / L of sodium citrate was prepared.

얻어진 현탁액을 70℃에서 교반하면서, 상기 니켈 도금액을 현탁액에 서서히 적하하고, 무전해 니켈 도금을 행하였다. 그 후, 현탁액을 여과함으로써, 입자를 취출하고, 수세하고, 건조함으로써, 수지 입자의 표면에 니켈-인 도전층(두께 0.1 ㎛)이 배치된 도전성 입자를 얻었다.While stirring the obtained suspension at 70 ° C, the nickel plating solution was slowly added dropwise to the suspension, and electroless nickel plating was performed. Thereafter, by filtering the suspension, particles were taken out, washed with water, and dried to obtain conductive particles in which a nickel-phosphorus conductive layer (0.1 µm thick) was disposed on the surface of the resin particles.

(실시예 15)(Example 15)

(1) 팔라듐 부착 공정(1) Palladium attachment process

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-203」)를 준비하였다. 이 수지 입자를 에칭하고, 수세하였다. 이어서, 팔라듐 촉매를 8중량％ 포함하는 팔라듐 촉매화 액 100mL 중에 수지 입자를 첨가하고, 교반하였다. 그 후, 여과하고, 세정하였다. pH6의 0.5중량％ 디메틸아민보란 액에 수지 입자를 첨가하여, 팔라듐이 부착된 수지 입자를 얻었다.Divinylbenzene resin particles having a particle diameter of 3.0 µm ("Micropearl SP-203" manufactured by Sekisui Chemical Co., Ltd.) were prepared. The resin particles were etched and washed with water. Subsequently, resin particles were added to 100 mL of the palladium catalyzed liquid containing 8% by weight of the palladium catalyst, and stirred. After that, it was filtered and washed. Resin particles were added to a 0.5 wt% dimethylamine borane solution at pH 6 to obtain resin particles with palladium attached thereto.

(2) 도전재 부착 공정(2) Conductive material attachment process

팔라듐이 부착된 수지 입자를 이온 교환수 400mL 중에서 3분간 교반하고, 분산시켜, 분산액을 얻었다. 이어서, 탄화텅스텐 입자(평균 입자 직경 100nm)를 5중량％ 포함하는 슬러리 400g을, 얻어진 분산액에 3분간 걸쳐 첨가하여, 도전재가 부착된 수지 입자를 포함하는 현탁액을 얻었다.The resin particles with palladium were stirred in 400 mL of ion-exchanged water for 3 minutes and dispersed to obtain a dispersion. Subsequently, 400 g of a slurry containing 5 wt% of tungsten carbide particles (average particle diameter of 100 nm) was added to the obtained dispersion solution over 3 minutes to obtain a suspension containing resin particles with a conductive material.

(3) 무전해 니켈 도금 공정(3) Electroless nickel plating process

황산니켈 0.25mol/L, 차아인산나트륨 0.25mol/L 및 시트르산나트륨 0.15mol/L을 포함하는 니켈 도금액(pH6.0)을 준비하였다.A nickel plating solution (pH6.0) containing 0.25 mol / L of nickel sulfate, 0.25 mol / L of sodium hypophosphite, and 0.15 mol / L of sodium citrate was prepared.

얻어진 현탁액을 60℃에서 교반하면서, 상기 니켈 도금액을 현탁액에 서서히 적하하고, 무전해 니켈 도금을 행하였다. 계속해서, 황산니켈 0.25mol/L, 차아인산나트륨 0.25mol/L 및 시트르산나트륨 0.15mol/L을 포함하는 니켈 도금액(pH10.0)을 현탁액에 서서히 적하하고, 무전해 니켈 도금을 행하였다. 그 후, 현탁액을 여과함으로써, 입자를 취출하고, 수세하고, 건조함으로써, 수지 입자의 표면에 니켈-인 도전층(두께 0.1㎛)이 배치된 도전성 입자를 얻었다.While stirring the obtained suspension at 60 ° C, the nickel plating solution was slowly added dropwise to the suspension, and electroless nickel plating was performed. Subsequently, a nickel plating solution (pH 10.0) containing 0.25 mol / L of nickel sulfate, 0.25 mol / L of sodium hypophosphite, and 0.15 mol / L of sodium citrate was slowly added dropwise to the suspension, and electroless nickel plating was performed. Thereafter, by filtering the suspension, particles were taken out, washed with water, and dried to obtain conductive particles in which a nickel-phosphorus conductive layer (0.1 µm thick) was disposed on the surface of the resin particles.

(실시예 16)(Example 16)

(1) 팔라듐 부착 공정(1) Palladium attachment process

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-203」)를 준비하였다. 이 수지 입자를 에칭하고, 수세하였다. 이어서, 팔라듐 촉매를 8중량％ 포함하는 팔라듐 촉매화 액 100mL 중에 수지 입자를 첨가하고, 교반하였다. 그 후, 여과하고, 세정하였다. pH6의 0.5중량％ 디메틸아민보란 액에 수지 입자를 첨가하여, 팔라듐이 부착된 수지 입자를 얻었다.Divinylbenzene resin particles having a particle diameter of 3.0 µm ("Micropearl SP-203" manufactured by Sekisui Chemical Co., Ltd.) were prepared. The resin particles were etched and washed with water. Subsequently, resin particles were added to 100 mL of the palladium catalyzed liquid containing 8% by weight of the palladium catalyst, and stirred. After that, it was filtered and washed. Resin particles were added to a 0.5 wt% dimethylamine borane solution at pH 6 to obtain resin particles with palladium attached thereto.

(2) 도전재 부착 공정(2) Conductive material attachment process

팔라듐이 부착된 수지 입자를 이온 교환수 400mL 중에서 3분간 교반하고, 분산시켜, 분산액을 얻었다. 이어서, 탄화텅스텐 입자(평균 입자 직경 100nm)를 5중량％ 포함하는 슬러리 400g을, 얻어진 분산액에 3분간 걸쳐 첨가하여, 도전재가 부착된 수지 입자를 포함하는 현탁액을 얻었다.The resin particles with palladium were stirred in 400 mL of ion-exchanged water for 3 minutes and dispersed to obtain a dispersion. Subsequently, 400 g of a slurry containing 5 wt% of tungsten carbide particles (average particle diameter of 100 nm) was added to the obtained dispersion solution over 3 minutes to obtain a suspension containing resin particles with a conductive material.

(3) 무전해 니켈 도금 공정(3) Electroless nickel plating process

황산니켈 0.23mol/L, 디메틸아민보란 0.92mol/L, 시트르산나트륨 0.5mol/L 및 텅스텐산 나트륨 0.01mol/L을 포함하는 니켈 도금액(pH8.5)을 준비하였다.A nickel plating solution (pH 8.5) containing 0.23 mol / L nickel sulfate, 0.92 mol / L dimethylamine borane, 0.5 mol / L sodium citrate, and 0.01 mol / L sodium tungstate was prepared.

얻어진 현탁액을 60℃에서 교반하면서, 상기 니켈 도금액을 현탁액에 서서히 적하하고, 무전해 니켈 도금을 행하였다. 그 후, 현탁액을 여과함으로써, 입자를 취출하고, 수세하고, 건조함으로써, 수지 입자의 표면에 니켈-텅스텐-붕소 도전층(두께 약 0.1㎛)이 설치된 도전성 입자를 얻었다.While stirring the obtained suspension at 60 ° C, the nickel plating solution was slowly added dropwise to the suspension, and electroless nickel plating was performed. Thereafter, the particles were taken out by filtration of the suspension, washed with water, and dried to obtain conductive particles in which a nickel-tungsten-boron conductive layer (about 0.1 µm thick) was provided on the surface of the resin particles.

(참고예 1)(Reference Example 1)

탄화텅스텐 입자(평균 입자 직경 100nm)를 니켈 입자(평균 입자 직경 100nm)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1 except that the tungsten carbide particles (average particle diameter 100 nm) were changed to nickel particles (average particle diameter 100 nm).

(비교예 1)(Comparative Example 1)

탄화텅스텐 입자(평균 입자 직경 100nm)를 구리 입자(평균 입자 직경 100nm)로 변경한 것 이외에는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1 except that the tungsten carbide particles (average particle diameter 100 nm) were changed to copper particles (average particle diameter 100 nm).

(비교예 2)(Comparative Example 2)

탄화텅스텐 입자(평균 입자 직경 100nm)를 실리카 입자(평균 입자 직경 100nm)로 변경한 것 이외는 실시예 1과 동일하게 하여, 도전성 입자를 얻었다.Conductive particles were obtained in the same manner as in Example 1 except that the tungsten carbide particles (average particle diameter 100 nm) were changed to silica particles (average particle diameter 100 nm).

(실시예 17)(Example 17)

(1) 팔라듐 부착 공정(1) Palladium attachment process

입자 직경이 3.0㎛인 디비닐벤젠 수지 입자(세끼스이 가가꾸 고교사 제조 「마이크로펄 SP-203」)를 준비하였다. 이 수지 입자를 에칭하고, 수세하였다. 이어서, 팔라듐 촉매를 8중량％ 포함하는 팔라듐 촉매화 액 100mL 중에 수지 입자를 첨가하고, 교반하였다. 그 후, 여과하고, 세정하였다. pH6의 0.5중량％ 디메틸아민보란 액에 수지 입자를 첨가하고, 팔라듐이 부착된 수지 입자를 얻었다.Divinylbenzene resin particles having a particle diameter of 3.0 µm ("Micropearl SP-203" manufactured by Sekisui Chemical Co., Ltd.) were prepared. The resin particles were etched and washed with water. Subsequently, resin particles were added to 100 mL of the palladium catalyzed liquid containing 8% by weight of the palladium catalyst, and stirred. After that, it was filtered and washed. Resin particles were added to a 0.5 wt% dimethylamine borane solution at pH 6 to obtain resin particles with palladium attached thereto.

(2) 도전재 부착 공정(2) Conductive material attachment process

팔라듐이 부착된 수지 입자를 이온 교환수 400mL 중에서 3분간 교반하고, 분산시켜, 분산액을 얻었다. 이어서, 탄화텅스텐 입자(평균 입자 직경 100nm)를 5중량％ 포함하는 슬러리 400g을, 얻어진 분산액에 3분간 걸쳐 첨가하고, 도전재가 부착된 수지 입자를 포함하는 현탁액을 얻었다.The resin particles with palladium were stirred in 400 mL of ion-exchanged water for 3 minutes and dispersed to obtain a dispersion. Subsequently, 400 g of a slurry containing 5 wt% of tungsten carbide particles (average particle diameter of 100 nm) was added to the obtained dispersion solution over 3 minutes to obtain a suspension containing resin particles with a conductive material.

(3) 무전해 구리 도금 공정(3) Electroless copper plating process

황산구리 0.23mol/L, 에틸렌디아민사아세트산염 2.3mol/L, 포르말린 0.5mol/L을 포함하는 구리 도금액(pH12.5)을 준비하였다. 얻어진 현탁액을 60℃에서 교반하면서, 상기 구리 도금액을 현탁액에 서서히 적하하고, 무전해 구리 도금을 행하였다. 그 후, 현탁액을 여과함으로써, 입자를 취출하고, 수세하고, 건조함으로써, 수지 입자의 표면 상에 구리 도전층(두께 0.1㎛)이 배치된 도전성 입자를 얻었다.A copper plating solution (pH12.5) containing 0.23 mol / L copper sulfate, 2.3 mol / L ethylenediamine tetraacetate, and 0.5 mol / L formalin was prepared. While stirring the obtained suspension at 60 ° C, the copper plating solution was slowly added dropwise to the suspension, and electroless copper plating was performed. Thereafter, the particles were taken out by filtration of the suspension, washed with water, and dried to obtain conductive particles in which a copper conductive layer (0.1 µm thick) was disposed on the surface of the resin particles.

(평가)(evaluation)

(1) 접속 저항(1) Connection resistance

접속 구조체의 제작:Construction of the connection structure:

비스페놀 A형 에폭시 수지(미쯔비시 가가꾸사 제조 「에피코트 1009」) 10중량부와, 아크릴 고무(중량 평균 분자량 약 80만) 40중량부와, 메틸에틸케톤 200중량부와, 마이크로 캡슐형 경화제(아사히 가세이 케미컬즈사 제조 「HX3941HP」) 50중량부와, 실란 커플링제(도레이 다우코닝 실리콘사 제조 「SH6040」) 2중량부를 혼합하고, 도전성 입자를 함유량이 3중량％가 되도록 첨가하고, 분산시켜, 수지 조성물을 얻었다.10 parts by weight of bisphenol A type epoxy resin ("Epitcoat 1009" manufactured by Mitsubishi Chemical Corporation), 40 parts by weight of acrylic rubber (about 800,000 by weight average molecular weight), 200 parts by weight of methyl ethyl ketone, and microcapsule curing agent ( 50 parts by weight of Asahi Kasei Chemicals (`` HX3941HP '') and 2 parts by weight of a silane coupling agent (`` SH6040 '' manufactured by Toray Dow Corning Silicone) were mixed, and the conductive particles were added to a content of 3% by weight and dispersed. A resin composition was obtained.

얻어진 수지 조성물을, 편면이 이형 처리된 두께 50㎛의 PET(폴리에틸렌테레프탈레이트) 필름에 도포하고, 70℃의 열풍에서 5분간 건조하여, 이방성 도전 필름을 제작하였다. 얻어진 이방성 도전 필름의 두께는 12㎛였다.The obtained resin composition was coated on a PET (polyethylene terephthalate) film having a thickness of 50 μm on one side and subjected to a release treatment, and dried in a hot air at 70 ° C. for 5 minutes to prepare an anisotropic conductive film. The thickness of the obtained anisotropic conductive film was 12 µm.

얻어진 이방성 도전 필름을 5mm×5mm의 크기로 절단하였다. 절단된 이방성 도전 필름을, 한쪽에 저항 측정용의 배선 선을 갖는 알루미늄 전극(높이 0.2㎛, L/S=20㎛/20㎛)을 갖는 유리 기판(폭 3cm, 길이 3cm)의 알루미늄 전극측의 거의 중앙에 부착하였다. 계속해서, 동일한 알루미늄 전극을 갖는 2층 플렉시블 프린트 기판(폭 2cm, 길이 1cm)을 전극끼리가 겹치도록 위치 정렬을 하고 나서 접합하였다. 이 유리 기판과 2층 플렉시블 프린트 기판과의 적층체를 10N, 180℃, 및 20초 간의 압착 조건에서 열 압착하고, 접속 구조체를 얻었다. 또한, 폴리이미드 필름에 알루미늄 전극이 직접 형성되어 있는 2층 플렉시블 프린트 기판을 사용하였다.The obtained anisotropic conductive film was cut to a size of 5 mm × 5 mm. The cut anisotropic conductive film on the aluminum electrode side of a glass substrate (width 3 cm, length 3 cm) having an aluminum electrode (0.2 µm high, L / S = 20 µm / 20 µm high) having a wiring line for measuring resistance on one side. It was almost centered. Subsequently, a two-layer flexible printed board (2 cm in width and 1 cm in length) having the same aluminum electrode was subjected to position alignment so that the electrodes overlapped and then joined. The laminated body of this glass substrate and a two-layer flexible printed circuit board was thermocompressed under 10N, 180 degreeC, and 20 second compression conditions, and the connection structure was obtained. In addition, a two-layer flexible printed board in which aluminum electrodes were directly formed on the polyimide film was used.

접속 저항의 측정:Measurement of connection resistance:

얻어진 접속 구조체가 대향하는 전극 간의 접속 저항을 4 단자법에 의해 측정하였다. 또한, 접속 저항을 다음의 기준으로 판정하였다.The connection resistance between the electrodes facing the obtained connection structure was measured by a four-terminal method. In addition, connection resistance was judged by the following criteria.

[접속 저항의 평가 기준][Evaluation criteria for connection resistance]

○○: 참고예 1의 도전성 입자를 사용한 경우의 접속 저항의 90％ 미만○○: less than 90% of the connection resistance when the conductive particles of Reference Example 1 were used

○: 참고예 1의 도전성 입자를 사용한 경우의 접속 저항의 90％ 이상, 95％ 미만○: 90% or more and less than 95% of the connection resistance when the conductive particles of Reference Example 1 were used.

△: 참고예 1의 도전성 입자를 사용한 경우의 접속 저항의 95％ 이상, 105％ 미만Δ: 95% or more and less than 105% of the connection resistance when the conductive particles of Reference Example 1 were used.

×: 참고예 1의 도전성 입자를 사용한 경우의 접속 저항의 105％ 이상×: 105% or more of the connection resistance when the conductive particles of Reference Example 1 were used

결과를 다음의 표 1, 2에 나타내었다.The results are shown in Tables 1 and 2 below.

Figure 112014114395923-pct00002
Figure 112014114395923-pct00002

Figure 112014114395923-pct00003
Figure 112014114395923-pct00003

1…도전성 입자
1a…돌기
2…기재 입자
3…도전층
3a…돌기
4…도전재
5…절연성 물질
11…도전성 입자
11a…돌기
12…제1 도전층
13…제2 도전층
13a…돌기
21…도전성 입자
22…도전층
51…접속 구조체
52…제1 접속 대상 부재
52a…제1 전극
53…제2 접속 대상 부재
53a…제2 전극
54…접속부One… Conductive particles
1a… spin
2… Substrate particles
3… Conductive layer
3a… spin
4… Conductive material
5… Insulating material
11… Conductive particles
11a… spin
12… 1st conductive layer
13… 2nd conductive layer
13a… spin
21… Conductive particles
22… Conductive layer
51… Connection structure
52… First connection target member
52a ... First electrode
53… Second connection target member
53a ... Second electrode
54… Connection

Claims (12)

기재 입자와,
상기 기재 입자의 표면 상에 배치된 도전층과,
상기 기재 입자의 표면 상의 일부의 영역에 배치된 도전재를 구비하고,
상기 도전재가 상기 도전층 내에 매입(
Figure 112019116755009-pct00009
)되어 있고,
상기 도전재의 재질이 니켈보다도 모스 경도가 높은 재질인 도전성 입자.Substrate particles,
A conductive layer disposed on the surface of the substrate particle,
It is provided with a conductive material disposed in a part of the area on the surface of the substrate particles,
The conductive material is embedded in the conductive layer (
Figure 112019116755009-pct00009
),
The conductive material is a material having a higher Mohs hardness than nickel. 제1항에 있어서,
상기 도전재의 재질이 몰리브덴, 탄화텅스텐, 텅스텐, 탄화티타늄 또는 탄화탄탈인 도전성 입자.According to claim 1,
The conductive material is made of molybdenum, tungsten carbide, tungsten, titanium carbide or tantalum carbide. 제1항 또는 제2항에 있어서, 복수의 상기 도전재를 구비하는 도전성 입자.The conductive particles according to claim 1 or 2, comprising a plurality of the conductive materials. 제1항 또는 제2항에 있어서, 상기 도전층이 외측의 표면에 돌기를 갖고, 상기 도전층의 상기 돌기의 내측에 상기 도전재가 배치되어 있는 도전성 입자.The conductive particle according to claim 1 or 2, wherein the conductive layer has a projection on an outer surface, and the conductive material is disposed inside the projection of the conductive layer. 제1항 또는 제2항에 있어서, 상기 도전층이 니켈층을 갖는 도전성 입자.The conductive particle according to claim 1 or 2, wherein the conductive layer has a nickel layer. 제1항 또는 제2항에 있어서, 상기 도전층이 상기 기재 입자측에 니켈층과, 상기 기재 입자측과는 반대측에 팔라듐층을 갖는 도전성 입자.The conductive particle according to claim 1 or 2, wherein the conductive layer has a nickel layer on the substrate particle side and a palladium layer on the opposite side to the substrate particle side. 제1항 또는 제2항에 있어서, 상기 도전층의 표면에 부착되어 있는 절연성 물질을 더 구비하는 도전성 입자.The conductive particle according to claim 1 or 2, further comprising an insulating material attached to the surface of the conductive layer. 제1항 또는 제2항에 있어서, 상기 도전재가 입자인 도전성 입자.The conductive particle according to claim 1 or 2, wherein the conductive material is a particle. 제1항 또는 제2항에 있어서,
상기 도전재의 재질이 몰리브덴, 탄화텅스텐, 텅스텐 또는 탄화탄탈인 도전성 입자.The method according to claim 1 or 2,
The conductive material is made of molybdenum, tungsten carbide, tungsten or tantalum carbide. 제1항 또는 제2항에 기재된 도전성 입자와 결합제 수지를 포함하는 도전 재료.A conductive material comprising the conductive particles according to claim 1 or 2 and a binder resin. 제1 전극을 표면에 갖는 제1 접속 대상 부재와,
제2 전극을 표면에 갖는 제2 접속 대상 부재와,
상기 제1 접속 대상 부재와 상기 제2 접속 대상 부재를 접속하고 있는 접속부를 구비하고,
상기 접속부가 제1항 또는 제2항에 기재된 도전성 입자에 의해 형성되어 있거나, 또는 상기 도전성 입자와 결합제 수지를 포함하는 도전 재료에 의해 형성되어 있고,
상기 제1 전극과 상기 제2 전극이 상기 도전성 입자에 의해 전기적으로 접속되어 있는 접속 구조체.A first connection target member having a first electrode on its surface,
A second connection target member having a second electrode on its surface,
And a connecting portion connecting the first connection target member and the second connection target member,
The connection portion is formed of the conductive particles according to claim 1 or 2, or is formed of a conductive material containing the conductive particles and a binder resin,
A connecting structure in which the first electrode and the second electrode are electrically connected by the conductive particles. 삭제delete
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