JP2006156964A5 - - Google Patents

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JP2006156964A5
JP2006156964A5 JP2005298384A JP2005298384A JP2006156964A5 JP 2006156964 A5 JP2006156964 A5 JP 2006156964A5 JP 2005298384 A JP2005298384 A JP 2005298384A JP 2005298384 A JP2005298384 A JP 2005298384A JP 2006156964 A5 JP2006156964 A5 JP 2006156964A5
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epoxy resin
sealant
molar amount
resin
bisphenol
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Priority claimed from US10/967,646 external-priority patent/US7381359B2/en
Priority claimed from US10/967,115 external-priority patent/US7311972B2/en
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光電子デバイス又は光学部品用の封止剤であって、熱膨張係数及び光透過率を特徴とする封止剤であって、
250μm未満の直径をもつガラス粒子から本質的になり、ガラス粒子1.48から1.60の範囲の値のガラス屈折率をもち、ホウケイ酸から本質的になり、かつ封止剤の全容積の10容量%から50容量%を構成することを特徴とする充填剤と、
硬化段階のエポキシ組成物の屈折率を特徴とする、硬化段階のエポキシ樹脂組成物を含む封止剤であって、
その際、封止剤の熱膨張係数が、50ppm/℃未満の平均値を有し、±30%未満のばらつきであり
ガラスの屈折率及び硬化段階のエポキシ樹脂組成物の屈折率が、封止剤の光透過率が400nmから900nmの範囲の波長で約1mmの封止剤厚さで測定した時に少なくとも20%になるように、十分に近似した値を有し、かつ
封止剤がエポキシ樹脂組成物を充填剤と混合して調製され、混合前のエポキシ樹脂組成物の粘度が300cPから40000cPの範囲の値を有し、かつエポキシ樹脂組成物が少なくとも1種の硬化剤、少なくとも1種の硬化促進剤、及びビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂、トリグリシジルイソシアヌレート樹脂からなる三元エポキシ混合物を含有する封止剤。
A sealant for an optoelectronic device or optical component, characterized by a thermal expansion coefficient and a light transmittance,
Consisting essentially of glass particles having a diameter of less than 250 μm, the glass particles having a glass refractive index in the range of 1.48 to 1.60 , consisting essentially of borosilicate, and all of the sealant A filler, characterized in that it comprises 10% to 50% by volume of the volume ;
A sealant comprising a curing stage epoxy resin composition, characterized by the refractive index of the curing stage epoxy composition,
At that time, the thermal expansion coefficient of the sealant has an average value of less than 50 ppm / ° C., and is a variation of less than ± 30% ,
The refractive index of the glass and the epoxy resin composition in the curing stage is at least 20% when the light transmittance of the sealant is measured at a sealant thickness of about 1 mm at a wavelength in the range of 400 nm to 900 nm. as described above, it has a value that is sufficiently approximate, and
A sealant is prepared by mixing an epoxy resin composition with a filler, the viscosity of the epoxy resin composition before mixing has a value in the range of 300 cP to 40000 cP, and the epoxy resin composition is at least one cured , sealants having free at least one curing accelerator, and bisphenol -A epoxy resin, alicyclic epoxy resin, a ternary epoxy mixture consisting triglycidyl isocyanurate resin.
封止剤の熱膨張係数が、±10%より小さいばらつきである請求項1に記載の封止剤。   The sealing agent according to claim 1, wherein the thermal expansion coefficient of the sealing agent has a variation smaller than ± 10%. 封止剤の熱膨張係数が、40ppm/℃未満の平均値を有する請求項1に記載の封止剤。   The sealant according to claim 1, wherein the sealant has an average coefficient of thermal expansion of less than 40 ppm / ° C. 封止剤の光透過率が、400nmから900nmの範囲の波長で約1mmの封止剤厚さで測定した時に少なくとも40%である請求項1に記載の封止剤。   The encapsulant of claim 1, wherein the encapsulant has a light transmittance of at least 40% when measured with a sealant thickness of about 1 mm at a wavelength in the range of 400 nm to 900 nm. 封止剤の光透過率が、400nmから900nmの範囲の波長で約1mmの封止剤厚さで測定した時に少なくとも60%である請求項1に記載の封止剤。   The encapsulant of claim 1, wherein the encapsulant has a light transmittance of at least 60% when measured at a sealant thickness of about 1 mm at a wavelength in the range of 400 nm to 900 nm. ガラス粒子が本質的にアルカリを含有しない請求項1に記載の封止剤。   The sealant according to claim 1, wherein the glass particles contain essentially no alkali. ガラス粒子が1μmから250μmの範囲の直径をもつ請求項1に記載の封止剤。   The sealant according to claim 1, wherein the glass particles have a diameter in the range of 1 μm to 250 μm. ガラス粒子が1μmから125μmの範囲の直径をもつ請求項1に記載の封止剤。   The sealant according to claim 1, wherein the glass particles have a diameter in the range of 1 μm to 125 μm. 60容量%未満の充填剤が、10μm未満の直径をもつガラス粒子を含む請求項1に記載の封止剤。   The sealant according to claim 1, wherein less than 60% by volume of the filler comprises glass particles having a diameter of less than 10 m. 20容量%未満の充填剤が、10μm未満の直径をもつガラス粒子を含む請求項1に記載の封止剤。   The sealant according to claim 1, wherein the filler of less than 20% by volume comprises glass particles having a diameter of less than 10 μm. 10容量%未満の充填剤が、10μm未満の直径をもつガラス粒子を含む請求項1に記載の封止剤。   The sealant according to claim 1, wherein less than 10% by volume of the filler comprises glass particles having a diameter of less than 10m. 充填剤が、封止剤の全容積の15から40容量%を構成する請求項1に記載の封止剤。   The sealant according to claim 1, wherein the filler constitutes 15 to 40% by volume of the total volume of the sealant. 充填剤が、熱処理温度で少なくとも約1時間熱処理されたガラス粒子を更に含み、熱処理温度がガラス粒子のひずみ点以下である請求項1に記載の封止剤。 The encapsulant of claim 1, wherein the filler further comprises glass particles that have been heat treated at a heat treatment temperature for at least about 1 hour, wherein the heat treatment temperature is below the strain point of the glass particles . 熱処理温度が、20℃とガラス粒子のひずみ点の間である請求項13に記載の封止剤。 The sealant according to claim 13 , wherein the heat treatment temperature is between 20 ° C. and the strain point of the glass particles . ガラス粒子が、熱処理温度で5時間から50時間、熱処理される請求項13に記載の封止剤。 The sealant according to claim 13 , wherein the glass particles are heat-treated at a heat treatment temperature for 5 to 50 hours. ガラス粒子が、熱処理温度で30時間から40時間、熱処理される請求項13に記載の封止剤。 The sealant according to claim 13 , wherein the glass particles are heat-treated at a heat treatment temperature for 30 to 40 hours. 充填剤が、アミノプロピルトリエトキシシラン、ビニルトリメトキシシラン、メタクリルオキシプロピルトリエトキシシラン、3−グリシドキシプロピルトリメトキシシラン、及びそれらの混合物からなる群から選ばれたシランカップリング剤と反応させたガラス粒子を更に含む請求項1に記載の封止剤。   The filler is reacted with a silane coupling agent selected from the group consisting of aminopropyltriethoxysilane, vinyltrimethoxysilane, methacryloxypropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, and mixtures thereof. The sealant according to claim 1, further comprising glass particles. シランカップリング剤が、アミノプロピルトリエトキシシラン、3−グリシドキシプロピルトリメトキシシラン、及びそれらの混合物からなる群から選ばれる請求項17に記載の封止剤。 The sealant according to claim 17 , wherein the silane coupling agent is selected from the group consisting of aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, and mixtures thereof. 硬化剤が、酸無水物硬化剤、フェノール硬化剤、及びそれらの混合物からなる群から選ばれる請求項に記載の封止剤。 Curing agent, acid anhydride curing agents, phenol curing agent, and encapsulating agent of claim 1 selected from the group consisting of mixtures thereof. 硬化剤が、無水フタル酸、無水マレイン酸、無水トリメリト酸、無水ピロメリト酸、無水ヘキサヒドロフタル酸、無水テトラヒドロフタル酸、無水メチルナデイック酸、無水ナデイック酸、無水グルタル酸、無水メチルヘキサヒドロフタル酸、無水メチルテトラヒドロフタル酸、及びフェノールノボラック樹脂硬化剤、及びそれらの混合物からなる群から選ばれる請求項に記載の封止剤。 The curing agent is phthalic anhydride, maleic anhydride, trimellitic anhydride, pyromellitic anhydride, hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methyl nadic anhydride, nadic anhydride, glutaric anhydride, methyl hexahydrophthalic anhydride. The sealant according to claim 1 , selected from the group consisting of acids, methyltetrahydrophthalic anhydride, phenol novolac resin curing agents, and mixtures thereof. 硬化剤が、無水フタル酸、無水ヘキサヒドロフタル酸、無水テトラヒドロフタル酸、無水メチルヘキサヒドロフタル酸、フェノールノボラック樹脂硬化剤、及びそれらの混合物からなる群から選ばれる請求項に記載の封止剤。 Curing agent, phthalic anhydride, hexahydrophthalic anhydride, tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, phenol novolak resin curing agent, and sealing of claim 1 selected from the group consisting of a mixture thereof Agent. 硬化剤が、無水ヘキサヒドロフタル酸である請求項に記載の封止剤。 Curing agent, sealing agent according to claim 1 which is hexahydrophthalic anhydride. 硬化促進剤が、1,8−ジアザビシクロ[5,4,0]ウンデセン−7、トリエチレンジアミン、第三級アミン、2−エチル−4−メチルイミダゾール、2−メチルイミダゾール、トリフェニルホスファイト、テトラフェニルホスホニウムテトラフェニルホウ酸、テトラ−n−ブチルホスホニウム、O,O−ヂエチルホスホロジチオエート、第四級アンモニウム塩、有機金属塩、及びそれらの混合物からなる群から選ばれる請求項に記載の封止剤。 The curing accelerator is 1,8-diazabicyclo [5,4,0] undecene-7, triethylenediamine, tertiary amine, 2-ethyl-4-methylimidazole, 2-methylimidazole, triphenyl phosphite, tetraphenyl phosphonium tetraphenyl borate, tetra -n- butyl phosphonium, O, O-diethyl phosphorodithioate, quaternary ammonium salts, organometallic salts, and according to claim 1 selected from the group consisting of a mixture thereof Sealant. 硬化促進剤が、トリフェニルホスファイト、2−エチル−4−メチルイミダゾール、及びそれらの混合物なる群から選ばれる請求項に記載の封止剤。 The sealant according to claim 1 , wherein the curing accelerator is selected from the group consisting of triphenyl phosphite, 2-ethyl-4-methylimidazole, and a mixture thereof. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するビスフェノール−Aエポキシ樹脂のモル量の比が、0.05から0.6の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the molar amount of the ratio of bisphenol -A epoxy resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 ranges from 0.05 to 0.6 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するビスフェノール−Aエポキシ樹脂のモル量の比が、0.15から0.40の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the molar amount of the ratio of bisphenol -A epoxy resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 ranges from 0.15 0.40 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する脂環式エポキシ樹脂のモル量の比が、0.05から0.70の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the ratio of the molar amount of the alicyclic epoxy resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 in the range of 0.05 0.70 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する脂環式エポキシ樹脂のモル量の比が、0.10から0.55の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the ratio of the molar amount of the alicyclic epoxy resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 ranges from 0.10 to 0.55 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するトリグリシジルイソシアヌレート樹脂のモル量の比が、0.05から0.70の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the molar amount of the ratio of the triglycidyl isocyanurate resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 in the range of 0.05 0.70 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するトリグリシジルイソシアヌレート樹脂のモル量の比が、0.20から0.65の範囲である請求項に記載の封止剤。 Bisphenol -A Epoxy resin, the molar amount of the ratio of the triglycidyl isocyanurate resin to the total molar amount of the alicyclic epoxy resins and triglycidyl isocyanurate resin, according to claim 1 ranges from 0.20 to 0.65 Sealant. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化剤のモル量の比が、0.50から1.20の範囲である請求項に記載の封止剤。 The sealing according to claim 1 , wherein the ratio of the molar amount of the curing agent to the total molar amount of the bisphenol-A epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin is in the range of 0.50 to 1.20. Agent. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化剤のモル量の比が、0.70から1.00の範囲である請求項に記載の封止剤。 The sealing according to claim 1 , wherein the ratio of the molar amount of the curing agent to the total molar amount of the bisphenol-A epoxy resin, the alicyclic epoxy resin and the triglycidyl isocyanurate resin is in the range of 0.70 to 1.00. Agent. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化促進剤のモル量の比が、0.001から0.050の範囲である請求項に記載の封止剤。 The sealing according to claim 1 , wherein the ratio of the molar amount of curing accelerator to the total molar amount of bisphenol-A epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin is in the range of 0.001 to 0.050. Stopper. ビスフェノール−Aエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化促進剤のモル量の比が、0.004から0.030の範囲である請求項に記載の封止剤。 The sealing according to claim 1 , wherein the ratio of the molar amount of curing accelerator to the total molar amount of bisphenol-A epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin is in the range of 0.004 to 0.030. Stopper. 請求項1に記載の封止剤に実質的に収納された光電子デバイスを含む組立品。   An assembly comprising an optoelectronic device substantially housed in the sealant of claim 1. 光電子デバイス又は光学部品用の封止剤であって、熱膨張係数及び光透過率を特徴とする封止剤であって、
(1)3−グリシドキシプロピルトリメトキシシランでシリル化され、アルカリを含有しないホウケイ酸ガラスから形成されたガラス粒子から本質的になる、15容量%から40重量%の充填剤であって、この粒子が1μmから250μmの範囲の直径を有し、その10容量%未満の粒子が10μm未満の直径を有し、このガラスが約1.526の値及び約0.001未満のばらつきのガラス屈折率を特徴とする充填剤、及び
(2)60容量%から85容量%の硬化段階のエポキシ樹脂組成物であって、ビスフェノール−Aのジグリシジルエーテル樹脂、脂環式エポキシ樹脂、トリグリシジルイソシアヌレート樹脂、硬化剤、及び硬化促進剤を含む組成物から製造されたエポキシ樹脂組成物であって、ビスフェノール−Aのジグリシジルエーテル樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するビスフェノール−Aのジグリシジルエーテル樹脂のモル量の比が、0.15から0.40の範囲の値を有し、ビスフェノール−Aのジグリシジルエーテルエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する脂環式エポキシ樹脂のモル量の比が、0.10から0.55であり、ビスフェノール−Aのジグリシジルエーテルエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対するトリグリシジルイソシアヌレート樹脂のモル量の比が、0.20から0.65であり、ビスフェノール−Aのジグリシジルエーテルエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化剤のモル量の比が0.70から1.00であり、ビスフェノール−Aのジグリシジルエーテルエポキシ樹脂、脂環式エポキシ樹脂及びトリグリシジルイソシアヌレート樹脂の総モル量に対する硬化促進剤のモル量の比が0.004から0.030である硬化段階のエポキシ樹脂組成物を含む封止剤であって、
その際、封止剤の熱膨張係数が、約40ppm/℃未満の平均値及び約±10%未満のばらつきであり、かつ封止剤の光透過率が、400nmから900nmの波長範囲で1mmの封止剤厚さで測定した時に、少なくとも20%であって、
充填剤がエポキシ樹脂組成物内に分散され、かつ
充填剤のエポキシ樹脂組成物内への分散前のエポキシ樹脂組成物の粘度が300cPから40000cPの範囲の値を有する封止剤。
A sealant for an optoelectronic device or optical component, characterized by a thermal expansion coefficient and a light transmittance,
(1) 15% to 40% by weight filler consisting essentially of glass particles silylated with 3-glycidoxypropyltrimethoxysilane and formed from an alkali-free borosilicate glass, The particles have a diameter in the range of 1 μm to 250 μm, less than 10% by volume of the particles have a diameter of less than 10 μm, and the glass has a glass refraction with a value of about 1.526 and a variation of less than about 0.001. And (2) an epoxy resin composition in a curing stage of 60% to 85% by volume, comprising a diglycidyl ether resin of bisphenol-A, an alicyclic epoxy resin, and triglycidyl isocyanurate An epoxy resin composition manufactured from a composition comprising a resin, a curing agent, and a curing accelerator, the diglycidyl ether of bisphenol-A The ratio of the molar amount of diglycidyl ether resin of bisphenol-A to the total molar amount of resin, cycloaliphatic epoxy resin and triglycidyl isocyanurate resin has a value in the range of 0.15 to 0.40, and bisphenol- The ratio of the molar amount of the alicyclic epoxy resin to the total molar amount of the diglycidyl ether epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin of A is 0.10 to 0.55, and the bisphenol-A The ratio of the molar amount of triglycidyl isocyanurate resin to the total molar amount of diglycidyl ether epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin is 0.20 to 0.65, and diglycidyl of bisphenol-A Ether epoxy resin, cycloaliphatic epoxy resin and triglycidyl Ratio of molar amount of curing agent to total molar amount of sosocyanurate resin is 0.70 to 1.00, and total molar amount of diglycidyl ether epoxy resin, alicyclic epoxy resin and triglycidyl isocyanurate resin of bisphenol-A A sealant comprising a curing stage epoxy resin composition wherein the ratio of the molar amount of curing accelerator to 0.004 to 0.030,
At that time, the thermal expansion coefficient of the encapsulant is an average value of less than about 40 ppm / ° C. and a variation of less than about ± 10%, and the light transmittance of the encapsulant is 1 mm in a wavelength range of 400 nm to 900 nm. when measured with an encapsulant thickness, I at least 20% der,
A filler is dispersed in the epoxy resin composition, and
Rufutomezai the viscosity of the epoxy resin composition before the dispersion into the epoxy resin composition of the filler have a value in the range of 40000cP from 300 cP.
JP2005298384A 2004-10-14 2005-10-13 Filled epoxy resin composition and method for producing the same Expired - Fee Related JP4570547B2 (en)

Applications Claiming Priority (2)

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US10/967,646 US7381359B2 (en) 2004-10-14 2004-10-14 Method for making filled epoxy resin compositions
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