JP2023016839A - 真空印刷用導電性ペースト - Google Patents
真空印刷用導電性ペースト Download PDFInfo
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- JP2023016839A JP2023016839A JP2022181785A JP2022181785A JP2023016839A JP 2023016839 A JP2023016839 A JP 2023016839A JP 2022181785 A JP2022181785 A JP 2022181785A JP 2022181785 A JP2022181785 A JP 2022181785A JP 2023016839 A JP2023016839 A JP 2023016839A
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- Prior art keywords
- conductive paste
- vacuum printing
- meth
- conductive
- solvent
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- 239000002904 solvent Substances 0.000 claims abstract description 64
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- 239000011347 resin Substances 0.000 claims abstract description 57
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
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- 239000011231 conductive filler Substances 0.000 claims abstract description 38
- 239000012298 atmosphere Substances 0.000 claims abstract description 35
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- 238000009835 boiling Methods 0.000 claims description 18
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
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Abstract
Description
そこで、本発明の一態様は、真空印刷を行う際の50kPa以下の減圧雰囲気では溶剤が揮発し難く、導電性ペーストの粘度の上昇を抑制して、真空印刷における印刷性を良好に維持することができ、加熱硬化時には溶剤が十分に揮発して、微細な溝は貫通孔にボイドが残存することなく、被印刷物への接着性に優れる真空印刷用導電性ペーストを提供することを目的とする。
[2]前記(D)溶剤の101.325kPaの圧力雰囲気における沸点が180~290℃である、前記[1]に記載の真空印刷用導電性ペーストである。
[3]さらに(E)反応性希釈剤を含む、前記[1]又は[2]に記載の真空印刷用導電性ペーストである。
[4]前記(A)導電性フィラーが、銀、ニッケル、銅及びこれらの合金から選択される金属からなる金属粉、並びに金属被覆導電粉末からなる群から選択される少なくとも一種を含む、前記[1]~[3]のいずれかに記載の真空印刷用導電性ペーストである。
[5]前記(B)熱硬化性樹脂が、エポキシ樹脂、(メタ)アクリル樹脂及びフェノール樹脂からなる群から選択される少なくとも一種の樹脂である、前記[1]~[4]のいずれかに記載の真空印刷用導電性ペーストである。
[6]前記(C)硬化剤が、フェノール系硬化剤及びイミダゾール系硬化剤である、前記[1]~[5]のいずれかに記載の真空印刷用導電性ペーストである。
[7]前記(D)溶剤が、アルコール類、グリコールエーテル類、環状エステル類、グリコールエーテルエステル類及びそれらの混合物から選択される、前記[1]~[6]のいずれかに記載の真空印刷用導電性ペーストである。
[8]前記(D)溶剤が、ブチルカルビトール、ベンジルアルコール、2-フェノキシエタノール、ジエチレングリコールモノヘキシルエーテル、ジメチルフタレート、ジエチレングリコールモノブチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、及び2,2,4-トリメチル-1,3-ペンタジオールモノイソブチラートからなる群から選択される少なくとも一種である、前記[1]~[7]のいずれか1項に記載の真空印刷用導電性ペーストである。
[9]さらに(F)エラストマーを含む、前記[1]~[8]のいずれかに記載の真空印刷用導電性ペーストである。
[10]さらに(G)カップリング剤を含む、前記[1]~[9]のいずれかに記載の真空印刷用導電性ペーストである。
[11]前記(B)熱硬化性樹脂の含有量が、前記(A)導電性フィラー100質量部に対して、1~15質量部である、前記[1]~[10]のいずれかに記載の真空印刷用導電性ペーストである。
[12]前記(D)溶剤の含有量が、前記(A)導電性フィラー100質量部に対して、1~30質量部である、前記[1]~[11]のいずれかに記載の真空印刷用導電性ペーストである。
(A)導電性フィラー、
(B)熱硬化性樹脂、
(C)硬化剤、及び
(D)20℃における蒸気圧が0.8~15Paである溶剤と、を含む。
下記表1に示す配合割合となるように各原料を、3本ロールミルを使用して混合・分散して真空印刷用導電性ペーストを製造した。表1中の各組成に関する数値は、質量部を表す。前記導電性ペーストの調整時に使用した原料(各成分)は、以下の通りである。
(A1)銀被覆ニッケル粉(ナミックス株式会社製、体積平均粒径D50:5μm、銀とニッケル粉(ニッケルの純度:99.9質量%)の合計100質量部に対して、銀の量が10質量部。特許第5764294号公報に記載の製造方法により製造した。)
(A2)フレーク状銀粉(商品名:FA2、DOWAエレクトロニクス株式会社製、平均厚さT:0.3μm、体積平均粒径D50:6μm、アスペクト比(T/D50):0.05)
(A3)銀被覆銅粉(商品名:アトマイズ銀粉HWQ5μm、福田金属箔粉工業株式会社製、体積平均粒径D50:5μm、銀と銅の合計100質量部に対して、銀の量が10質量部)
(B1)ビスフェノールF型エポキシ樹脂・ビスフェノールA型エポキシ樹脂混合物(商品名:エピクロンEXA835LV、DIC株式会社製)
(B2)ビスフェノールA型エポキシ樹脂(商品名:AER6072、旭化成イーマテリアルズ株式会社製、AER6072)
(C1)ノボラック型フェノール樹脂(商品名:タマノル758、荒川化学工業株式会社製)
(C2)1-シアノエチル-2-ウンデシルイミダゾール(商品名:キュアゾ-ルC11Z-CN、四国化成株式会社製)
(C3)2-フェニル-4-メチル-5-ヒドロキシメチルイミダゾール(商品名:キュアゾール2P4MHZ-PW、四国化成工業株式会社)
(D1)ジエチレングリコールモノ-n-ブチルエーテルアセテート(米山薬品工業株式会社製、沸点:246.7℃、蒸気圧:5.3Pa(20℃))
(D2)ジメチルフタレート(商品名:DMP、大八化学工業株式会社製、沸点:282℃、蒸気圧:0.8Pa(20℃))
(D3)ジエチレングリコールモノヘキシルエーテル(商品名:キョーワノールHX20、KHネオケム株式会社製、沸点:260℃、蒸気圧:1.3Pa未満(<1.3Pa)(20℃)(蒸気圧は、カタログ又は安全データシート(SDS)に記載の値を記載した。))
(D4)2,2,4-トリメチル-1,3-ペンタジオールモノイソブチラート(商品名:テキサノール、長瀬産業株式会社製、沸点:255℃~261.5℃、蒸気圧:1.3Pa(20℃)(沸点は、カタログ又は安全データシート(SDS)に記載の値を記載した。))
(D5)ブチルカルビトール(大伸化学株式会社製、沸点:231℃、蒸気圧:13Pa(20℃))
(D6)2-フェノキシエタノール(商品名:ハイソルブEPH、東邦化学株式会社製、沸点:245℃、蒸気圧:1.3Pa(20℃))
(D7)ベンジルアルコール(富士フィルム和光純薬株式会社製、沸点:205℃、蒸気圧:13.2Pa(20℃)
(D8)ジエチレングリコールモノエチルエーテルアセテート(商品名:ECA、ダイセル化学工業株式会社製、沸点:218.5℃、蒸気圧:13.3Pa(20℃))
(D9)2-(2-エトキシエトキシ)エタノール(商品名:JCT-EDG、ジャパンケムテック株式会社製、沸点:210.9℃、蒸気圧:15.6Pa(20℃))
(D10)1,3-ブチレングリコールジアセテート(ダイセル化学工業株式会社製、沸点:232℃、蒸気圧:0.0026Pa(20℃))。
各溶剤の沸点は、101.325kPaにおける沸点であり、各溶剤の蒸気圧は20℃における蒸気圧である。
(E1)1,2-エポキシ-4-(2-メチルオキシラニル)-1-メチルシクロヘキサン(商品名:セロキサイド3000、ダイセル化学工業株式会社製)
(E2)炭素数が12~13の混合アルコールのグリシジルエーテル(商品名:エポゴーセEN、四日市合成株式会社製)
(F1)シリコーンゴム(商品名:シリコーン複合パウダーKMP-605、信越化学工業株式会社製)
(F2)カルボキシル基末端アクリロニトリル-ブタジエンゴム(商品名:Hycar-CTBN1300×13、宇部興産株式会社製)
(G1)シランカップリング剤(3-グリシドキシプロピルトリメトキシシラン)(商品名:KBM-403、信越化学工業株式会社製)
レーザー回折散乱法により、粒子径分布測定装置(商品名:マイクロトラックMT3000II、マイクロトラックベル株式会社製)を用いて、(A1)~(A3)の導電性フィラーの体積平均粒径(メジアン径:D50)を測定した。(A2)フレーク状銀粉は、走査型電子顕微鏡を用いて観察し、20個の銀粉の平均厚さTを測定し、アスペクト比
T/D50)を算出した。
1mm×71mmの配線パターンの開口部を有するメッシュスクリーンマスクを使用して、大気圧(標準気圧101.325kPa程度)下で、アルミナ基板上に各実施例及び比較例の導電性ペーストをスクリーン印刷により塗布し、塗布した配線パターンを160℃で30分間硬化させ、硬化物を得た。得られた硬化物の厚さを、表面粗さ・輪郭形状統合測定機(商品名:サーフコム1300SD-2、株式会社東京精密製)を用いて測定した。得られた硬化物の電気抵抗値をデジタルマルチメータ(商品名:ケースレー2001、株式会社TFFケースレーインスツルメンツ製)を用いて測定した。硬化物の厚さ及び電気抵抗値から電気抵抗率(比抵抗値)(10-3Ω・cm)を測定した。結果を表1に示す。
1.5mm角×25個の開口部を有するメッシュスクリーンマスクを使用して、大気圧(標準気圧101.325kPa程度)下で、各実施例及び比較例の導電性ペーストを、20mm角のアルミナ基板上にスクリーン印刷により塗布し、25個のブロック状の印刷パターンのうち、10箇所に10枚の3.2mm×1.6mmサイズのアルミナチップを搭載させた試験片を作製し、200℃、30分間硬化させ、試験片を得た。強度試験機(型番:Model 1605HTP、アイコーエンジニアリング株式会社製)を用いて、加重速度12mm/分における各試験片のせん断強度を求めた。結果を表1に示す。
真空印刷機(型番:LS-100VC、ニューロング精密工業株式会社製)を用いて、各実施例及び比較例の導電性ペーストを、50kPa以下の減圧雰囲気において、アルミナ基板上に1000回スクリーン印刷を行った。スクリーン印刷前の各実施例及び比較例の導電性ペーストの粘度と、1000回スクリーン印刷後の各実施例及び比較例の導電性ペーストの粘度を、ブルックフィールド粘度計(型番:HBDV-1、ブルックフィールド社製)を用いて、25℃で、14号ローターを用いて、10rpmにて測定した。以下の式(1)に示すように、印刷後の粘度から印刷前の粘度を減じて、印刷前の粘度で除した値の比率を真空印刷による粘度変化率として測定した。結果を表1に示す。実施例1の導電性ペーストは、印刷前の粘度が156Pa・sであり、印刷後の粘度が171Pa・sであり、真空印刷による粘度変化率が10%であった。実施例2の導電性ペーストは、印刷前の粘度が468Pa・sであり、印刷後の粘度が540Pa・sであり、粘度変化率が15%であった。実施例3の導電性ペーストは、印刷前の粘度が12Pa・sであり、印刷後の粘度が14Pa・sであり、真空印刷による粘度変化率が17%であった。
(1)粘度変化率(%)=〔印刷後の導電性ペーストの粘度(Pa・s)-印刷前の導電性ペーストの粘度(Pa・s)〕÷印刷前の導電性ペーストの粘度(Pa・s)×100
下記表1に示す配合割合となるように各原料を、3本ロールミルを使用して混合・分散して真空印刷用導電性ペーストを製造した。表1中の各組成に関する数値は、質量部を表す。前記導電性ペーストの調整時に使用した原料(各成分)は、以下の通りである。
Claims (12)
- (A)導電性フィラーと、(B)熱硬化性樹脂と、(C)硬化剤と、(D)20℃における蒸気圧が0.8~15Paである溶剤とを含む、真空印刷用導電性ペースト。
- 前記(D)溶剤の101.325kPaの圧力雰囲気における沸点が180~290℃である、請求項1に記載の真空印刷用導電性ペースト。
- さらに(E)反応性希釈剤を含む、請求項1又は2に記載の真空印刷用導電性ペースト。
- 前記(A)導電性フィラーが、銀、ニッケル、銅及びこれらの合金からなる群から選択される金属からなる金属粉、並びに金属被覆導電粉末からなる群から選択される少なくとも一種を含む、請求項1~3のいずれか1項に記載の真空印刷用導電性ペースト。
- 前記(B)熱硬化性樹脂が、エポキシ樹脂、(メタ)アクリル樹脂及びフェノール樹脂からなる群から選択される少なくとも一種の樹脂である、請求項1~4のいずれか1項に記載の真空印刷用導電性ペースト。
- 前記(C)硬化剤が、フェノール系硬化剤及びイミダゾール系硬化剤である、請求項1~5のいずれか1項に記載の真空印刷用導電性ペースト。
- 、
前記(D)溶剤が、アルコール類、グリコールエーテル類、環状エステル類、グリコールエーテルエステル類及びそれらの混合物から選択される、請求項1~6のいずれか1項に記載の真空印刷用導電性ペースト。 - 前記(D)溶剤が、ブチルカルビトール、ベンジルアルコール、2-フェノキシエタノール、ジエチレングリコールモノヘキシルエーテル、ジメチルフタレート、ジエチレングリコールモノブチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、及び2,2,4-トリメチル-1,3-ペンタジオールモノイソブチラートからなる群から選択される少なくとも一種である、請求項1~7のいずれか1項に記載の真空印刷用導電性ペースト。
- さらに(F)エラストマーを含む、請求項1~8のいずれか1項に記載の真空印刷用導電性ペースト。
- さらに(G)カップリング剤を含む、請求項1~9のいずれか1項に記載の真空印刷用導電性ペースト。
- 前記(B)熱硬化性樹脂の含有量が、前記(A)導電性フィラー100質量部に対して、1~15質量部である、請求項1~10のいずれか1項に記載の真空印刷用導電性ペースト。
- 前記(D)溶剤の含有量が、前記(A)導電性フィラー100質量部に対して、1~30質量部である、請求項1~11のいずれか1項に記載の真空印刷用導電性ペースト。
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