JP2020032657A - 導電性積層体の製造方法、導電性積層体及び2剤型導電膜形成剤 - Google Patents
導電性積層体の製造方法、導電性積層体及び2剤型導電膜形成剤 Download PDFInfo
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- JP2020032657A JP2020032657A JP2018162447A JP2018162447A JP2020032657A JP 2020032657 A JP2020032657 A JP 2020032657A JP 2018162447 A JP2018162447 A JP 2018162447A JP 2018162447 A JP2018162447 A JP 2018162447A JP 2020032657 A JP2020032657 A JP 2020032657A
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Abstract
Description
本実施形態の導電性積層体の製造方法は、基材と、基材上に設けられた導電性を有する膜とを備える導電性積層体を製造する方法であって、基材上に熱硬化性樹脂を含む樹脂組成物層を設ける工程S1と、樹脂組成物層上に銅含有粒子を含む金属粒子含有層を設ける工程S2と、樹脂組成物層及び金属粒子含有層を加熱することにより、樹脂組成物層の硬化物によって基材に接着された導電膜を形成する工程S3とを備える。
基材としては、特に制限されず、導電性を有していても有していなくてもよい。基材の材質としては、例えば、金、銀、銅、白金、パラジウム、亜鉛、ニッケル、錫、コバルト、鉄、アルミニウム等の金属、これら金属の合金、酸化インジウム錫、酸化亜鉛、酸化インジウム亜鉛、酸化インジウムガリウム亜鉛、ケイ素、炭化ケイ素、窒化ガリウム等の半導体、石英ガラス、ホウケイ酸ガラス、ソーダ石灰ガラス等のガラス、黒鉛、グラファイト等のカーボン材料、樹脂、紙などを挙げることができる。
金属粒子含有層は、銅含有粒子を含む導体形成用組成物を用いて形成することができる。導体形成用組成物は、銅含有粒子の他に、必要に応じて、分散媒、樹脂成分等のその他の成分を含有うすることができる。
工程S3では、樹脂組成物層及び金属粒子含有層を加熱することにより、基材上に、樹脂組成物層の硬化物(樹脂硬化物)を形成するとともに、銅含有粒子を焼結させて導体化し、樹脂硬化物上に銅含有粒子の焼結体を含む導電膜を形成する。これにより、樹脂組成物層の硬化物によって基材に接着された導電膜が得られる。なお、金属粒子含有層が被覆銅粒子を含む場合、加熱により銅を含むコア粒子の表面を被覆する有機物が除去され、コア粒子同士が接触することで導体化が達成され得る。
本実施形態の導電性積層体は上述の導電性積層体の製造方法により得ることができ、導電性積層体は、基材と、該基材上に設けられた導電膜とを備え、導電膜が銅含有粒子の焼結体を含み、基材と導電膜との間に、これらを接着する熱硬化性樹脂組成物の硬化物を有する。本実施形態の導電性積層体は、基材及び硬化物の間並びに硬化物及び導電膜の間が充分な接着性を有することができ、導電膜が導電性を確保しやすいものになり得る。
本実施形態の2剤型導電膜形成剤は、熱硬化性樹脂を含むa剤と、銅含有粒子を含むb剤とを備える。a剤としては、上述した熱硬化性樹脂組成物が挙げられる。b剤としては、上述した導体形成用組成物が挙げられる。
[熱硬化性樹脂組成物の調製]
ビスフェノールA骨格及び炭素原子数6の直鎖状炭化水素を有するエポキシ樹脂である「EPICLON EXA4816」(DIC株式会社製、商品名)40質量部を、テルピネオール(和光純薬工業株式会社製)60質量部に溶解させた。この溶液に、硬化剤として「FXR−1081」(T&K TOKA株式会社製、商品名)を、エポキシ樹脂100質量部に対して5質量部の割合で加え、自転公転式撹拌機「あわとり錬太郎」(シンキー株式会社製、商品名)を使用して攪拌し、熱硬化性樹脂組成物を得た。
<銅含有粒子の用意>
銅含有粒子として、下記の球状の銅含有粒子(A)と、下記の扁平状の銅含有粒子(B)とを質量比70:30で混合したものを用意した。なお、[(A)の含有量]/[(B)の含有量]が70/30である。
球状の銅含有粒子(A):「CH−0200」(三井金属鉱業株式会社製、製品名、メジアン径(D50):0.15μm)
扁平状の銅含有粒子(B):「1050YF」(三井金属鉱業株式会社製、製品名、メジアン径(D50):1.4μm、アスペクト比(平均):7)
分散媒として、テルピネオール(日本テルペン化学株式会社製)と、イソボルニルシクロヘキサノール(日本テルペン化学株式会社)とを質量比70:30で混合したものを用意した。
<樹脂組成物層の形成>
LCP基材である「スミカスーパーE6007」(住友化学株式会社製、商品名)上に、上述の熱硬化性樹脂組成物を、スピンコータ「1H−DX1」(ミカサ株式会社製、商品名)を用いて、回転数500rpmでスピンコートし、樹脂組成物層を形成した。その後、樹脂組成物層を、80℃のオーブン(大気)で30分間加熱し、乾燥した。乾燥後の樹脂組成物層の厚さは15μmであった。
乾燥後の樹脂組成物層上に、上述の導体形成用組成物を、バーコーター(塗布ギャップ:55μm)を用いて塗布し、金属粒子含有層を形成した。
上記で形成した樹脂組成物層及び金属粒子含有層を備える基材を、水素焼結接合装置(神港精機株式会社製)に入れ、100%水素雰囲気において225℃で90分間の加熱処理を行った。こうして、LCP基材上に、樹脂硬化物によって接着された、金属銅(焼結銅)の薄膜からなる導電膜が設けられた導電性積層体を得た。
<体積低効率の測定>
導電膜の体積抵抗率を、4端針面抵抗測定器「ロレスタGP MCP−T610」(株式会社三菱化学アナリテック製、商品名)で測定した面抵抗値と、接触式の段差計「ET200」(株式会社小坂製作所製、商品名)で求めた膜厚とから計算した。結果を表1に示す。
導電性積層体における導電膜と基材との90度ピール強度を下記の方法で測定し、導電膜の接着性を評価した。
スピンコータの回転数を1000rpmとして樹脂組成物層(乾燥後の厚さ10μm)を形成した以外は、実施例1と同様にして導電性積層体を作製し、同様の評価を行った。結果を表1に示す。
スピンコータの回転数を2000rpmとして樹脂組成物層(乾燥後の厚さ5μm)を形成した以外は、実施例1と同様にして導電性積層体を作製し、同様の評価を行った。結果を表1に示す。
60℃のオーブン(大気)で30分間加熱して樹脂組成物層(乾燥後の厚さ20μm)を形成した以外は、実施例2と同様にして導電性積層体を作製し、同様の評価を行った。結果を表1に示す。
エポキシ樹脂としてビスフェノールA骨格を有する、「JER828」(三菱ケミカル株式会社 商品名)を使用した以外は、実施例2と同様にして導電性積層体を作製し、同様の評価を行った。結果を表1に示す。
樹脂組成物層を形成しなかった以外は、実施例1と同様にして導電性積層体を作製し、同様の評価を行った。結果を表1に示す。
Claims (10)
- 基材と、基材上に設けられた導電膜と、を備える導電性積層体を製造する方法であって、
前記基材上に熱硬化性樹脂を含む樹脂組成物層を設ける工程と、
前記樹脂組成物層上に銅含有粒子を含む金属粒子含有層を設ける工程と、
前記樹脂組成物層及び前記金属粒子含有層を加熱することにより、前記樹脂組成物層の硬化物によって前記基材に接着された導電膜を形成する工程と、
を備える、導電性積層体の製造方法。 - 前記熱硬化性樹脂が、ビスフェノール骨格と炭素数4以上の直鎖状炭化水素基とを有するエポキシ樹脂、及び/又は、ビスフェノール骨格と3以上のエーテル結合を含むポリオキシアルキレン基とを有するエポキシ樹脂含む、請求項1に記載の導電性積層体の製造方法。
- 前記銅含有粒子が、銅を含むコア粒子と、前記コア粒子の表面の少なくとも一部を被覆する有機被覆層とを有する被覆銅粒子である、請求項1又は2に記載の導電性積層体の製造方法。
- 前記金属粒子含有層が、前記銅含有粒子を含む導体形成用組成物を前記樹脂組成物層上に塗布することにより形成され、
前記導体形成用組成物における前記銅含有粒子の含有量が、前記導体形成用組成物の全質量100質量部に対して、20〜80質量部である、請求項1〜3のいずれか一項に記載の導電性積層体の製造方法。 - 前記加熱の温度が100℃〜250℃である、請求項1〜4のいずれか一項に記載の導電性積層体の製造方法。
- 基材と、該基材上に設けられた導電膜と、を備える導電性積層体であって、
前記導電膜が銅含有粒子の焼結体を含み、
前記基材と前記導電膜との間に、これらを接着する熱硬化性樹脂組成物の硬化物を有する、導電性積層体。 - 前記熱硬化性樹脂組成物が、ビスフェノール骨格と炭素数4以上の直鎖状炭化水素基とを有するエポキシ樹脂、及び/又は、ビスフェノール骨格と3以上のエーテル結合を含むポリオキシアルキレン基とを有するエポキシ樹脂を含む、請求項6に記載の導電性積層体。
- 熱硬化性樹脂を含むa剤と、
銅含有粒子を含むb剤と、を備える、2剤型導電膜形成剤。 - 前記熱硬化性樹脂が、ビスフェノール骨格と炭素数4以上の直鎖状炭化水素基とを有するエポキシ樹脂、及び/又は、ビスフェノール骨格と3以上のエーテル結合を含むポリオキシアルキレン基とを有するエポキシ樹脂を含む、請求項8に記載の2剤型導電膜形成剤。
- 前記銅含有粒子が、銅を含むコア粒子と、前記コア粒子の表面の少なくとも一部を被覆する有機被覆層とを有する被覆銅粒子である、請求項8又は9に記載の2剤型導電膜形成剤。
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