JP7078537B2 - 導電性接着剤組成物 - Google Patents
導電性接着剤組成物 Download PDFInfo
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- JP7078537B2 JP7078537B2 JP2018540086A JP2018540086A JP7078537B2 JP 7078537 B2 JP7078537 B2 JP 7078537B2 JP 2018540086 A JP2018540086 A JP 2018540086A JP 2018540086 A JP2018540086 A JP 2018540086A JP 7078537 B2 JP7078537 B2 JP 7078537B2
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/002—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds
- C08G65/005—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens
- C08G65/007—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens containing fluorine
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- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
- C09J167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C09J167/025—Polyesters derived from dicarboxylic acids and dihydroxy compounds containing polyether sequences
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Description
パワーデバイスは電力損失を抑え、電力変換を高効率に変換できる半導体素子として、電気自動車、ハイブリッド自動車、急速充電器等の分野で普及が進んでおり、また、太陽光発電システム、メガソーラーシステム等の新エネルギー分野においても需要の高まりが期待されている。
1.(A)導電性粒子、(B)熱可塑性樹脂、(C)非極性溶剤、及び(D)非水溶性のフッ素系界面活性剤を含む導電性接着剤組成物。
2.前記導電性接着剤組成物全体に対して、フッ素を20質量ppm以上含有する、前記1に記載の導電性接着剤組成物。
3.前記導電性接着剤組成物全体に対して、フッ素を40質量ppm以上含有する、前記1に記載の導電性接着剤組成物。
4.前記(D)非水溶性のフッ素系界面活性剤のフッ素含有率が20~70%である、前記1~3のいずれか1に記載の導電性接着剤組成物。
5.前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するフッ素系界面活性剤である、前記1~4のいずれか1に記載の導電性接着剤組成物。
6.前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するエチレンオキシド付加物である、前記1~5のいずれか1に記載の導電性接着剤組成物。
7.前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するオリゴマー化合物である、前記1~6のいずれか1に記載の導電性接着剤組成物。
8.前記(A)導電性粒子は、Ag又はCuを主成分とする粉状の金属粒子である、前記1~7のいずれか1に記載の導電性接着剤組成物。
9.前記(B)熱可塑性樹脂が、エステル樹脂である、前記1~8のいずれか1に記載の導電性接着剤組成物。
10.前記エステル樹脂が、飽和エステル樹脂である、前記9に記載の導電性接着剤組成物。
11.前記(C)非極性溶剤が脂肪族または芳香族炭化水素である、前記1~10のいずれか1に記載の導電性接着剤組成物。
A.接着剤組成物の調製
表1に記載された各材料を三本ロールやホモジナイザーにて混練し、表1に示す組成の接着剤組成物を調製した(各材料の数値は接着剤組成物の総質量に対する質量%を表す)。使用した材料は下記の通りである。なお、混練の順番は、(C)非極性溶剤、(B)エステル樹脂、(A)導電性粒子、(D)フッ素系界面活性剤の順である。200℃で1時間加熱後に室温まで放冷し接着剤組成物の硬化体を得た。
導電性粒子として、田中貴金属工業社製の平均粒子径(D50)が3μmでフレーク状の銀粉と田中貴金属工業社製の平均粒子径(D50)が6μmでフレーク状の銀粉を1:1で混合した銀粉を使用した。
熱可塑性樹脂として、田中貴金属工業社製の粉末状の飽和エステル樹脂(ガラス転移点:70~80℃、軟化点120~130℃)を使用した。樹脂のサイズとしては平均粒子径(D50)が10μmである。使用された熱可塑性樹脂は、接着剤組成物中でも溶解せず、粉末状で存在していることを確認した。
非極性溶剤として、FORMOSAN UNION CHEMICAL CORP.製BAB(アルキルベンゼン)とJX日鉱日石エネルギー株式会社製ノルマルパラフィンHを1:1で混合した溶剤を使用した。
・パーフルオロアルキルエチレンオキシド化合物[サーフロンS420、AGCセイケミカル株式会社] フッ素含有率:47%、酢酸エチル0.5%濃度表面張力(mN/m):23.1
・パーフルオロアルキル基を有するオリゴマー化合物[サーフロンS651、AGCセイケミカル株式会社] フッ素含有率23%、0.5%濃度表面張力(mN/m):23.0
・パーフルオロアルキル基を有するオリゴマー化合物[サーフロンS611、AGCセイケミカル株式会社] フッ素含有率:10%、酢酸エチル0.5%濃度表面張力(mN/m):18.4
なお、上記フッ素系界面活性剤のフッ素含有率はイオンクロマトグラフィーを用いて測定した。
比較例で、非水溶性のフッ素系界面活性剤の代わりに使用した非フッ素系界面活性剤は以下のとおりである。
・日本乳化剤製アントックスEDH-400(比較例2)
・日本乳化剤製ニューコール2609(比較例3)
・日本乳化剤製ニューコール565-PS(比較例4)
・花王株式会社AMIET320(比較例5)
・花王株式会社HOMOGENOL L-95(比較例6)
1.ブリードアウト性
まず、各サンプル5.0gを5cc武蔵シリンジに詰めた。ディスペンサーを使い、銅フレームまたは銀めっき銅フレームに0.15mg、10ドットずつ塗布した。
オリンパス社製マイクロスコープSTM7を使い、ブリードアウトの状態を下記(1)及び(2)の条件で観察した。
(1)塗布してからすぐ(0時間後)
(2)塗布してから2時間後
測定は円形に塗布された接着剤の末端からブリードアウトの末端までの幅(μm)を測定した。また、測定ポイントは1ドットにつき、上下左右4箇所とした。
サンプルごと、条件ごとにブリードアウトの平均値を求め、下記の基準で評価した。○はブリードアウト抑制効果が優良、△は良好、×は不良を示す。
○:ブリードアウト100μm未満
△:ブリードアウト100μm以上200μm未満
×:ブリードアウト200μm以上
銅フレーム
○:ブリードアウト100μm未満
△:ブリードアウト100μm以上300μm未満
×:ブリードアウト300μm以上
上記調製した接着剤組成物を、それぞれガラス基板上に日栄化工社製の透明PETシートテープでマスキングし、幅0.5mm、長さ60mmのパターンでステンシル印刷し、オーブンに入れ、200℃60分の条件で硬化させた。その後、室温まで冷却し硬化膜の長さ5cm間の両端に端子を当てて抵抗値を測定した。更に、硬化膜の膜厚を測定した。測定された抵抗値と膜厚から体積抵抗値を算出し導電性(μΩ・cm)を評価した。尚、硬化膜の抵抗値は日置電機株式会社製の3540ミリオームハイテスタを用いて測定した。また、硬化膜の膜厚は、株式会社小坂研究所社製の表面粗さ計サーフコーダSE-30Hを用いて測定した。結果を表1に示す。
本出願は、2017年3月31日出願の日本特許出願特願2017-072959に基づくものであり、その内容はここに参照として取り込まれる。
Claims (11)
- (A)導電性粒子、(B)熱可塑性樹脂、(C)非極性溶剤、及び(D)非水溶性のフッ素系界面活性剤を含む導電性接着剤組成物であって、
前記(B)熱可塑性樹脂が、ポリエステル樹脂およびポリアミド樹脂の少なくとも一方を含む、導電性接着剤組成物。 - 前記導電性接着剤組成物全体に対して、フッ素を20質量ppm以上含有する、請求項1に記載の導電性接着剤組成物。
- 前記導電性接着剤組成物全体に対して、フッ素を40質量ppm以上含有する、請求項1に記載の導電性接着剤組成物。
- 前記(D)非水溶性のフッ素系界面活性剤のフッ素含有率が20~70%である、請求項1~3のいずれか1項に記載の導電性接着剤組成物。
- 前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するフッ素系界面活性剤である、請求項1~4のいずれか1項に記載の導電性接着剤組成物。
- 前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するエチレンオキシド付加物である、請求項1~5のいずれか1項に記載の導電性接着剤組成物。
- 前記(D)非水溶性のフッ素系界面活性剤が、パーフルオロアルキル基を有するオリゴマー化合物である、請求項1~6のいずれか1項に記載の導電性接着剤組成物。
- 前記(A)導電性粒子は、Ag又はCuを主成分とする粉状の金属粒子である、請求項1~7のいずれか1項に記載の導電性接着剤組成物。
- 前記(B)熱可塑性樹脂が、ポリエステル樹脂である、請求項1~8のいずれか1項に記載の導電性接着剤組成物。
- 前記ポリエステル樹脂が、飽和ポリエステル樹脂である、請求項9に記載の導電性接着剤組成物。
- 前記(C)非極性溶剤が脂肪族または芳香族炭化水素である、請求項1~10のいずれか1項に記載の導電性接着剤組成物。
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