JP2015159128A - 金属薄膜積層体の製造方法 - Google Patents
金属薄膜積層体の製造方法 Download PDFInfo
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- JP2015159128A JP2015159128A JP2015105296A JP2015105296A JP2015159128A JP 2015159128 A JP2015159128 A JP 2015159128A JP 2015105296 A JP2015105296 A JP 2015105296A JP 2015105296 A JP2015105296 A JP 2015105296A JP 2015159128 A JP2015159128 A JP 2015159128A
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- Prior art keywords
- thin film
- metal
- copper
- metal thin
- fine particles
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Abstract
【解決手段】 金属薄膜積層体の製造方法であって、前記金属薄膜は、少なくとも金属微粒子と樹脂バインダーからなり、前記金属微粒子はその表面が銅および/または銅化合物からなるものであり、前記金属薄膜の断面に対し金属微粒子断面が占める割合が40%以上80%以下であり、前記金属薄膜の20℃における体積抵抗率が1×10−4Ω・cm以下であり、前記金属微粒子、前記樹脂バインダー及び有機溶剤を含有する分散体をフレキシブルな絶縁性基材に塗布又は印刷して塗膜を形成し、次いで有機溶剤の少なくとも一部を揮発させた後、さらに150℃以上の過熱水蒸気による加熱処理を施すことを特徴とする、金属薄膜積層体の製造方法。
【選択図】 なし
Description
(1)金属薄膜積層体の製造方法であって、
前記金属薄膜は、少なくとも金属微粒子と樹脂バインダーからなり、
前記金属微粒子はその表面が銅および/または銅化合物からなるものであり、
前記金属薄膜の断面に対し金属微粒子断面が占める割合が40%以上80%以下であり、
前記金属薄膜の20℃における体積抵抗率が1×10−4Ω・cm以下であり、
前記金属微粒子、前記樹脂バインダー及び有機溶剤を含有する分散体をフレキシブルな絶縁性基材に塗布又は印刷して塗膜を形成し、次いで有機溶剤の少なくとも一部を揮発させた後、さらに150℃以上の過熱水蒸気による加熱処理を施すことを特徴とする、金属薄膜積層体の製造方法。
(2)前記過熱水蒸気による加熱処理において、200℃以上の過熱水蒸気を使用する(1)記載の金属薄膜積層体の製造方法。
(3)前記樹脂バインダーがポリエステル樹脂またはポリウレタン樹脂の少なくとも1種からなる(1)又は(2)記載の金属薄膜積層体の製造方法。
(4)前記金属微粒子の平均粒径が0.01μm以上2μm以下である(1)〜(3)のいずれかに記載の金属薄膜積層体の製造方法。
(5)前記金属微粒子が銅および/または銅酸化物からなるものである(1)〜(4)のいずれかに記載の金属薄膜積層体の製造方法。
(6)前記金属薄膜の厚さが20μm以下である(1)〜(5)のいずれかに記載の金属薄膜積層体の製造方法。
横河M&C社製直流精密測定器ダブルブリッジ2769−10を用いて測定した。電気抵抗は体積抵抗率で表示した。
ニチバン株式会社製セロテープ(登録商標)「CT405AP−15」の1cm幅のものを使用し、金属薄膜面にその接着テープを5cm長貼り付け、剥がした際に金属薄膜面が損傷を受けているかどうか、目視観察により判断した。金属薄膜に剥がれ、浮き、亀裂等の何らかの損傷が認められた場合には×、損傷が認められなかった場合には○と判定した。
金属薄膜試料の小片を樹脂包埋し、クロスセクションポリッシャー(日本電子株式会社製SM−09010)を用いて金属薄膜断面試料を作製した。走査型電子顕微鏡(日立ハイテクノロジーズ社製S4800)を用い、無蒸着、加速電圧5kVで金属薄膜断面試料を観察した。観察倍率は、一視野中の金属粒子数が50〜500個となる倍率とした。実施例1の場合は20000倍とした。金属薄膜の断面写真から、金属薄膜層中に金属粒子の断面積が占める割合を面積率で求めた。面積率の決定は以下のようにして行った;
1)観察倍率2万倍の電子顕微鏡写真を長さ基準2倍に拡大コピーした。
2)切り抜き重量法により、1)の写真における金属薄膜断面積に対する金属粒子の断面積の比率を求めた。なお、電子顕微鏡写真上で金属薄膜断面の外縁が判別できない場合は、金属薄膜内の最も基材側に存在する金属粒子を連結する線と最も包埋樹脂側に存在する金属粒子を連結する線を金属薄膜の外縁と仮定した。
3)同様にして11箇所の断面金属比率をとり、小さい順にならべ、4〜8番目のデータの平均値をその試料の断面金属比率とした。
銅微粒子(1):三井金属鉱業社製銅粉「1020Y」。平均粒径360nmの湿式銅粉。
下記の配合割合の組成物をサンドミルにいれ、800rpmで、6時間分散した。メディアは半径1mmのジルコニアビーズを用いた。さらに、日本ポリウレタン社製ポリイソシアネート「コロネートHX」を0.2部添加してよく振って溶解させた。このようにして得た硬化剤を含有する銅微粒子分散体をアプリケーターによりポリイミドフィルム上に乾燥後の厚みが2μmになるように塗布し、100℃で5分熱風乾燥し、金属薄膜積層体1を得た。
バインダー樹脂の溶液 2.5部
トルエン/シクロヘキサノン=1/1(重量比)の40重量%溶液
バインダー樹脂:共重合ポリエステル、東洋紡積社製バイロン300
銅微粒子(1) 15部
メチルエチルケトン(希釈溶剤) 8部
トルエン (希釈溶剤) 8部
シクロヘキサノン (希釈溶剤) 8部
理炉で行った。金属薄膜積層体1Bについて、膜厚、断面金属比率、電気抵抗および接着力を評価した。膜厚は0.4μmであった。断面の電子顕微鏡写真の一例を図1に、断面金属比率等の評価結果を表1に示した。
実施例1で得られた金属薄膜積層体1Aを比較例とし、実施例1と同様に膜厚、断面金属比率、電気抵抗および接着力を評価した。断面の電子顕微鏡写真の一例を図2に、断面金属比率等の評価結果を表1に示した。
下記の配合割合の組成物とメディアとして直径1mmのガラスビーズとをサンドミルにいれ、800rpmで、4時間分散し、銅微粒子分散体2を得た。
バインダー樹脂の溶液 2.2部
トルエン/シクロヘキサノン=1/1(重量比)の45重量%溶液
バインダー樹脂:共重合ポリエステル、東洋紡積社製バイロン300
銅微粒子(1)(平均粒径360nm) 15部
メチルエチルケトン(希釈溶剤) 8部
トルエン (希釈溶剤) 8部
シクロヘキサノン (希釈溶剤) 8部
する熱処理炉で行った。金属薄膜積層体2Bについて、膜厚、断面金属比率、電気抵抗および接着力を評価した。膜厚は1.2μm、断面金属比率は47%、体積抵抗率は9.6×10−5Ω・cm、接着力は○であった。金属積層体2Bの断面の電子顕微鏡写真の一例を図3に示した。
下記の配合割合の組成物とメディアとして直径1mmのガラスビーズとをサンドミルにいれ、800rpmで、4時間分散し、銅微粒子分散体3を得た。
バインダー樹脂の溶液 7部
トルエン/シクロヘキサノン=1/1(重量比)の45重量%溶液
バインダー樹脂:共重合ポリエステル、東洋紡積社製バイロン300
銅微粒子(1)(平均粒径360nm) 13部
メチルエチルケトン(希釈溶剤) 8部
トルエン (希釈溶剤) 8部
シクロヘキサノン (希釈溶剤) 8部
する熱処理炉で行った。金属薄膜積層体3Bについて、膜厚、断面金属比率、電気抵抗および接着力を評価した。膜厚は2.1μm、断面金属比率は25%、体積抵抗率は>1000Ω・cm、接着力は○であった。
2:金属薄膜
3:包埋樹脂
Claims (6)
- 金属薄膜積層体の製造方法であって、
前記金属薄膜は、少なくとも金属微粒子と樹脂バインダーからなり、
前記金属微粒子はその表面が銅および/または銅化合物からなるものであり、
前記金属薄膜の断面に対し金属微粒子断面が占める割合が40%以上80%以下であり、
前記金属薄膜の20℃における体積抵抗率が1×10−4Ω・cm以下であり、
前記金属微粒子、前記樹脂バインダー及び有機溶剤を含有する分散体をフレキシブルな絶縁性基材に塗布又は印刷して塗膜を形成し、次いで有機溶剤の少なくとも一部を揮発させた後、さらに150℃以上の過熱水蒸気による加熱処理を施すことを特徴とする、金属薄膜積層体の製造方法。 - 前記過熱水蒸気による加熱処理において、200℃以上の過熱水蒸気を使用する請求項1記載の金属薄膜積層体の製造方法。
- 前記樹脂バインダーがポリエステル樹脂またはポリウレタン樹脂の少なくとも1種からなる請求項1又は2記載の金属薄膜積層体の製造方法。
- 前記金属微粒子の平均粒径が0.01μm以上2μm以下である請求項1〜3のいずれかに記載の金属薄膜積層体の製造方法。
- 前記金属微粒子が銅および/または銅酸化物からなるものである請求項1〜4のいずれかに記載の金属薄膜積層体の製造方法。
- 前記金属薄膜の厚さが20μm以下である請求項1〜5のいずれかに記載の金属薄膜積層体の製造方法。
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