JP2010226093A - シリコーン樹脂で封止された光半導体装置 - Google Patents
シリコーン樹脂で封止された光半導体装置 Download PDFInfo
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- JP2010226093A JP2010226093A JP2010020606A JP2010020606A JP2010226093A JP 2010226093 A JP2010226093 A JP 2010226093A JP 2010020606 A JP2010020606 A JP 2010020606A JP 2010020606 A JP2010020606 A JP 2010020606A JP 2010226093 A JP2010226093 A JP 2010226093A
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Images
Classifications
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/42—Wire connectors; Manufacturing methods related thereto
- H01L24/47—Structure, shape, material or disposition of the wire connectors after the connecting process
- H01L24/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
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Abstract
【解決手段】光半導体素子10と、リード21a、21b、光半導体素子を載置するパッケージ20と、光半導体素子を封止するシリコーン樹脂組成物の硬化物30を備える光半導体装置であって、該硬化物の固体29Si−DD/MAS分析から求められる(ΦSiO3/2)単位(但しΦはフェニル基を表す)の量が、0.13モル/100g〜0.37モル/100gである、光半導体装置である。
【選択図】図3
Description
固体29Si−DD/MAS(Dipolar Decoupling/Magic Angle Spinning)は、核磁気共鳴装置(AVANCE700、ブルカー社製)を用い、固体試料(シリコーン硬化物)約100mgを外径4mmのジルコニア製ローターにつめ、9000Hzで回転させながら、30度パルスを30秒間隔で照射して、約1,000回積算して測定した。得られた29Si−DD/MASスペクトルの一例を図4に示す。こうして得られた29Si−DD/MASスペクトルから、試料を構成する全種のシロキサン単位の種類毎に含まれるケイ素原子の割合を、モル%で求めた。このケイ素原子の割合は当該種類のシロキサン単位の割合(モル%)と同じである。同様にして、すべての種類のシロキサン単位の割合(モル%)を求めた。次に、求めたおのおのの種類のシロキサン単位のモル%に、そのシロキサン単位の式量[例えばT−Φ単位であれば130(=29+77+16×3/2)]を乗じることにより、その種のシロキサン単位の質量基準の割合を求めた。次に、全種のシロキサン単位について求めた質量割合の和でT−Φ単位のモル%を除し、さらに100を乗じて、T−Φ単位量(モル/100g)を算出した。下表1に示すように、原料中の濃度からTΦ単位の理論量が既知の硬化物を4種類測定し、ほぼ理論量通りの結果が得られることが確認された。
R1 aR2 bR3 c(OX)dSiO(4−a−b−c−d)/2 (1)
(R1は独立にメチル基、エチル基、プロピル基又はシクロヘキシル基、好ましくはメチル基であり、R2はフェニル基であり、R3は脂肪族不飽和基であり、Xは水素原子または炭素原子数1〜6のアルキル基、但し(OX)はその酸素原子を介してケイ素に結合されており、aは0.4〜1.6、bは1.6〜3.6、cは0.4〜0.8、dは0〜0.05であり、0<a+b+c+d<4である。)
(A−2)下記式(2)で示される、25℃における粘度が10〜500,000mPa・sである直鎖状の両末端に脂肪族不飽和基を有するオルガノポリシロキサンからなる。
又は、脂肪族不飽和結合を含有する一価炭化水素基であるが、R8の少なくとも1個は式(5)の有機基である。〕
[合成例1](A−1)成分の合成
フェニルトリクロロシラン148.1g(70mol%)、およびジメチルビニルクロロシラン36.15g(30mol%)の混合物を、80℃に加熱した水250g及びトルエン100gの混合溶媒中に攪拌しながら1時間かけて滴下した。滴下終了後2時間還流させることにより共加水分解縮合物のトルエン溶液を得た。この溶液を静置して室温まで冷却し水層を除去した後、トルエン層の水洗の洗浄廃水が中性になるまで行った。得られたオルガノポリシロキサンのトルエン溶液(有機層1)にKOHを当量でクロル分の20倍量加え2時間還流した。反応後、トリメチルクロロシランで中和し、水洗をトルエン層が中性になるまで行なった(有機層2)。有機層2を、無水芒硝を用いて脱水した後、ろ過して不純物を除去した。得られたろ液からトルエンを除去(減圧下)し、固形状のレジン(以下、樹脂A−1aという)が得られた。
フェニルトリクロロシラン116.3g(55mol%)、ジメチルジクロロシラン19.35g(15mol%)およびメチルビニルジクロロシラン42.3g(30mol%)の混合物を、80℃に加熱した水250g及びトルエン100gの混合溶媒中に攪拌しながら1時間かけて滴下した。滴下終了後2時間還流させることにより共加水分解縮合物のトルエン溶液を得た。この溶液を静置して室温まで冷却し水層を除去した後、トルエン層の水洗の洗浄廃水が中性になるまで行った。得られたオルガノポリシロキサンのトルエン溶液(有機層1)にKOHを当量でクロル分の20倍量加え2時間還流した。反応後、トリメチルクロロシランで中和し、水洗をトルエン層が中性になるまで行なった(有機層2)。有機層2を、無水芒硝を用いて脱水した後、ろ過して不純物を除去した。得られたろ液からトルエンを除去(減圧下)し、固形状のレジン(以下、樹脂A−1bという)が得られた。
3−グリシドキシプロピルメチルジメトキシシラン(信越化学製、KBM−402)67.7g、ジメトキシジメチルシラン370g、ビニルメチルジメトキシシラン20g、イソプロピルアルコール3,000mlを仕込んだ後、水酸化テトラメチルアンモニウムの25%水溶液25g、水270gを添加し、室温で3時間攪拌した。反応終了後、系内にトルエン1,000mlいれ、リン酸二水素ナトリウム水溶液で中和した。分液漏斗を用いて、残渣を熱水にて洗浄した。減圧下トルエンを除去して目的の接着助剤を得た。
合成例2のビニル基含有樹脂(樹脂A−1b)23g、下記の(6)で示され、25℃での粘度が4,000mPa・sである直鎖状ビニルシロキサン70gと、
樹脂(A−1b)の量を31gに、上記の式(6)で示される直鎖状ビニルシロキサンの量を36gに、上記式(7)で示されるオルガノハイドロジェンシロキサンの量を14.1gに、それぞれ変えた以外は、比較例1と同様にして組成物1を得た。該組成物1を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、1.5であった。
樹脂(A−1b)の代わりに合成例1のビニル基含有樹脂(樹脂A−1a)100gを使用し、そして、上記の式(6)で示される直鎖状ビニルシロキサンの量を100gに、上記式(7)で示されるオルガノハイドロジェンシロキサンの量を79gに、それぞれ変えた以外は、比較例1と同様にして組成物2を得た。該組成物2を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、2.4であった。
樹脂(A−1b)の代わりに合成例1の樹脂(A−1a)60gを使用し、そして、上記の式(6)で示される直鎖状ビニルシロキサンの量を40gに、上記式(7)で示されるオルガノハイドロジェンシロキサンの量を32.4gに、上記式(8)で示されるオルガノハイドロジェンシロキサンの量を2.3gに変えた以外は、比較例1と同様にして組成物3を得た。該組成物3を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、1.7であった。
樹脂(A−1b)の代わりに合成例1の樹脂(A−1a)71.4gを使用し、そして、上記の式(6)で示される直鎖状ビニルシロキサンの量を30gに変更し、上記式(7)で示されるオルガノハイドロジェンシロキサンの量を43.2gに変更し、上記式(8)で示されるオルガノハイドロジェンシロキサンの量を1.5gに、それぞれ変えた以外は、比較例1と同様にして組成物4を得た。該組成物4を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、2.0であった。
樹脂(A−1b)の代わりに合成例1の樹脂(A−1a)76.9gを使用し、そして、上記の式(6)で示される直鎖状ビニルシロキサンの量を40gに、上記式(7)で示されるオルガノハイドロジェンシロキサンの量を34.44gに、上記式(8)で示されるオルガノハイドロジェンシロキサンの量を1.5gに、それぞれ変えた以外は、比較例1と同様にして組成物5を得た。該組成物5を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、1.5であった。
樹脂(A−1b)の代わりに合成例1の樹脂(A−1a)40.1gを使用し、そして上記の式(8)で示されるオルガノハイドロジェンシロキサンの量を15.2gに変更した以外は、比較例1と同様にして比較組成物2を得た。該比較組成物2を比較例1と同様に加熱して硬化物を得た。なお、上記オルガノハイドロジェンポリシロキサンのケイ素原子結合水素原子は、上記ビニル基含有樹脂及び直鎖状ビニルシロキサン中の脂肪族不飽和基に対して、モル基準で、1.2であった。
1)組成物の粘度(25℃)
BL型回転粘度計により測定した。
JIS K 6301に準拠し、引張強度(0.2mm厚)、硬度(タイプA型スプリング試験機を用いて測定)及び伸び率(0.2mm厚)を測定した。
核磁気共鳴装置(AVANCE700、ブルカー社製)を用い、硬化物から削り取った試料約100mgを外径4mmのジルコニア製ローターにつめ、9,000Hzで回転させながら、30度パルスを30秒間隔で照射して、約1,000回積算して固体29Si−DD/MAS測定を行なった。
リフロー炉に半導体装置を通過させてクラックの有無を調べるリフロー試験を行った。半導体装置のパッケージとして、型番NSSW108(日亜化学工業株式会社製)を使用した。パッケージの凹部内の、リードフレーム上に光半導体素子がダイボンド剤により載置されており、ワイヤによって電極に接続されている。該凹部に各組成物を注入し、150℃/4時間の条件で硬化して、光半導体素子及びワイヤを封止した。こうして得られた半導体装置10個を、最高温度260℃のIRリフロー炉を通した後に、クラックの発生を光学顕微鏡(倍率×10)にて観察した。表2において、○はクラックが認められなかったことを、×はクラックが認められたことを示す。
上記4)と同様に作製した10個の装置を、密閉容器内で25℃、H2Sガス0.1ppm雰囲気下で1ヶ月間保管したのち、光度を測定し、装置作成直後の光度を100%として光度の維持率を求めた。該維持率が高いほど、変色がないことを示す。
11 保護素子
20 パッケージ
21 リード
30 封止部材
40 ダイボンド部材
50 ワイヤ
60 蛍光物質
Claims (5)
- 光半導体素子と、該光半導体素子を封止するシリコーン樹脂組成物の硬化物を備える光半導体装置であって、該硬化物の固体29Si−DD/MAS分析から求められる(ΦSiO3/2)単位(但しΦはフェニル基を表す)の量が、0.13モル/100g〜0.37モル/100gである、光半導体装置。
- (ΦSiO3/2)単位(但しΦはフェニル基を表す)の量が、0.17モル/100g〜0.25モル/100gである、請求項1記載の光半導体装置。
- 前記光半導体素子が、発光ダイオードである、請求項1または2記載の光半導体装置。
- 前記シリコーン樹脂組成物が、
(A)(A−1)下記平均組成式(1):
R1 aR2 bR3 c(OX)dSiO(4−a−b−c−d)/2 (1)
(R1は独立にメチル基、エチル基、プロピル基又はシクロヘキシル基であり、R2はフェニル基であり、R3は脂肪族不飽和基であり、Xは水素原子または炭素原子数1〜6のアルキル基、但し(OX)はその酸素原子を介してケイ素に結合されており、aは0.4〜1.6、bは1.6〜3.6、cは0.4〜0.8、dは0〜0.05であり、0<a+b+c+d<4である。)
で表される脂肪族不飽和基含有シリコーンレジン、及び
(A−2)下記式(2):
で示される、25℃における粘度が10〜500,000mPa・sである直鎖状の両末端に脂肪族不飽和基を有するオルガノポリシロキサンからなる脂肪族不飽和基含有オルガノポリシロキサン、
(B)(B−1)下記式(3):
(R7は夫々に独立にメチル基、エチル基、プロピル基、シクロヘキシル基、又はフェニル基であり、p、qは、夫々、0〜100の整数、x及びyは独立に0、1、2又は3であり、但し、p+qが3以上であり、x+y+pは2以上の整数である。)
で示される、直鎖状のオルガノハイドロジェンポリシロキサン、及び、
(B−2)分岐状のオルガノハイドロジェンポリシロキサン
からなるオルガノハイドロジェンポリシロキサン、
(C)白金族金属系触媒
を含むものである請求項1に記載の光半導体装置。 - 前記組成物がさらに接着助剤を含む請求項4に記載の光半導体装置。
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