WO2016068165A1 - 導電材料 - Google Patents
導電材料 Download PDFInfo
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- WO2016068165A1 WO2016068165A1 PCT/JP2015/080327 JP2015080327W WO2016068165A1 WO 2016068165 A1 WO2016068165 A1 WO 2016068165A1 JP 2015080327 W JP2015080327 W JP 2015080327W WO 2016068165 A1 WO2016068165 A1 WO 2016068165A1
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
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- C23C18/1655—Process features
- C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—Multistep pretreatment
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C23C18/48—Coating with alloys
- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
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- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R11/00—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts
- H01R11/01—Individual connecting elements providing two or more spaced connecting locations for conductive members which are, or may be, thereby interconnected, e.g. end pieces for wires or cables supported by the wire or cable and having means for facilitating electrical connection to some other wire, terminal, or conductive member, blocks of binding posts characterised by the form or arrangement of the conductive interconnection between the connecting locations
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- H01R4/00—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation
- H01R4/10—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation effected solely by twisting, wrapping, bending, crimping, or other permanent deformation
- H01R4/18—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation effected solely by twisting, wrapping, bending, crimping, or other permanent deformation by crimping
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- H01R4/10—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation effected solely by twisting, wrapping, bending, crimping, or other permanent deformation
- H01R4/18—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation effected solely by twisting, wrapping, bending, crimping, or other permanent deformation by crimping
- H01R4/188—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation effected solely by twisting, wrapping, bending, crimping, or other permanent deformation by crimping having an uneven wire-receiving surface to improve the contact
Definitions
- the thickness of the conductive layer 30 is preferably 50 nm or more and 250 nm or less, more preferably 80 nm or more and 150 nm or less. If the thickness of the conductive layer 30 is too small, it will be difficult to function as conductive particles, and if the thickness is too large, the height of the protrusion 30a will be lost.
- FIG. 3 is a cross-sectional view schematically showing a third configuration example of the conductive particles.
- a plurality of conductive particles of the third configuration example are attached to the surface of the resin core particle 10, the first conductive layer 33 covering the surface of the resin core particle 10, and the first conductive layer 33.
- Insulating particles 20 serving as a core material, and a first conductive layer 33 and a second conductive layer 34 covering the surfaces of the insulating particles 20 are provided. That is, in the third configuration example, the insulating particles 20 are attached to the surface of the first conductive layer 33, and the second conductive layer 34 is further formed. Thereby, it is possible to prevent the insulating particles 20 from biting into the resin core particles 10 during pressure bonding, and the protrusions can easily break through the oxide layer on the electrode surface.
- the thickness of the first conductive layer 33 is preferably 10 nm to 200 nm, more preferably 50 nm to 150 nm. If the thickness is too large, the effect of elasticity of the resin core particle 10 is reduced, and the conduction reliability is lowered.
- a stress relaxation agent examples include a hydrogenated styrene-butadiene block copolymer and a hydrogenated styrene-isoprene block copolymer.
- the silane coupling agent examples include epoxy, methacryloxy, amino, vinyl, mercapto sulfide, and ureido.
- the inorganic filler examples include silica, talc, titanium oxide, calcium carbonate, magnesium oxide and the like.
- connection structure As shown in Table 1, using the anisotropic conductive film to which the conductive particles are added, a TiO 2 / Al coated glass substrate and an IC are pressure-bonded under a pressure bonding condition of 190 ° C.-60 MPa-5 sec to obtain a connection structure. Got. The initial resistance value of the connection structure was 0.3 ⁇ , the resistance value after the reliability test was 0.5 ⁇ , the occurrence rate of wiring cracks was 0%, and the overall judgment was OK.
- ⁇ Comparative example 2> As shown in Table 1, using an anisotropic conductive film to which the same conductive particles as in Comparative Example 1 were added, a TiO 2 / Al coated PET substrate and an IC were bonded under pressure bonding conditions of 190 ° C.-60 MPa-5 sec. As a result, a connection structure was obtained. The initial resistance value of the connection structure was 3.0 ⁇ , the resistance value after the reliability test was 6.0 ⁇ , the occurrence rate of wiring cracks was 0%, and the overall judgment was NG.
Abstract
Description
1.導電性粒子
2.導電材料
3.接続構造体の製造方法
4.実施例
本実施の形態に係る導電性粒子は、樹脂コア粒子と、樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、樹脂コア粒子及び前記絶縁性粒子の表面に配置される導電層とを備え、絶縁性粒子のモース硬度が、7より大きいものである。これにより、導電性粒子が電極表面の酸化物層を突き破って十分に食い込み、優れた導通信頼性が得られる。特に、被着体である回路部材が、PET(Poly Ethylene Terephthalate)基板などの低弾性率のプラスチック基板である場合、圧着時の圧力を高くすることなく、基材変形の影響を軽減して低抵抗を実現できるため、非常に有効である。
図1は、導電性粒子の第1の構成例の概略を示す断面図である。第1の構成例の導電性粒子は、樹脂コア粒子10と、樹脂コア粒子10の表面に複数付着され、突起30aの芯材となる絶縁性粒子20と、樹脂コア粒子10及び絶縁性粒子20を被覆する導電層30とを備える。
K値(N/mm2)=(3/21/2)・F・S-3/2・R-1/2
F:導電性粒子が20%圧縮変形したときの荷重値(N)
S:導電性粒子が20%圧縮変形したときの圧縮変位(mm)
R:導電性粒子の半径(mm)
図2は、導電性粒子の第2の構成例の概略を示す断面図である。第2の構成例の導電性粒子は、樹脂コア粒子10と、樹脂コア粒子10の表面に複数付着され、突起32aの芯材となる絶縁性粒子20と、樹脂コア粒子10及び絶縁性粒子20の表面を被覆する第1の導電層31と、導電層31を被覆する第2の導電層32とを備える。すなわち、第2の構成例は、第1の構成例の導電層30を2層構造としたものである。導電層を2層構造とすることにより、最外殻を構成する第2の導電層32の密着性を向上させ、導通抵抗を低下させることができる。
図3は、導電性粒子の第3の構成例の概略を示す断面図である。第3の構成例の導電性粒子は、樹脂コア粒子10と、樹脂コア粒子10の表面を被覆する第1の導電層33と、第1の導電層33の表面に複数付着され、突起34aの芯材となる絶縁性粒子20と、第1の導電層33及び絶縁性粒子20の表面を被覆する第2の導電層34とを備える。すなわち、第3の構成例は、第1の導電層33の表面に絶縁性粒子20を付着させ、さらに第2の導電層34を形成したものである。これにより、圧着時に絶縁性粒子20が樹脂コア粒子10に食い込むのを防止し、突起が電極表面の酸化物層を容易に突き破ることができる。
本実施の形態に係る導電材料は、樹脂コア粒子と、樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、樹脂コア粒子及び絶縁性粒子の表面に配置される導電層とを備え、絶縁性粒子のモース硬度が、7より大きい導電性粒子を含有する。導電材料としては、フィルム状、ペースト状などの形状が挙げられ、例えば、異方性導電フィルム(ACF:Anisotropic Conductive Film)、異方性導電ペースト(ACP:Anisotropic Conductive Paste)などが挙げられる。また、導電材料の硬化型としては、熱硬化型、光硬化型、光熱併用硬化型などが挙げられる。
本実施の形態に係る接続構造体の製造方法は、樹脂コア粒子と、樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、樹脂コア粒子及び絶縁性粒子の表面に配置される導電層とを備え、絶縁性粒子のモース硬度が、7より大きい導電性粒子を含有する導電材料を介して、第1の回路部材の端子と第2の回路部材の端子とを圧着する。これにより前述の導電性粒子により第1の回路部材の端子と第2の回路部材の端子とが接続されてなる接続構造体を得ることができる。
以下、本発明の実施例について説明する。本実施例では、突起を有する導電性粒子を作製し、これを含有する異方性導電フィルムを用いて接続構造体を作製した。そして、接続構造体の導通抵抗、及び配線クラックの発生率について評価した。なお、本発明はこれらの実施例に限定されるものではない。
ACF層とNCF層とが積層された2層構造の異方性導電フィルムを作製した。先ず、フェノキシ樹脂(YP50、新日鐵化学(株))20質量部、液状エポキシ樹脂(EP828、三菱化学(株))30質量部、固形エポキシ樹脂(YD-014、新日鐵化学(株))10質量部、マイクロカプセル型潜在性硬化剤(ノバキュア3941H、旭化成イーマテリアルズ)30質量部、導電性粒子10質量部を配合して、厚み6μmのACF層を得た。次に、フェノキシ樹脂(YP50、新日鐵化学(株))20質量部、液状エポキシ樹脂(EP828、三菱化学(株))30質量部、固形エポキシ樹脂(YD-014、新日鐵化学(株))10質量部、マイクロカプセル型潜在性硬化剤(ノバキュア3941H、旭化成イーマテリアルズ)30質量部を配合して、厚み12μmのNCF層を得た。そして、ACF層とNCF層とを貼り合わせて、厚み18μmの2層構造の異方性導電フィルムを得た。
評価基材として、TiO2/Alコーティングガラス基板(0.3mmt、TiO2厚み:50nm、Al厚み:300nm)、TiO2/AlコーティングPET(Poly Ethylene Terephthalate)基板(0.3mmt、TiO2厚み:50nm、Al厚み:300nm)、及び、IC(1.8mm×20mm、T:0.3mm、Au-plated bump:30μm×85μm、h=15μm)を準備した。また、圧着条件は、190℃-60MPa-5sec、又は190℃-100MPa-5secとした。
デジタルマルチメーター(商品名:デジタルマルチメーター7561、横河電機社製)を用いて、初期の接続構造体の導通抵抗(Ω)の測定を行った。また、接続構造体を、85℃、85%RHの高温高湿環境下に500h放置して信頼性試験を行った後、接続構造体の導通抵抗(Ω)の測定を行った。
接続構造体の基板側の配線の任意の20箇所を金属顕微鏡にて観察し、配線クラックをカウントして発生率を算出した。
初期の導通抵抗と信頼性試験後の導通抵抗との差が0.3Ω以下、且つ配線クラックの発生率が0%の場合を「OK」を評価し、それ以外を「NG」と評価した。
樹脂コア粒子として、次のようにジビニルベンゼン系樹脂粒子を作製した。ジビニルベンゼン、スチレン、ブチルメタクリレートの混合比を調整した溶液に重合開始剤としてベンゾイルパーオキサイドを投入して高速で均一攪拌しながら加熱を行い、重合反応を行うことにより微粒子分散液を得た。微粒子分散液をろ過し、減圧乾燥することにより微粒子の凝集体であるブロック体を得た。そして、ブロック体を粉砕することにより、平均粒子径3.0μmのジビニルベンゼン系樹脂粒子を得た。この樹脂コア粒子の20%圧縮されたときの圧縮弾性率(20%K値)は、12000N/mm2であった。
表1に示すように、実施例1と同一の導電性粒子を添加した異方性導電フィルムを用いて、TiO2/AlコーティングPET基板とICとを190℃-60MPa-5secの圧着条件で圧着し、接続構造体を得た。接続構造体の初期の抵抗値は0.7Ω、信頼性試験後の抵抗値は1.0Ω、配線クラックの発生率は0%であり、総合判定はOKであった。
導電層用のメッキ液として、硫酸ニッケル0.23mol/L、ジメチルアミンボラン0.25mol/L、クエン酸ナトリウム0.5mol/L及びタングステン酸ナトリウム0.35mol/Lを含むNi-W-Bめっき液(pH8.5)を使用した。これ以外は、実施例1と同様にして、アルミナで形成された突起と、Ni-W-Bメッキの導電層とを有する導電性粒子を得た。この導電性粒子を金属顕微鏡にて観察したところ、平均粒子径は3~4μmであり、粒子1個当たりの突起の数は約70であり、また、導電層の厚みは約100nmであった。
表1に示すように、実施例3と同一の導電性粒子を添加した異方性導電フィルムを用いて、TiO2/AlコーティングPET基板とICとを190℃-60MPa-5secの圧着条件で圧着し、接続構造体を得た。接続構造体の初期の抵抗値は0.6Ω、信頼性試験後の抵抗値は0.8Ω、配線クラックの発生率は0%であり、総合判定はOKであった。
絶縁性粒子として、平均粒子径が150nmであるシリカ(SiO2)を使用した。これ以外は、実施例1と同様にして、シリカで形成された突起と、Ni-Bメッキの導電層とを有する導電性粒子を得た。この導電性粒子を金属顕微鏡にて観察したところ、平均粒子径は3~4μmであり、粒子1個当たりの突起の数は約70であり、また、導電層の厚みは約100nmであった。
表1に示すように、比較例1と同一の導電性粒子を添加した異方性導電フィルムを用いて、TiO2/AlコーティングPET基板とICとを190℃-60MPa-5secの圧着条件で圧着し、接続構造体を得た。接続構造体の初期の抵抗値は3.0Ω、信頼性試験後の抵抗値は6.0Ω、配線クラックの発生率は0%であり、総合判定はNGであった。
絶縁性粒子として、平均粒子径が150nmであるシリカ(SiO2)を使用した。また、導電層用のメッキ液として、硫酸ニッケル0.23mol/L、ジメチルアミンボラン0.25mol/L、クエン酸ナトリウム0.5mol/L及びタングステン酸ナトリウム0.35mol/Lを含むNi-W-Bめっき液(pH8.5)を使用した。これ以外は、実施例1と同様にして、シリカで形成された突起と、Ni-W-Bメッキの導電層とを有する導電性粒子を得た。この導電性粒子を走査型電子顕微鏡(SEM)にて観察したところ、平均粒子径は3~4μmであり、粒子1個当たりの突起の数は約70であり、また、導電層の厚みは約100nmであった。
表1に示すように、比較例3と同一の導電性粒子を添加した異方性導電フィルムを用いて、TiO2/AlコーティングPET基板とICとを190℃-60MPa-5secの圧着条件で圧着し、接続構造体を得た。接続構造体の初期の抵抗値は1.8Ω、信頼性試験後の抵抗値は3.6Ω、配線クラックの発生率は0%であり、総合判定はNGであった。
表1に示すように、比較例3と同一の導電性粒子を添加した異方性導電フィルムを用いて、TiO2/AlコーティングPET基板とICとを190℃-100MPa-5secの圧着条件で圧着し、接続構造体を得た。接続構造体の初期の抵抗値は0.7Ω、信頼性試験後の抵抗値は1.0Ω、配線クラックの発生率は25%であり、総合判定はNGであった。
Claims (8)
- 樹脂コア粒子と、前記樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、前記樹脂コア粒子及び前記絶縁性粒子の表面に配置される導電層とを備え、前記絶縁性粒子のモース硬度が、7より大きい導電性粒子を含有する導電材料。
- 前記導電性粒子の導電層が、ニッケル又はニッケル合金である請求項1記載の導電材料。
- 前記導電性粒子の絶縁性粒子が、ジルコニア、アルミナ、炭化タングステン、及びダイヤモンドの内の少なくとも1種以上である請求項1又は2記載の導電材料。
- 前記導電性粒子の絶縁性粒子の平均粒子径が、50~250nmであり、
前記導電性粒子の樹脂コア粒子の表面に形成された突起の個数が、1~500である請求項1~3のいずれか1項に記載の導電材料。 - 前記導電性粒子の樹脂コア粒子の20%圧縮されたときの圧縮弾性率が、500~20000N/mm2である請求項1~4のいずれか1項に記載の導電材料。
- プラスチック基板上の酸化物層が設けられた端子を接続する請求項1~5のいずれか1項に記載の導電材料。
- 樹脂コア粒子と、前記樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、前記樹脂コア粒子及び前記絶縁性粒子の表面に配置される導電層とを備え、前記絶縁性粒子のモース硬度が、7より大きい導電性粒子により第1の回路部材の端子と第2の回路部材の端子とが接続されてなる接続構造体。
- 樹脂コア粒子と、前記樹脂コア粒子の表面に複数配置され、突起を形成する絶縁性粒子と、前記樹脂コア粒子及び前記絶縁性粒子の表面に配置される導電層とを備え、前記絶縁性粒子のモース硬度が、7より大きい導電性粒子を含有する導電材料を介して、第1の回路部材の端子と第2の回路部材の端子とを圧着する接続構造体の製造方法。
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JP2013149611A (ja) * | 2011-12-22 | 2013-08-01 | Sekisui Chem Co Ltd | 導電性粒子、導電材料及び接続構造体 |
JP2015057757A (ja) * | 2013-08-09 | 2015-03-26 | 積水化学工業株式会社 | 導電性粒子、導電材料及び接続構造体 |
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CN112863732A (zh) | 2021-05-28 |
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KR102545861B1 (ko) | 2023-06-21 |
KR20220068267A (ko) | 2022-05-25 |
CN112863732B (zh) | 2023-01-17 |
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