JPWO2019230881A1 - スペーサ粒子、接着剤及び接着構造体 - Google Patents
スペーサ粒子、接着剤及び接着構造体 Download PDFInfo
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Images
Classifications
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/16—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
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Abstract
Description
本発明に係るスペーサ粒子では、200℃における30%圧縮したときの圧縮弾性率の、25℃における30%圧縮したときの圧縮弾性率に対する比は、0.5以上0.9以下である。
F:スペーサ粒子が30%圧縮変形したときの荷重値(N)
S:スペーサ粒子が30%圧縮変形したときの圧縮変位(mm)
R:スペーサ粒子の半径(mm)
L1:負荷を与えるときの原点用荷重値から反転荷重値に至るまでの圧縮変位
L2:負荷を解放するときの反転荷重値から原点用荷重値に至るまでの除荷変位
上記スペーサ粒子の材料は特に限定されない。上記スペーサ粒子の材料は、有機材料であってもよく、無機材料であってもよい。
ρ:スペーサ粒子の粒子径の標準偏差
Dn:スペーサ粒子の粒子径の平均値
本発明に係る接着剤は、上述したスペーサ粒子と、接着性成分とを含む。上記スペーサ粒子は、接着性成分中に分散されて用いられることが好ましく、接着性成分中に分散された接着剤を得るために用いられることが好ましい。
上記熱硬化性成分は特に限定されない。上記接着剤は、上記熱硬化性成分として、熱硬化性化合物及び熱硬化剤とを含んでいてもよい。接着剤をより一層良好に硬化させるために、上記接着剤は、熱硬化性成分として、熱硬化性化合物と熱硬化剤とを含むことが好ましい。接着剤をより一層良好に硬化させるために、上記接着剤は、熱硬化性成分として硬化促進剤を含むことが好ましい。
上記熱硬化性化合物は特に限定されない。上記熱硬化性化合物としては、オキセタン化合物、エポキシ化合物、エピスルフィド化合物、(メタ)アクリル化合物、フェノール化合物、アミノ化合物、不飽和ポリエステル化合物、ポリウレタン化合物、シリコーン化合物及びポリイミド化合物等が挙げられる。熱硬化性接着剤の硬化性及び粘度をより一層良好にする観点からは、上記熱硬化性化合物としては、エポキシ化合物又はエピスルフィド化合物が好ましく、エポキシ化合物がより好ましい。上記熱硬化性化合物は、エポキシ化合物を含むことが好ましい。上記熱硬化性化合物は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記熱硬化剤は特に限定されない。上記熱硬化剤は、上記熱硬化性化合物を熱硬化させる。上記熱硬化剤としては、イミダゾール硬化剤、アミン硬化剤、フェノール硬化剤、ポリチオール硬化剤等のチオール硬化剤、酸無水物硬化剤、熱カチオン開始剤(熱カチオン硬化剤)及び熱ラジカル発生剤等が挙げられる。上記熱硬化剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記接着剤は硬化促進剤を含んでいてもよい。上記硬化促進剤は特に限定されない。上記硬化促進剤は、上記熱硬化性化合物と上記熱硬化剤との反応において硬化触媒として作用することが好ましい。上記硬化促進剤は、上記熱硬化性化合物の反応において硬化触媒として作用することが好ましい。上記硬化促進剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記接着剤は、複数の金属原子含有粒子を含むことが好ましい。上記金属原子含有粒子としては、金属粒子及び金属化合物粒子等が挙げられる。上記金属化合物粒子は、金属原子と、該金属原子以外の原子とを含む。上記金属化合物粒子の具体例としては、金属酸化物粒子、金属の炭酸塩粒子、金属のカルボン酸塩粒子及び金属の錯体粒子等が挙げられる。上記金属化合物粒子は、金属酸化物粒子であることが好ましい。例えば、上記金属酸化物粒子は、還元剤の存在下で接着時の加熱で金属粒子となった後に焼結する。上記金属酸化物粒子は、金属粒子の前駆体である。上記金属のカルボン酸塩粒子としては、金属の酢酸塩粒子等が挙げられる。
上述した接着剤を用いて、被着体を接着することにより、接着構造体を得ることができる。
(1)スペーサ粒子の作製
種粒子として平均粒子径0.8μmのポリスチレン粒子を用意した。上記ポリスチレン粒子3.9重量部と、イオン交換水500重量部と、5重量%ポリビニルアルコール水溶液120重量部とを混合し、混合液を調製した。上記混合液を超音波により分散させた後、セパラブルフラスコに入れて、均一に撹拌した。
銀粒子(平均粒子径15nm)40重量部と、ジビニルベンゼン樹脂粒子(平均粒子径30μm、CV値5%)1重量部と、上記スペーサ粒子10重量部と、溶媒であるトルエン40重量部とを配合し、混合して接着剤を作製した。
第1の被着体として、被着面にNi/Auめっきが施されたパワー半導体素子を用意した。第2の被着体として、窒化アルミニウム基板を用意した。
スペーサ粒子を作製する際に、ジビニルベンゼン150重量部をジビニルベンゼン75重量部及びテトラメチロールメタンテトラアクリレート75重量部に変更したこと、及びスペーサ粒子の粒子径を3.01μmに変更したこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
スペーサ粒子を作製する際に、スペーサ粒子の粒子径を30.5μmに変更したこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
スペーサ粒子を作製する際に、ジビニルベンゼン150重量部をジビニルベンゼン100重量部及びスチレン50重量部に変更したこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
スペーサ粒子を作製せず、スペーサ粒子を用いなかったこと以外は、実施例1と同様にして、接着剤及び接着構造体を得た。
スペーサ粒子として、シリカ粒子(粒子径3.00μm)を用いたこと以外は、実施例1と同様にして、接着剤及び接着構造体を得た。
スペーサ粒子を作製する際に、ジビニルベンゼン150重量部を、イソボルニルアクリレート90重量部と、1,6−ヘキサンジオールジメタクリレート30重量部と、テトラメチロールメタンテトラアクリレート30重量部とに変更し、かつ、スペーサ粒子の粒子径を3.00μmに変更した。これらの変更をしたこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
スペーサ粒子を作製する際に、ジビニルベンゼン150重量部を、ジビニルベンゼン112.5重量部と、PEG200#ジアクリレート37.5重量部とに変更したこと、及びスペーサ粒子の粒子径を3.02μmに変更をしたこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
スペーサ粒子を作製する際に、ジビニルベンゼン150重量部を、ジビニルベンゼン105重量部と、PEG200#ジアクリレート30重量部と、テトラメトロールメタンテトラアクリレート15重量部とに変更し、かつ、スペーサ粒子の粒子径を2.75μmに変更をした。これらの変更をしたこと以外は、実施例1と同様にして、スペーサ粒子、接着剤及び接着構造体を得た。
(1)スペーサ粒子の圧縮弾性率
得られたスペーサ粒子について、25℃における30%圧縮したときの圧縮弾性率(30%K値(25))及び200℃における30%圧縮したときの圧縮弾性率(30%K値(200))を、上述した方法により、微小圧縮試験機(フィッシャー社製「フィッシャースコープH−100」)を用いて測定した。測定結果から、30%K値(25)及び30%K値(200)を算出した。得られた測定結果から、30%K値(200)の、30%K値(25)に対する比(30%K値(200)/30%K値(25))を算出した。
得られたスペーサ粒子について、25℃における圧縮回復率(圧縮回復率(25))及び200℃における圧縮回復率(圧縮回復率(200))を、上述した方法により、微小圧縮試験機(フィッシャー社製「フィッシャースコープH−100」)を用いて測定した。得られた測定結果から、圧縮回復率(200)の、圧縮回復率(25)に対する比(圧縮回復率(200)/圧縮回復率(25))を算出した。
得られた10個の接着構造体について断面研磨を行い、その断面の画像から接着層の厚みを走査型電子顕微鏡を用いて測定した。接着層の厚みのばらつきを以下の基準で判定した。
○○:接着層の厚みの最大値に対する接着層の厚みの最小値の比(接着層の厚みの最小値/接着層の厚みの最大値)が0.9以上
○:接着層の厚みの最大値に対する接着層の厚みの最小値の比(接着層の厚みの最小値/接着層の厚みの最大値)が0.7以上0.9未満
×:接着層の厚みの最大値に対する接着層の厚みの最小値の比(接着層の厚みの最小値/接着層の厚みの最大値)が0.7未満
得られた接着構造体について、マウント強度測定装置(レスカ社製「ボンディングテスターPTR−1100」)を用いて、260℃での接着強度を測定した。なお、シェアスピードは0.5mm/secとして、第2の被着体と接着層との接着部分に水平方向の負荷をかけて測定した。接着強度を以下の基準で判定した。
○○:シェア強度が150N/cm2以上
○:シェア強度が100N/cm2以上150N/cm2未満
×:シェア強度が100N/cm2未満
得られた接着構造体について断面研磨を行い、その断面の画像から接着構造体の接着層においてクラックが発生しているか否かを、走査型電子顕微鏡を用いて観察した。応力緩和特性を以下の基準で判定した。
○○:クラックが発生していない
○:クラックが発生している(実使用上問題なし)
×:クラックが発生している
1A…スペーサ粒子
11…接着構造体
12…第1の被着体
13…第2の被着体
14…接着層
21…液晶表示素子
22…透明ガラス基板
23…透明電極
24…配向膜
25…液晶
26…シール剤
Claims (8)
- 200℃における30%圧縮したときの圧縮弾性率の、25℃における30%圧縮したときの圧縮弾性率に対する比が、0.5以上0.9以下である、スペーサ粒子。
- 200℃における圧縮回復率の、25℃における圧縮回復率に対する比が、0.4以上0.8以下である、請求項1に記載のスペーサ粒子。
- 200℃における圧縮回復率が、20%以上である、請求項1又は2に記載のスペーサ粒子。
- 接着剤を得るために用いられる、請求項1〜3のいずれか1項に記載のスペーサ粒子。
- 請求項1〜4のいずれか1項に記載のスペーサ粒子と、
接着性成分とを含む、接着剤。 - 前記接着性成分が、熱硬化性成分を含み、
接着剤は、熱硬化性接着剤である、請求項5に記載の接着剤。 - 前記接着性成分が、加熱により焼結可能な金属原子含有粒子を含む、請求項5又は6に記載の接着剤。
- 第1の被着体と、
第2の被着体と、
前記第1の被着体及び前記第2の被着体を接着している接着層とを備え、
前記接着層の材料が、請求項1〜4のいずれか1項に記載のスペーサ粒子を含む、接着構造体。
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JP2001083524A (ja) * | 1999-09-09 | 2001-03-30 | Canon Inc | スペーサー付カラーフィルタとその製造方法、該製造方法に用いるビーズ入りスペーサー形成材、該カラーフィルタを用いた液晶素子 |
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CN115322743A (zh) | 2022-11-11 |
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