JP7363918B2 - 異方性導電材料 - Google Patents
異方性導電材料 Download PDFInfo
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- JP7363918B2 JP7363918B2 JP2021558357A JP2021558357A JP7363918B2 JP 7363918 B2 JP7363918 B2 JP 7363918B2 JP 2021558357 A JP2021558357 A JP 2021558357A JP 2021558357 A JP2021558357 A JP 2021558357A JP 7363918 B2 JP7363918 B2 JP 7363918B2
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- Prior art keywords
- acid
- anisotropic conductive
- alloy
- conductive material
- electrodes
- Prior art date
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- 239000000956 alloy Substances 0.000 claims description 40
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- 239000011347 resin Substances 0.000 claims description 28
- 238000002844 melting Methods 0.000 claims description 22
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- 239000002184 metal Substances 0.000 claims description 22
- 229920001187 thermosetting polymer Polymers 0.000 claims description 22
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- 230000008018 melting Effects 0.000 claims description 20
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000002723 alicyclic group Chemical group 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 229910052785 arsenic Inorganic materials 0.000 description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 4
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 description 3
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 3
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 3
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LCFVJGUPQDGYKZ-UHFFFAOYSA-N Bisphenol A diglycidyl ether Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C(C=C1)=CC=C1OCC1CO1 LCFVJGUPQDGYKZ-UHFFFAOYSA-N 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 229910020888 Sn-Cu Inorganic materials 0.000 description 3
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000008064 anhydrides Chemical class 0.000 description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 3
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 238000011156 evaluation Methods 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- IWYDHOAUDWTVEP-UHFFFAOYSA-N mandelic acid Chemical compound OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 description 3
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 3
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- 235000005074 zinc chloride Nutrition 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- MHVJRKBZMUDEEV-UHFFFAOYSA-N (-)-ent-pimara-8(14),15-dien-19-oic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(C=C)(C)C=C1CC2 MHVJRKBZMUDEEV-UHFFFAOYSA-N 0.000 description 2
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 description 2
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 description 2
- VOJUXHHACRXLTD-UHFFFAOYSA-N 1,4-dihydroxy-2-naphthoic acid Chemical compound C1=CC=CC2=C(O)C(C(=O)O)=CC(O)=C21 VOJUXHHACRXLTD-UHFFFAOYSA-N 0.000 description 2
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 description 2
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Images
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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
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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
- H01B1/20—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
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- H—ELECTRICITY
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- 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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Description
1. 熱硬化性樹脂と、重合開始剤と、導電性粒子とを含み、
上記導電性粒子が、導電性コアと、該導電性コアを被覆する絶縁膜とを有し、該導電性コアが、60~250℃の融点を有し、かつ、その融点以下の温度で液体状態である過冷却金属で形成されていることを特徴とする異方性導電材料。
2. 上記導電性コアが、In-Bi-Sn系合金、Bi-Sn系合金またはSn-Ag-Cu系合金を含む1の異方性導電材料。
3. 上記熱硬化性樹脂が、エポキシ樹脂、フェノール樹脂から選ばれる1種または2種である1または2の異方性導電材料。
4. 上記重合開始剤が、アニオン重合開始剤またはカチオン重合開始剤である請求項1~3のいずれかの異方性導電材料。
5. 1~4のいずれかの異方性導電材料から得られる異方性導電層。
6. 5の異方性導電層を有する電子素子。
エポキシ樹脂としては、特に制限されないが、分子内にエポキシ基を平均で2個以上有する化合物であることが好ましい。
本発明において、「過冷却」とは、物質が液体から固体に変わる温度(融点)以下の温度でも液体のままでいる状態を意味する。この過冷却状態は、示差走査熱量測定により、所定の温度領域にて昇温・降温を繰り返した際の発熱ピークおよび吸熱ピークを観測することにより確認することができる(例えば、図1を参照)。
塗布の際、異方性導電材料の粘度と表面張力、所望する薄膜の厚さ等を考慮し、ディスペンサー法、印刷法(凸版、凹版、平版、スクリーン印刷等)、インクジェット法、ドロップキャスト法、スピンコート法、ブレードコート法、ディップコート法、ロールコート法、バーコート法、ダイコート法、スリットコート法、スプレーコート法およびカーテンコート法等の各種ウェットプロセス法の中から最適なものを採用すればよい。
装置:Perkin Elmer社製 Diamond DSC
測定条件:窒素雰囲気下
昇温速度:20℃/分(-65~100℃)
(2)自転・公転ミキサー
装置:(株)シンキー製 泡とり錬太郎 ARE-310
(3)走査電子顕微鏡(SEM)
装置:サーモフィッシャーサイエンティフィック(株)製 Helios G3
(4)異方性導電材料の塗布
装置:マイクロ-テック(株)製 高精度スクリーン印刷機 MT-320T
Liq.62:In-Bi-Snをコア部として過冷却させたコア-シェル粒子(80質量%酢酸エチル分散体)[SAFI-Tech, Inc.製、Liquital(登録商標)62]
Liq.139:Bi-Snをコア部として過冷却させたコア-シェル粒子[SAFI-Tech, Inc.製、Liquital(登録商標)139]
Field’s metal:(In51質量%、Bi32.5質量%、Sn16.5質量%よりなる合金) [Alfa Aesar製]
EPN:フェノールノボラック型エポキシ樹脂[三菱ケミカル(株)製、jER(登録商標)-152]
ECA:脂環式エポキシ樹脂[(株)ダイセル製、エポリード GT401]
TEPeIC:トリス(4,5-エポキシペンチル)イソシアヌレート[日産化学(株)製、TEPIC(登録商標)-VL]
TEOIC:トリス(7,8-エポキシオクチル)イソシアヌレート[日産化学(株)製、TEPIC(登録商標)-FL]
SI-100:カチオン重合開始剤[三新化学工業(株)製、サンエイドSI-100]
2EHGE:2-エチルヘキシルグリシジルエーテル
(1)過冷却状態をとる粒子の示差走査熱量測定
風乾したLiq.62を17.3mg測量し、DSCにて-65℃と90℃の温度領域にて昇温・降温を2回繰り返した。得られた示差走査熱量測定のスペクトルを図1に示す。
1回目の昇温では吸熱ピークが観測されたが非常に小さいピークであった。降温では室温以下の温度で凝固の発熱を観測した。2回目の昇温では融点となる吸熱のピークを観測し、降温では室温以下の温度で凝固の発熱を観測した。2回目の昇温にて融点の吸熱ピークが観測されたことは、Liq.62の導電性コアが常温では過冷却状態の液体金属であることを示唆している。この結果は、より低い温度および圧力で導電性コアの流出が可能となることを意味する。
Field’s metalを10.9mg測量し、DSCにて-65℃と90℃の温度領域にて昇温・降温を2回繰り返した。得られた示差走査熱量測定のスペクトルを図2に示す。
Field’s metalでは、1回目および2回目の昇温・降温のいずれにおいても、室温以上で融点・凝固点が観測された。この結果は、Field’s metalが通常の低融点金属であることを示唆しており、電子部品の接続/接着処理時には、この低融点金属を溶解させる温度まで加熱する必要があることを意味する。
(1)導電性粒子の形状
風乾したLiq.62を加速電圧10kVで観察した走査電子顕微鏡写真を図3に示す。画像からは、導電性粒子が数μm程度の球形またはそれと類似した形態を有していることが分かる。
導電性粒子の導電性コアに過冷却状態の液体金属が含まれていることを確認するために、シリコンウエハ上に粒子をローディングし、風乾後、エアブロー(4mm口径、0.4MPa)することで人為的に破壊した。エアブロー後の粒子の状態を加速電圧3kVで観察した走査電子顕微鏡写真を図4に示す。
図4の結果から、導電性粒子が破壊され、過冷却状態のIn-Bi-Snが流れ出た後、固化していることが確認された。これは、流出した過冷却金属が凝固して、金属本来の融点を有する固体状となることを示しており、これにより高い耐熱信頼性が発現可能となると示している。
本発明の異方性導電材料に用いる導電性粒子に関し、破壊のために必要な条件を確認した。
過冷却粒子を含む樹脂配合物
硬化性エポキシ樹脂としてBADGEを100質量部、反応性希釈剤として2EHGEを30質量部、風乾したLIq.62を37質量部配合し、自転・公転ミキサーにて樹脂配合物を調製した。
シリコンウエハ基板上にCu電極を連続的に配置した後、基板上に調製例1で得た樹脂配合物をおよそ100mg垂らし、その上に、上部ガラスを配置した。次いで、3MPaの圧力を印荷しながら80℃に加温し、Cu電極とガラスを圧着させた。ガラス越しにCu電極を顕微鏡観察し、金属光沢の有無を確認した。
参考例2における上部ガラスへの印加圧力を1.5MPaに変更したこと以外は参考例2と同様に操作し評価した。
参考例2における上部ガラスへの印加圧力を0.3MPaに変更したこと以外は参考例2と同様に操作し評価した。結果を表1に併せて示す。
熱硬化性樹脂としてEPNを100質量部、カチオン重合開始剤としてSI-100を1質量部、および導電性粒子としてLiq.62を68質量部(固形分換算量)配合し、エバポレーターにて溶媒を留去し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例1にて調製した異方性導電材料をスクリーン印刷にてガラス基板上に塗布した。印刷条件は表2に示した。塗膜をホットプレート上で160℃、3分加熱することで厚さ6.9μmの硬化膜を作製した。作製した塗膜の導電性を抵抗テスターにて確認したところ、測定不能であり絶縁性であることを確認した。結果を表2に示す。
熱硬化性樹脂としてECAを100質量部、希釈剤として2EHGEを4質量部、およびカチオン重合開始剤としてSI-100を1質量部、ならびに導電性粒子としてLiq.62を68質量部(固形分換算量)配合し、エバポレーターにて溶媒を留去し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例3にて調製した異方性導電材料をスクリーン印刷にてガラス基板上に塗布した。印刷条件は表2に示した。塗膜をホットプレート上で160℃、3分加熱することで厚さ8.8μmの硬化膜を作製した。作製した塗膜の導電性を抵抗テスターにて確認したところ、測定不能であり絶縁性であることを確認した。結果を表2に示す。
熱硬化性樹脂としてTEPeICを100質量部、カチオン重合開始剤としてSI-100を1質量部、ならびに導電性粒子Liq.62を68質量部(固形分換算量)配合し、エバポレーターにて溶媒を留去し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例5にて調製した異方性導電材料をスクリーン印刷にてガラス基板上に塗布した。印刷条件は表2に示した。塗膜をホットプレート上で160℃、3分加熱することで厚さ4.9μmの硬化膜を作製した。作製した塗膜の導電性を抵抗テスターにて確認したところ、測定不能であり絶縁性であることを確認した。結果を表2に示す。
熱硬化性樹脂としてTEOICを100質量部、希釈剤として2EHGEを4質量部、およびカチオン重合開始剤としてSI-100を1質量部、ならびに導電性粒子Liq.62を68質量部(固形分換算量)配合し、エバポレーターにて溶媒を留去し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例7にて調製した異方性導電材料をスクリーン印刷にてガラス基板上に塗布した。印刷条件は表2に示した。塗膜をホットプレート上で160℃、3分加熱することで厚さ3.3μmの硬化膜を作製した。作製した塗膜の導電性を抵抗テスターにて確認したところ、測定不能であり絶縁性であることを確認した。結果を表2に示す。
図5(A)に示すように、ガラス基板1上に500個(100個×5列)のCu電極3と、隣接するCu電極3,3同士を接続するCu配線4を配置した後、両端の電極3,3(図中、ガラス基板1上の左下および右上に位置する電極)のそれぞれにCuからなる末端配線5を接続してCu電極付きガラス基板Aを作製した。別途、図5(B)に示すように、シリコンウエハ基板2上に500個(100個×5列)のCu電極3と、隣接するCu電極3,3同士を接続する配線4を配置し、Cu電極付きシリコンウエハ基板Bを作製した。両基板をCu電極3を配置した面同士で貼り合わせるときの断面のイメージを図6に示す。図6中、両基板上のCu電極3は、互いに、対向する基板上の隣接する2個の電極を接続できる位置に交互に配置されており、Cu電極付きガラス基板Aの電極3上には本発明の異方性導電材料からなる異方性導電層(図示せず)が形成されている。そして、この図示しない異方性導電層が両基板上のCu電極3により上下方向から挟み込まれ、当該異方性導電層を介して導電経路が形成される。電極間の導通は、末端配線5,5に抵抗テスターをあてて抵抗値を測定することで確認することができる。
作製例1にて作製したCu電極付きガラス基板AのCu電極3上に実施例1にて調製した異方性導電材料を少量のせた(図示せず)。次いで、その上から、Cu電極付きシリコンウエハ基板Bを、当該基板BのCu電極3とCu電極付きガラス基板AのCu電極3とが向かい合うように配置した。180℃に加熱しながら、2MPaの圧力を印荷し、180秒保持してCu電極付きガラス基板AとCu電極付きシリコンウエハ基板Bとを圧着させるとともに、圧着面上の全てのCu電極3を含む範囲に異方性導電層(図示せず)を形成した。電極3,3から延長された末端配線5,5に抵抗テスターをあてて抵抗値を測定し、導通することを確認した。
熱硬化性樹脂としてEPNを100質量部、反応性希釈剤として2EHGEを4質量部、およびカチオン重合開始剤としてSI-100を1質量部配合し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例9における異方性導電材料を、比較例1にて調製したものに変更したこと以外は、実施例9と同様にして異方性導電層を形成した。電極から延長された末端配線に抵抗テスターをあてて抵抗値を測定し、導通しないことを確認した。
図7に示す形状の2つのCu電極3’が形成されたガラス基板1’上に、図8に示すように、厚さ100μmのシリコーンゴム製スペーサー6を置き、両電極3’,3’を覆うように実施例1にて調製した異方性導電材料7を塗布し、塗布基板Cを得た。この塗布基板Cに、予めオプツール(登録商標)DSX[ダイキン工業(株)製]で離型処理した、塗布基板Cと同サイズの石英ガラス基板(図示せず)を被せた。この状態で塗布基板Cをホットプレート上で160℃、3分間加熱し、塗布した異方性導電材料7を硬化させ、厚さ100μmの硬化物とした。その後、石英ガラス基板(図示せず)およびスペーサー6を取り去り、図9に示すような、両電極3’,3’が硬化物8で封止された試験片Dを得た。
実施例10における異方性導電材料を、比較例1にて調製したものに変更したこと以外は、実施例10と同様にして試験片を作製した。
熱硬化性樹脂としてEPNを100質量部、カチオン重合開始剤としてSI-100を1質量部、および導電性粒子としてLiq.139を75質量部配合し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例11にて調製した異方性導電材料をスピンコートにて3,000rpmでガラス基板上に塗布した。塗膜をホットプレート上で250℃、3分加熱することで厚さ9.3μmの硬化膜を作製した。作製した塗膜の導電性を抵抗テスターにて確認したところ、測定不能であり絶縁性であることを確認した。
図10(A)に示すように、ガラス基板1”上に2個のITO電極9を配置した後、これらの電極9,9のそれぞれにITOからなる末端配線10を接続してITO電極付きガラス基板Eを作製した。別途、図10(B)に示すように、シリコンウエハ基板2”上に2個のAu電極11と、これらのAu電極11,11同士を接続する配線12を配置し、Au電極付きシリコンウエハ基板Fを作製した。両基板をITO電極9とAu電極11を配置した面同士で貼り合わせるときの断面のイメージを図11に示す。ITO電極付きガラス基板Eの電極9上には本発明の異方性導電材料からなる異方性導電層(図示せず)が形成されている。そして、この図示しない異方性導電層がITO電極付きガラス基板EのITO電極9とAu電極付きシリコンウエハ基板FのAu電極11により上下方向から挟み込まれ、当該異方性導電層を介して導電経路が形成される。電極間の導通は、末端配線10,10に抵抗テスターをあてて抵抗値を測定することで確認することができる。
作製例2にて作製したITO電極付きガラス基板EのITO電極9上に実施例11にて調製した異方性導電材料を少量のせた(図示せず)。次いで、その上から、Au電極付きシリコンウエハ基板Fを、当該基板FのAu電極11とAu電極付きガラス基板EのITO電極9とが向かい合うように配置した。180℃に加熱しながら、2MPaの圧力を印荷し、30秒保持してAu電極付きガラス基板EとAu電極付きシリコンウエハ基板Fとを圧着させ異方性導電層(図示せず)を形成した。電極9,9から延長された末端配線10,10に抵抗テスターをあてて抵抗値を測定し、導通することを確認した。
熱硬化性樹脂としてEPNを100質量部、カチオン重合開始剤としてSI-100を1質量部配合し、自転・公転ミキサーにて混合して異方性導電材料を調製した。
実施例13における異方性導電材料を、比較例4にて調製したものに変更したこと以外は、実施例13と同様にして異方性導電層を形成した。電極から延長された末端配線に抵抗テスターをあてて抵抗値を測定し、導通しないことを確認した。
図7に示す形状の2つのCu電極3’が形成されたガラス基板1’上に、図8に示すように、厚さ200μmのシリコーンゴム製スペーサー6を置き、両電極3’,3’を覆うように実施例11にて調製した異方性導電材料7を塗布し、塗布基板Cを得た。この塗布基板Cに、予めオプツール(登録商標)DSX[ダイキン工業(株)製]で離型処理した、塗布基板Cと同サイズの石英ガラス基板(図示せず)を被せた。この状態で塗布基板Cをホットプレート上で250℃、30秒加熱し、塗布した異方性導電材料7を硬化させ、厚さ200μmの硬化物とした。その後、石英ガラス基板(図示せず)およびスペーサー6を取り去り、図9に示すような、両電極3’,3’が硬化物8で封止された試験片Dを得た。
実施例14における異方性導電材料を、比較例4にて調製したものに変更し、硬化条件を250℃、180秒に変更した以外は、実施例14と同様にして試験片を作製した。
2、2” シリコンウエハ基板
3、3’ Cu電極
4 Cu配線
5 末端配線
6 スペーサー
7 異方性導電材料
8 硬化物
9 ITO電極
10 末端配線
11 Au電極
12 Au配線
A Cu電極付きガラス基板
B Cu電極付きシリコンウエハ基板
C 塗布基板
D 試験片
E ITO電極付きガラス基板
F Au電極付きシリコンウエハ基板
Claims (6)
- 熱硬化性樹脂と、重合開始剤と、導電性粒子とを含み、
上記導電性粒子が、導電性コアと、該導電性コアを被覆する絶縁膜とを有し、該導電性コアが、60~250℃の融点を有し、かつ、その融点以下の温度で液体状態である過冷却金属で形成されていることを特徴とする異方性導電材料。 - 上記導電性コアが、In-Bi-Sn系合金、Bi-Sn系合金またはSn-Ag-Cu系合金を含む請求項1記載の異方性導電材料。
- 上記熱硬化性樹脂が、エポキシ樹脂、フェノール樹脂から選ばれる1種または2種である請求項1または2記載の異方性導電材料。
- 上記重合開始剤が、アニオン重合開始剤またはカチオン重合開始剤である請求項1~3のいずれか1項記載の異方性導電材料。
- 請求項1~4のいずれか1項記載の異方性導電材料から得られる異方性導電層。
- 請求項5記載の異方性導電層を有する電子素子。
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