JP6520872B2 - 半導体封止用熱硬化性樹脂組成物 - Google Patents
半導体封止用熱硬化性樹脂組成物 Download PDFInfo
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- JP6520872B2 JP6520872B2 JP2016170688A JP2016170688A JP6520872B2 JP 6520872 B2 JP6520872 B2 JP 6520872B2 JP 2016170688 A JP2016170688 A JP 2016170688A JP 2016170688 A JP2016170688 A JP 2016170688A JP 6520872 B2 JP6520872 B2 JP 6520872B2
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Description
下記(A)〜(E)成分を含む半導体封止用熱硬化性樹脂組成物。
(A)下記式(1)で表され、JIS K7117−1:1999記載の方法で、B型回転粘度計を用いて測定した23℃における粘度が50Pa・s以下であるシアネートエステル化合物を含む、1分子中に2個以上のシアナト基を有するシアネートエステル化合物
(C)硬化促進剤
(A)成分100質量部に対して0.01〜5質量部
(D)レーザー回折法で測定した平均粒径が1〜20μmの球状であり、下記式(7)で表されるシランカップリング剤で表面処理された無機質充填材
(E)下記式(12)で表されるエステル化合物
R4−CH2CH2−NH−CH2CH2−R5 (12)
(R4、R5は、炭素数2〜30の飽和エステル残基を示す)
(A)及び(B)成分の合計100質量部に対して1〜10質量部
前記(A)成分中、式(1)で表されるシアネートエステル化合物以外のシアネートエステル化合物が(A)成分全体の配合量に対して10質量%未満含まれる[1]に記載の半導体封止用熱硬化性樹脂組成物。
前記(B)成分において、式(6)で表されるレゾルシノール型フェノール樹脂が(B)成分全体の配合量に対して10質量%以上100質量%以下である[1]又は[2]に記載の半導体封止用熱硬化性樹脂組成物。
[4]
前記(B)成分のフェノール硬化剤中の水酸基1当量に対して(A)成分のシアネートエステル化合物中のシアナト基が0.5〜100当量である[1]〜[3]のいずれか1項に記載の半導体封止用熱硬化性樹脂組成物。
JIS K 7197:2012に記載の方法に基づいて、5×5×15mmの試験片を用いて、昇温速度5℃/分、荷重19.6mNで測定したときの線膨張係数が3.0〜5.0ppm/℃の範囲である[1]〜[4]のいずれか1項に記載の半導体封止用熱硬化性樹脂組成物。
1個以上の半導体素子を載置したシリコンウエハー又は基板全体を、半導体封止用熱硬化性樹脂組成物の硬化物で一括封止する工程を有する樹脂封止型半導体装置の製造方法であって、該工程が、[1]〜[5]に記載の半導体封止用熱硬化性樹脂組成物を押圧下に被覆するか、又は真空雰囲気下で減圧被覆し、該樹脂組成物を加熱硬化して半導体素子を封止することを特徴とする樹脂封止型半導体装置の製造方法。
[(A)シアネートエステル化合物]
(A)成分は、本発明の組成物の主成分であり、2個以上のシアナト基を有するシアネートエステル化合物であり、上記式(1)で表される化合物を含むものである。
(B)成分は、下記式(6)で表されるレゾルシノール型フェノール樹脂を含むフェノール硬化剤である。
(C)成分としては、1,8−ジアザビシクロ[5.4.0]ウンデセン−7(DBU)、1,5−ジアザビシクロ[4.3.0]ノネン−5(DBN)、これらのN−アルキル置換体、N−アリール置換体及びこれら含窒素複素環化合物の塩、並びにアミン系硬化促進剤等が挙げられる。(C)成分の硬化促進剤の配合量は、(A)成分100質量部に対して、5質量部以下が好ましく、0.01〜5質量部がより好ましい。
本発明の樹脂組成物に配合される無機質充填材は、エポキシ樹脂組成物に通常配合されるものを使用することができる。無機質充填材の具体例としては、例えば、溶融シリカ、結晶性シリカ等のシリカ類、アルミナ、窒化珪素、窒化アルミニウム、ボロンナイトライド、酸化チタン、ガラス繊維等が挙げられる。
本明細書において、「球状」とは、粒子の形状が、真球であるだけでなく、最長軸の長さ/最短軸の長さ(アスペクト比)が平均して、通常、1〜4、好ましくは1〜2、より好ましくは1〜1.6、更に好ましくは1〜1.4の範囲にある変形した球でもあることを意味する。粒子の形状は、該粒子を光学顕微鏡や電子顕微鏡にて観察することにより確認することができる。
(E)成分は、下記式(12)で表されるエステル化合物である。
R4−CH2CH2−NH−CH2CH2−R5 (12)
(R4、R5は、炭素数2〜30の飽和エステル残基を示す)
本発明の耐熱性樹脂組成物は、上記成分(A)〜(E)の所定量を配合することによって得られるが、その他の添加剤を必要に応じて本発明の目的、効果を損なわない範囲で添加することができる。かかる添加剤としては、無機充填材、難燃剤、イオントラップ剤、酸化防止剤、接着性付与剤、低応力剤、着色材等が挙げられる。
本発明の熱硬化性樹脂組成物は、例えば、以下に示されるような方法で調製することができる。まず、(A)シアネートエステル化合物と(B)フェノール硬化剤とを、同時に又は別々に、必要に応じて加熱処理を行いながら混合、撹拌及び/又は分散させることにより、(A)及び(B)成分の混合物を得る。(A)及び(B)成分の混合物に(C)硬化促進剤と(E)エステル化合物を混合、撹拌及び/又は分散させることにより、(A)〜(C)及び(E)成分の混合物を得る。そして、(A)〜(C)及び(E)成分の混合物に(D)無機質充填材を混合、撹拌及び/又は分散させることにより(A)〜(E)成分の混合物を得る。用途によって、(A)及び(B)成分の混合物、(A)〜(C)、及び(E)成分の混合物、(A)〜(E)成分の混合物に、難燃剤及びイオントラップ剤の添加剤のうち少なくとも1種を配合して混合してもよい。
熱硬化性樹脂組成物に含まれる以下に示す各成分を表1に示す割合で混合し、2本ロールで混錬することにより熱硬化性樹脂組成物を得た。表1中の配合比を示す数値の単位は「質量部」である。
(A1)下記式(17)で表わされる1,1−ビス(4−シアナトフェニル)エタン(粘度:0.08Pa・s)(商品名LECy、LOZNA(株)製)
(B1)下記式(19)で表わされるレゾルシノール型フェノール樹脂(n=0〜4、R1及びR2はアリル基、重量平均分子量450〜600、当量107)(商品名MEH−8400、明和化成株式会社製)
(B2)下記式(19)で表わされるレゾルシノール型フェノール樹脂(n=5〜7、R1及びR2はアリル基、重量平均分子量800〜1100、当量132)(明和化成株式会社製)
(C1)DBU系テトラフェニルボレート塩(商品名U−CAT 5002、サンアプロ社製)
(D1)処理シリカ
ベース球状溶融シリカ(平均粒径12μmの球状溶融シリカ(龍森製))100質量部に対して、0.3質量部のN−フェニル−3−アミノプロピルトリメトキシシラン(商品名KBM573、信越化学工業株式会社製)で乾式表面処理を行い、処理シリカ(D1)を調製した。
(D2)処理シリカ
ベース球状溶融シリカ(平均粒径12μmの球状溶融シリカ(龍森製))100質量部に対して、0.3質量部のγ−グリシドキシプロピルトリメトキシシラン(商品名KBM403、信越化学工業株式会社製)で乾式表面処理を行い、処理シリカ(D2)を調製した。
(D3)処理シリカ
ベース球状溶融シリカ(平均粒径0.8μmの球状シリカ(龍森製))100質量部に対して、0.3質量部のN−フェニル−3−アミノプロピルトリメトキシシラン(商品名KBM573、信越化学工業株式会社製)で乾式表面処理を行い、処理シリカ(D3)を調製した。
(D4)無処理シリカ
(D1)で用いた球状溶融シリカ(平均粒径12μm、龍森製)を表面処理することなく、無処理の状態で用いた。
(E1)下記式(20)で表わされるモンタン酸エステル化合物
C27H55−COO−CH2CH2−NH−CH2CH2−OOC−C27H55 (20)
(F1)接着性付与剤:γ−グリシドキシプロピルトリメトキシシラン(商品名KBM403、信越化学工業株式会社製)
(F2)着色材:カーボンブラック(商品名三菱カーン3230MJ、三菱化学製)
<ガラス転移温度及び線膨張係数>
JIS K 7197:2012に記載の方法に基づいて、実施例及び比較例において製造したシート状の硬化物を、5×5×15mmの試験片にそれぞれを加工した後、それらの試験片を熱膨張計TMA8140C(株式会社リガク社製)にセットした。そして、昇温速度5℃/分の加熱と、19.6mNの一定荷重とが試験片に加わるように設定し、25℃から300℃までの間で試験片の寸法変化を測定した。この寸法変化と温度との関係をグラフにプロットした。このようにして得られた寸法変化と温度とのグラフから、下記に説明するガラス転移温度の決定方法により、実施例及び比較例におけるガラス転移温度を求めた。
図1において、変曲点の温度以下で寸法変化−温度曲線の接線が得られる任意の温度2点をT1及びT2とし、変曲点の温度以上で同様の接線が得られる任意の温度2点をT1’及びT2’とした。T1及びT2における寸法変化をそれぞれD1及びD2として、点(T1、D1)と点(T2、D2)とを結ぶ直線と、T1’及びT2’における寸法変化をそれぞれD1’及びD2’として、点(T1’、D1’)と点(T2’、D2’)とを結ぶ直線との交点をガラス転移温度(Tg)とした。T1〜T2の傾きをTg以下の線膨張係数(線膨張係数1)、T1’〜T2’の傾きをTg以上の線膨張係数(線膨張係数2)とした。
シリコンウエハー12インチ/775μm厚を使用し、アピックヤマダ社製ウエハーモールドにて、熱硬化性樹脂組成物を175℃で600秒間、樹脂厚み500μmにコンプレッション成形後、180℃/1時間にて完全硬化(ポストキュアー)させた。その後、ウエハーの反り(mm)を測定した。
厚さ200μmの8インチシリコンウエハーに、厚膜スクリーン印刷機(THICK FILM PRINTER タイプMC212)を用いて、ダイボンド材SFX−513M1(信越化学工業株式会社製)を20μm厚に印刷し、Bステージ状態で7mm角大にダイシング装置を用いてダイシングして、半導体チップを準備した。
Claims (6)
- 下記(A)〜(E)成分を含む半導体封止用熱硬化性樹脂組成物。
(A)下記式(1)で表され、JIS K7117−1:1999記載の方法で、B型回転粘度計を用いて測定した23℃における粘度が50Pa・s以下であるシアネートエステル化合物を含む、1分子中に2個以上のシアナト基を有するシアネートエステル化合物
(C)硬化促進剤
(A)成分100質量部に対して0.01〜5質量部
(D)レーザー回折法で測定した平均粒径が1〜20μmの球状であり、下記式(7)で表されるシランカップリング剤で表面処理された無機質充填材
(E)下記式(12)で表されるエステル化合物
R4−CH2CH2−NH−CH2CH2−R5 (12)
(R4、R5は、炭素数2〜30の飽和エステル残基を示す)
(A)及び(B)成分の合計100質量部に対して1〜10質量部 - 前記(A)成分中、式(1)で表されるシアネートエステル化合物以外のシアネートエステル化合物が(A)成分全体の配合量に対して10質量%未満含まれる請求項1に記載の半導体封止用熱硬化性樹脂組成物。
- 前記(B)成分において、式(6)で表されるレゾルシノール型フェノール樹脂が(B)成分全体の配合量に対して10質量%以上100質量%以下である請求項1又は2に記載の半導体封止用熱硬化性樹脂組成物。
- 前記(B)成分のフェノール硬化剤中の水酸基1当量に対して(A)成分のシアネートエステル化合物中のシアナト基が0.5〜100当量である請求項1〜3のいずれか1項に記載の半導体封止用熱硬化性樹脂組成物。
- JIS K 7197:2012に記載の方法に基づいて、5×5×15mmの試験片を用いて、昇温速度5℃/分、荷重19.6mNで測定したときの線膨張係数が3.0〜5.0ppm/℃の範囲である請求項1〜4のいずれか1項に記載の半導体封止用熱硬化性樹脂組成物。
- 1個以上の半導体素子を載置したシリコンウエハー又は基板全体を、半導体封止用熱硬化性樹脂組成物の硬化物で一括封止する工程を有する樹脂封止型半導体装置の製造方法であって、該工程が、請求項1〜5に記載の半導体封止用熱硬化性樹脂組成物を押圧下に被覆するか、又は真空雰囲気下で減圧被覆し、該樹脂組成物を加熱硬化して半導体素子を封止することを特徴とする樹脂封止型半導体装置の製造方法。
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