JP7092670B2 - 樹脂粒子、接続材料及び接続構造体 - Google Patents
樹脂粒子、接続材料及び接続構造体 Download PDFInfo
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- JP7092670B2 JP7092670B2 JP2018532346A JP2018532346A JP7092670B2 JP 7092670 B2 JP7092670 B2 JP 7092670B2 JP 2018532346 A JP2018532346 A JP 2018532346A JP 2018532346 A JP2018532346 A JP 2018532346A JP 7092670 B2 JP7092670 B2 JP 7092670B2
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Description
本発明に係る樹脂粒子は、一般式:[(R)3SiO1/2]で表されるM単位、一般式:[(R)2SiO2/2]で表されるD単位、一般式:[(R)SiO3/2]で表されるT単位及び一般式:[SiO4/2]で表されるQ単位の合計の全個数100%中、上記T単位及び上記Q単位の合計の個数が、4%以下である。なお、M単位、D単位、T単位、及びQ単位が、上記の一般式で表されることは、公知である。上記一般式におけるRは、任意の基を表す。Rの任意の基として、上記一般式の単位外のSiに結合しているO1/2基は除かれる。
十分に乾燥させた樹脂粒子を用いて、下記測定条件における29Si-固体NMR測定(DD/MAS法)により、上記の各単位のシグナル量の積分値を得ることができる。得られた上記の各単位のシグナル量の積分値からTnQnを算出することができる。
装置:Jeol Resonance社製「JNM-ECX400」
観測核:29Si
プローブ:固体NMR用8mmプローブ
MAS回転数:7kHz
測定法:Single pulse(DD/MAS)
パルス幅:3.45μ秒(29Si/90度)
遅延時間:315秒
取り込み時間:21ミリ秒
スキャン回数:500回
D単位:-30ppm~-5ppm
T単位:-75ppm~-50ppm
Q単位:-120ppm~-100ppm
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
F:樹脂粒子が10%圧縮変形したときの荷重値(N)
S:樹脂粒子が10%圧縮変形したときの圧縮変位(mm)
R:樹脂粒子の半径(mm)
ρ:樹脂粒子の粒子径の標準偏差
Dn:樹脂粒子の粒子径の平均値
内部応力をより一層効果的に緩和する観点、及びスプリングバックの発生をより一層効果的に抑制する観点からは、上記樹脂粒子は、シリコーン樹脂を含む粒子であることが好ましい。
上記接続材料は、2つの接続対象部材を接続する接続部を形成するために用いられる。上記接続材料は、上述した樹脂粒子と、バインダー又は金属原子含有粒子とを含む。上記接続材料は、金属原子含有粒子の焼結体によって、上記接続部を形成するために用いられることが好ましい。上記バインダーには、本発明に係る樹脂粒子は含まれない。上記金属原子含有粒子には、本発明に係る樹脂粒子は含まれない。
上述した樹脂粒子とバインダー又は金属原子含有粒子とを含む接続材料を用いて、接続対象部材を接続することにより、接続構造体を得ることができる。
(1)樹脂粒子A(シリコーン粒子A)の作製
両末端アクリルシリコーンオイル(信越化学工業社製「X-22-2445」)30重量部に、tert-ブチル-2-エチルペルオキシヘキサノアート(重合開始剤、日油社製「パーブチルO」)0.5重量部を溶解させた溶解液Aを用意した。また、イオン交換水150重量部に、ラウリル硫酸トリエタノールアミン塩40重量%水溶液(乳化剤)0.8重量部とポリビニルアルコール(重合度:約2000、けん化度:86.5~89モル%、日本合成化学社製「ゴーセノールGH-20」)の5重量%水溶液80重量部とを混合して、水溶液Bを用意した。温浴槽中に設置したセパラブルフラスコに、上記溶解液Aを入れた後、上記水溶液Bを添加した。その後、Shirasu Porous Glass(SPG)膜(細孔平均径約5μm)を用いることで、乳化を行った。その後、85℃に昇温して、9時間重合を行った。重合後の粒子の全量を遠心分離により水洗浄した後、分級操作を行った後、凍結乾燥させて樹脂粒子A(シリコーン粒子A)を得た。
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、上記樹脂粒子A10重量部と、溶媒であるトルエン40重量部とを配合し、混合して接続材料を作製した。
第1の接続対象部材として、パワー半導体素子を用意した。第2の接続対象部材として、窒化アルミニウム基板を用意した。
液晶滴下工法用シール剤の作製:
以下の材料を用意した。
樹脂粒子A(シリコーン粒子A)30重量部
ビスフェノールA型エポキシメタクリレート(熱硬化性化合物、ダイセル・オルネクス社製「KRM7985」)50重量部
カプロラクトン変性ビスフェノールA型エポキシアクリレート(熱硬化性化合物、ダイセル・オルネクス社製「EBECRYL3708」)20重量部
部分アクリル変性ビスフェノールE型エポキシ樹脂(熱硬化性化合物、ダイセル・オルネクス社製「KRM8276」)30重量部
2,2-ジメトキシ-2-フェニルアセトフェノン(光ラジカル重合開始剤、BASF Japan社製「IRGACURE651」)2重量部
マロン酸ジヒドラジド(熱硬化剤、大塚化学社製「MDH」)10重量部
シリカ(充填剤、アドマテックス社製「アドマファインSO-C2」)20重量部
3-グリシドキシプロピルトリメトキシシラン(シランカップリング剤、信越化学工業社製「KBM-403」)2重量部
得られたシール剤100重量部に対して、スペーサ粒子(平均粒子径5μm、積水化学工業社製「ミクロパールSP-205」)1重量部を配合し、遊星式撹拌装置を用いて、シール剤中にスペーサ粒子を均一に分散させた。得られたスペーサ粒子含有シール剤をディスペンス用シリンジ(武蔵エンジニアリング社製「PSY-10E」)に充填し、脱泡処理を行った。その後、ディスペンサー(武蔵エンジニアリング社製「SHOTMASTER300」)を用いて、ITO薄膜が形成された透明電極基板上に長方形の枠を描くように、スペーサ粒子含有シール剤を塗布した。次いで、液晶滴下装置を用いて、TN液晶(チッソ社製「JC-5001LA」)の微小滴を、透明電極基板のスペーサ粒子含有シール剤が塗布された長方形の内側に滴下して塗布した。シール剤及びTN液晶が塗布された透明電極基板と、シール剤及びTN液晶が塗布されていない透明電極基板を、真空貼り合わせ装置を用いて5Paの真空下にて貼り合わせた。次いで、シール剤を塗布した部分にメタルハライドランプを用いて100mW/cm2の紫外線を30秒照射した後、120℃で1時間加熱してシール剤を熱硬化させ、液晶表示素子(セルギャップ5μm)を得た。
樹脂粒子を作製する際に、信越化学工業社製「X-22-2445」の代わりに信越化学工業社製「X-22-1602」を用いたこと以外は参考例1と同様にして樹脂粒子B(シリコーン粒子B)を得た。樹脂粒子Aを樹脂粒子Bに変更したこと以外は、参考例1と同様にして、接続材料、接続構造体及び液晶表示素子を得た。
(1)樹脂粒子C(樹脂被覆シリコーン粒子C)の作製
温浴槽内に設置した500mlのセパラブルフラスコに、参考例1で得られた樹脂粒子A(シリコーン粒子A)6.5重量部と、ヘキサデシルトリメチルアンモニウムブロミド0.6重量部と、蒸留水240重量部と、メタノール120重量部とを入れ、40℃で1時間攪拌した。次いで、ジビニルベンゼン3.0重量部とスチレン0.5重量部とをセパラブルフラスコ内に添加して、75℃まで昇温し、0.5時間攪拌した。次いで、2,2’-アゾビス(イソ酪酸)ジメチル0.4重量部をセパラブルフラスコ内に添加して、8時間攪拌し、重合反応させた。重合反応後、遠心分離を行うことで得られた粒子を水洗浄して、樹脂粒子C(樹脂被覆シリコーン粒子C)を得た。
接続材料及び液晶表示素子を作製する際に、樹脂粒子Aの代わりにシリコーンパウダー「KMP-605」(信越化学工業社製)を用いたこと以外は、参考例1と同様にして、接続材料、接続構造体及び液晶表示素子を得た。
接続材料及び液晶表示素子を作製する際に、樹脂粒子Aの代わりにシリコーンパウダー「KMP-590」(信越化学工業社製)を用いたこと以外は、参考例1と同様にして、接続材料、接続構造体及び液晶表示素子を得た。
(1)T単位及びQ単位の合計の個数(TnQn)
上記M単位、上記D単位、上記T単位及び上記Q単位の合計の個数100%中、上記T単位及び上記Q単位の合計の個数(TnQn)を、29Si-固体NMR分析することにより、上述した方法で算出した。
得られた樹脂粒子の粒子径を、粒度分布測定装置(ベックマンコールター社製「Multisizer4」)を用いて、約100000個の樹脂粒子の粒子径を測定し、平均値を算出することにより求めた。
得られた樹脂粒子の変動係数を、上述した方法で測定した。
得られた樹脂粒子の10%K値を、上述した方法で測定した。
得られた樹脂粒子の40%圧縮変形させた際の圧縮回復率を、上述した方法で測定した。
マウント強度測定装置を用いて、得られた接続構造体の260℃での接続強度を測定した。接続強度を以下の基準で判定した。
○○:シェア強度が150N/cm2以上
〇:シェア強度が100N/cm2以上、150N/cm2未満
×:シェア強度が100N/cm2未満
走査型電子顕微鏡により、得られた接続構造体の接続部においてスプリングバックが発生しているか否かを観察した。スプリングバックを以下の基準で判定した。
○:スプリングバックが発生していない
×:スプリングバックが発生している
走査型電子顕微鏡により、得られた接続構造体の接続部においてクラックが発生しているか否かを観察した。内部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
得られた接続構造体を、-65℃から150℃に加熱し、-65℃に冷却する過程を1サイクルとする冷熱サイクル試験を1000サイクル実施した。超音波探傷装置(SAT)により、接続部においてクラック及び剥離の発生の有無を観察した。冷熱サイクル特性(接続信頼性)を以下の基準で判定した。
○:接続部にクラック及び剥離なし
×:接続部にクラック又は剥離がある
得られた液晶表示素子を温度80℃、湿度90%RHの環境下にて72時間保管した後、AC3.5Vの電圧駆動をさせ、中間調のシール部周辺を目視で観察した。透湿性を下記の基準で判定した。
○:シール部周辺に色むらなし
△:シール部周辺に色むらがわずかに発生
×:シール部周辺に目立つ色むらが発生
1A…樹脂粒子
51…接続構造体
52…第1の接続対象部材
53…第2の接続対象部材
54…接続部
61…ギャップ制御粒子
62…金属接続部
81…液晶表示素子
82…透明ガラス基板
83…透明電極
84…配向膜
85…液晶
86…シール剤
Claims (10)
- シリコーン樹脂と、シリコーン樹脂とは異なる樹脂とを含む樹脂粒子であり、
前記シリコーン樹脂の外表面が前記シリコーン樹脂とは異なる樹脂により覆われた樹脂粒子であり、
前記シリコーン樹脂とは異なる樹脂の材料が、ジビニルベンゼン又はスチレンであり、
一般式:[(R)3SiO1/2]で表されるM単位、一般式:[(R)2SiO2/2]で表されるD単位、一般式:[(R)SiO3/2]で表されるT単位及び一般式:[SiO4/2]で表されるQ単位の合計の全個数100%中、前記T単位及び前記Q単位の合計の個数が、4%以下であり、
粒子径のCV値が、10%以下であり、
40%圧縮変形させた際の圧縮回復率が、10%以下である、樹脂粒子。 - 10%K値が、500N/mm2以下である、請求項1に記載の樹脂粒子。
- 粒子径が、0.5μm以上500μm以下である、請求項1又は2に記載の樹脂粒子。
- スペーサとして用いられる、請求項1~3のいずれか1項に記載の樹脂粒子。
- 請求項1~4のいずれか1項に記載の樹脂粒子と、
バインダー又は金属原子含有粒子とを含む、接続材料。 - バインダーを含む、請求項5に記載の接続材料。
- 金属原子含有粒子を含む、請求項5又は6に記載の接続材料。
- 前記樹脂粒子の熱分解温度が、前記金属原子含有粒子の融点よりも高い、請求項7に記載の接続材料。
- 2つの接続対象部材を接続する接続部を形成するために用いられ、
前記金属原子含有粒子の焼結体によって、前記接続部を形成するために用いられる、請求項7又は8に記載の接続材料。 - 第1の接続対象部材と、
第2の接続対象部材と、
前記第1の接続対象部材と、前記第2の接続対象部材とを接続している接続部とを備え、
前記接続部の材料が、請求項1~4のいずれか1項に記載の樹脂粒子を含む、接続構造体。
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WO2016088812A1 (ja) | 2014-12-04 | 2016-06-09 | 積水化学工業株式会社 | シリコーン粒子、液晶滴下工法用シール剤及び液晶表示素子 |
JP2016108563A (ja) | 2014-12-04 | 2016-06-20 | 積水化学工業株式会社 | 基材粒子、導電性粒子、導電材料及び接続構造体 |
WO2017082353A1 (ja) | 2015-11-11 | 2017-05-18 | 積水化学工業株式会社 | 粒子、粒子材料、接続材料及び接続構造体 |
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WO2018203500A1 (ja) | 2018-11-08 |
TWI838336B (zh) | 2024-04-11 |
KR102584161B1 (ko) | 2023-10-04 |
CN116675819A (zh) | 2023-09-01 |
CN110088160B (zh) | 2023-06-13 |
CN110088160A (zh) | 2019-08-02 |
KR20190139194A (ko) | 2019-12-17 |
TW201843214A (zh) | 2018-12-16 |
JPWO2018203500A1 (ja) | 2020-03-12 |
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