TWI389925B - Optoelectronic semiconductors - Google Patents
Optoelectronic semiconductors Download PDFInfo
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- TWI389925B TWI389925B TW094139299A TW94139299A TWI389925B TW I389925 B TWI389925 B TW I389925B TW 094139299 A TW094139299 A TW 094139299A TW 94139299 A TW94139299 A TW 94139299A TW I389925 B TWI389925 B TW I389925B
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- Taiwan
- Prior art keywords
- methacrylate
- acrylate
- light
- sealing material
- manufactured
- Prior art date
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- 239000004065 semiconductor Substances 0.000 title claims description 45
- 230000005693 optoelectronics Effects 0.000 title claims description 25
- 239000003566 sealing material Substances 0.000 claims description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
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- 238000010526 radical polymerization reaction Methods 0.000 claims description 8
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- -1 polyoxymethylene Polymers 0.000 description 39
- 239000000126 substance Substances 0.000 description 19
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- 125000002723 alicyclic group Chemical group 0.000 description 18
- 238000011156 evaluation Methods 0.000 description 18
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- 229940044192 2-hydroxyethyl methacrylate Drugs 0.000 description 2
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- DGUJJOYLOCXENZ-UHFFFAOYSA-N 4-[2-[4-(oxiran-2-ylmethoxy)phenyl]propan-2-yl]phenol Chemical compound C=1C=C(OCC2OC2)C=CC=1C(C)(C)C1=CC=C(O)C=C1 DGUJJOYLOCXENZ-UHFFFAOYSA-N 0.000 description 2
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- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 125000004216 fluoromethyl group Chemical group [H]C([H])(F)* 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
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- IQRVNLYKJBNWHE-UHFFFAOYSA-N heptan-2-yl prop-2-enoate Chemical compound CCCCCC(C)OC(=O)C=C IQRVNLYKJBNWHE-UHFFFAOYSA-N 0.000 description 1
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- 125000001867 hydroperoxy group Chemical group [*]OO[H] 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- ITUWQZXQRZLLCR-UHFFFAOYSA-N n,n-dioctadecylhydroxylamine Chemical compound CCCCCCCCCCCCCCCCCCN(O)CCCCCCCCCCCCCCCCCC ITUWQZXQRZLLCR-UHFFFAOYSA-N 0.000 description 1
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- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
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- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 description 1
- 229940065472 octyl acrylate Drugs 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- QSYOAKOOQMVVTO-UHFFFAOYSA-N pentan-2-yl 2-methylprop-2-enoate Chemical compound CCCC(C)OC(=O)C(C)=C QSYOAKOOQMVVTO-UHFFFAOYSA-N 0.000 description 1
- RNGPDYJPLDLVJI-UHFFFAOYSA-N pentan-2-yl prop-2-enoate Chemical compound CCCC(C)OC(=O)C=C RNGPDYJPLDLVJI-UHFFFAOYSA-N 0.000 description 1
- QONHNMFEHWGACQ-UHFFFAOYSA-N pentan-3-yl prop-2-enoate Chemical compound CCC(CC)OC(=O)C=C QONHNMFEHWGACQ-UHFFFAOYSA-N 0.000 description 1
- GYDSPAVLTMAXHT-UHFFFAOYSA-N pentyl 2-methylprop-2-enoate Chemical compound CCCCCOC(=O)C(C)=C GYDSPAVLTMAXHT-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920002098 polyfluorene Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 1
- QTECDUFMBMSHKR-UHFFFAOYSA-N prop-2-enyl prop-2-enoate Chemical compound C=CCOC(=O)C=C QTECDUFMBMSHKR-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000006057 reforming reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- FQZYTYWMLGAPFJ-OQKDUQJOSA-N tamoxifen citrate Chemical compound [H+].[H+].[H+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.C=1C=CC=CC=1C(/CC)=C(C=1C=CC(OCCN(C)C)=CC=1)/C1=CC=CC=C1 FQZYTYWMLGAPFJ-OQKDUQJOSA-N 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- 235000019149 tocopherols Nutrition 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
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- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C08F220/10—Esters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
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Description
本發明係關於光電半導體裝置(半導體發光裝置)中發光元件或受光元件等的封閉材料及光電變換元件與光電變換裝置。詳細言之,為關於對紫外光安定、不會變黃,而且除了能賦予對耐熱性,折射率均衡性優異的硬化物之外,在加工性亦優異的光電半導體用透明封閉材料,及使用該等光電變換元件與光電變換裝置。
習知,光電半導體裝置(半導體發光裝置),具備以在結晶基板上成長的半導體層形成p-n結合,該接合區域中為發光層之LED(發光二極體)晶片之作為發光元件的光電半導體裝置,在各種顯示器裝置、顯示用機器等廣泛地被運用。
該光電半導體裝置的例子方面,有例如,使用GaN,GaAIN,InGaN及InAIGaN等的氮化鎵系化合物半導體之可視光發光裝置,或高溫動作電子裝置,最近,在藍色發光二極體、紫外發光二極體的領域正進行開發中。
具備作為LED晶片之發光元件的光電半導體裝置,係在引導框架(lead frame)的發光面側搭載LED晶片,LED晶片與引導框架(lead frame)藉由連線銲接(wire bonding)進行電性連接,進而,以兼具發光元件的保護及透鏡機能的樹脂予以封閉。
近年,作為新光源的白色LED被注意到了,今後,據稱將會擴大以照明用途為中心之廣大的市場。白色LED係在GaN的裸晶片(bare chip)上塗佈YAG螢光體,將GaN的藍色發光與螢光體的黃色發光混色,使呈白色發光的型態與使紅藍綠3晶片成為1封裝體化,呈白色發光的型態實用化。又,近年,由於色調的改良,以紫外LED晶片為光源,組合多種螢光體材料的方法亦被開發。進而,使用於照明用途等的LED,其耐久性的改良被尋求著
另一方面,封閉LED(發光二極體)晶片等的發光元件時所使用的封閉材料方面,大多利用環氧基樹脂。環氧基樹脂由於透明,加工性良好等因素而被利用。一般LED封閉用的環氧基樹脂幾乎為雙酚A環氧丙基醚與甲基六氫酞酸酐、胺系或者磷系等的硬化促進劑所成者。但是,該等成分會因紫外光的吸收而產生羰基,故有吸收可視光而變黃的缺點。為了解決該等問題,使用氫化雙酚A環氧丙基醚的方法(非專利文獻1)被提案,但是完全沒有提及性能。
為了改良因紫外光而變黃或亮度的降低,廣泛地運用了聚矽氧樹脂。聚矽氧樹脂在紫外領域中,透明性優異,因紫外光而變黃或透過率降低的情形極少。但是,聚矽氧樹脂因折射率低,光擷取的效率低或極性低,有與引導框架(lead frame)或反射器的密接性變差的問題。
又,表面組裝型的LED中,以回流銲接(reflow soldering)的方式進行銲錫。在回流爐內,因以260℃的
熱曝光約10秒,習知的環氧基樹脂或聚矽氧樹脂因熱而產生變形、破裂。
非專利文獻1:NEDO「高效率電光變換化合物半導體開發 成果報告 平成13年度21世紀的照明計畫」
本發明鑑於如上述的狀況,以提供對紫外光安定、不會變黃,而且除了賦予耐熱性、折射率均衡性之優異的硬化物之外,在黏接性或加工性亦優異的光電半導體用透明封閉材料及光電變換元件與光電變換裝置為目的。
本發明人等為了達成該目的,一再重覆戮力研究的結果,藉由使用碳數7以上的含脂環式烴基之甲基丙烯酸酯予以自由基聚合而成的聚合物,所得為折射率或加工性優異的光電半導體用封閉材料,又含有該含脂環式烴基之甲基丙烯酸酯與含羥基丙烯酸酯的熱硬化性樹脂組成物,除了黏接性或加工性優異之外,對紫外光安定,也不會變黃,而且為能賦予耐熱性,折射率均衡性之優異的硬化物,進而首先發現所得為優異的光電半導體用封閉材料,本發明係根據斯等真知灼見而完成者。
亦即,本發明係為提供以下的光電半導體封閉材料、光電變換元件及光電變換裝置者。
(1)含有碳數7以上之含脂環式烴基之甲基丙烯酸酯予以自由基聚合所成的聚合物為其特徵之光電半導體封閉材料。
(2)進而含有熱塑性樹脂0.5~20質量%之(1)的光電半導體封閉材料。
(3)碳數7以上的脂環式烴基為含有金剛烷基,降基或二環戊基之基的(1)或(2)的光電半導體封閉材料。
(4)含有碳數7以上的含脂環式烴基之甲基丙烯酸酯50~97質量%,與含羥基之丙烯酸酯3~50質量%予以自由基聚合所成之聚合物為其特徵之光電半導體封閉材料。
(5)碳數7以上的脂環式烴基為含有金剛烷基,降基或二環戊基之基之(4)的任一項之光電半導體封閉材料。
(6)使用(1)~(5)中任一項記載的光電半導體封閉材料為特徵之光電變換元件。
(7)使用(6)的光電變換元件為其特徵之光電變換裝置。
首先,本發明的光電半導體封閉材料為含有碳數7以上的含脂環式烴基之甲基丙烯酸酯予以自由基聚合所成之聚合物者。
碳數7以上的脂環式烴基方面,可以例舉2-十氫萘基、金剛烷基、1-甲基金剛烷基、2-甲基金剛烷基、雙金剛烷基、二甲基金剛烷基、降基、1-甲基-降基
、5,6-二甲基-降基、異基(isobornyl)基、四環[4.4.0.12,5
.17,10
]十二基、9-甲基-四環[4.4.0.12,5
.17,10
]十二基、基、二環戊基等,以金剛烷基、降基及二環戊基為佳。其中以金剛烷基為更佳,1-金剛烷基為特佳。本發明的光電半導體封閉材料所使用之單體方面,係使用具有該等脂環式烴基之甲基丙烯酸酯。脂環式烴基的碳數若不足7,耐熱性、折射率大多變得不完全。又,在該甲基丙烯酸酯的酯取代基含有芳香族等時,容易因紫外線而產生劣化。
本發明的光電半導體封閉材料所含有的含脂環式烴基甲基丙烯酸酯的自由基聚合物,可於前述碳數7以上的含脂環式羥基之甲基丙烯酸酯之單獨聚合物,亦可將該酯以2種以上之組合聚合所成之共聚合物中。或亦可於碳數7以上的含脂環式羥基之甲基丙烯酸酯1種以上與為共聚單體以外的(甲基)丙烯酸酯1種以上聚合所成的共聚合物中。其他的(甲基)丙烯酸酯方面,例如可以例舉甲基丙烯酸酯、氟甲基丙烯酸酯、乙基丙烯酸酯、丁基丙烯酸酯、異丁基丙烯酸酯、三級丁基丙烯酸酯、2,2,2-三氟乙基丙烯酸酯、2-羥基乙基丙烯酸酯、1,2,2,2-四氯乙基丙烯酸酯、丙基丙烯酸酯、異丙基丙烯酸酯、2-氯-1-(氯二氟甲基)乙基丙烯酸酯、1,2,2,2-四氟-1-(三氟甲基)乙基丙烯酸酯、2,2,2-三氟-1-(三氟甲基)乙基丙烯酸酯、2,2,3,3,3-五氟丙基丙烯酸酯、1-甲基乙基丙烯酸酯、2-(甲基硫)乙基丙烯酸酯、2-甲氧基
乙基丙烯酸酯、2-羥基丙基丙烯酸酯、2-丙烯基丙烯酸酯、1-乙氧基-2,2,2-三氟乙基丙烯酸酯、2-(乙基硫代)乙基丙烯酸酯、2-乙氧基乙基丙烯酸酯、2,2,3,3,4,4,4-七氟丁基丙烯酸酯、3-(甲基硫代)丙基丙烯酸酯、1-甲基丙基丙烯酸酯、2,2,3,4,4,4-六氟丁基丙烯酸酯、4-氧戊基丙烯酸酯、2-(三氟乙氧基)乙基丙烯酸酯、2-(1,1,2,2-四氟乙氧基)乙基丙烯酸酯、3-(乙基硫代)丙基丙烯酸酯、1-乙基丙基丙烯酸酯、2,2,3,3,4,4,5,5-八氟戊基丙烯酸酯、2,2-二甲基丙基丙烯酸酯、2,2,3,3,4,4,5,5,5-九氟戊基丙烯酸酯、4-甲基硫代丁基丙烯酸酯,2-甲基丁基丙烯酸酯、3-甲基丁基丙烯酸酯、4-氧己基丙烯酸酯、3-甲氧基丁基丙烯酸酯、己基丙烯酸酯、環己基丙烯酸酯、2-乙基丁基丙烯酸酯、2-甲基戊基丙烯酸酯、4-甲基-2-戊基丙烯酸酯、苯基丙烯酸酯、2-氯苯基丙烯酸酯、4-氯苯基丙烯酸酯、2,4-二氯苯基丙烯酸酯、五氯丙烯酸酯、3,3,4,4,5,5,6,6,6-十一氟丙烯酸酯、五氟丙烯酸酯、庚基丙烯酸酯、苯基甲基丙烯酸酯、2-甲基苯基丙烯酸酯、3-甲基苯基丙烯酸酯、4-甲基苯基丙烯酸酯、1-甲基己基丙烯酸酯、4-甲氧基苯基丙烯酸酯、辛基丙烯酸酯、2-苯基乙基丙烯酸酯、1-甲基丁基丙烯酸酯、壬基丙烯酸酯、癸基丙烯酸酯等的丙烯酸酯或甲基甲基丙烯酸酯、乙基甲基丙烯酸酯、2-氯乙基甲基丙烯酸酯、2,2,2-三氟乙基甲基丙烯酸酯、2-硝基乙基甲基丙烯酸酯、2
-羥基乙基甲基丙烯酸酯、丙基甲基丙烯酸酯、異丙基甲基丙烯酸酯、2-甲氧基乙基甲基丙烯酸酯、烯丙基甲基丙烯酸酯、環氧丙基甲基丙烯酸酯、2-氯丙基甲基丙烯酸酯、三甲基單矽烷基甲基丙烯酸酯、2,2,2-三氟-1-甲基乙基甲基丙烯酸酯、2,2,3,3-四氟丙基甲基丙烯酸酯、七氟異丙基甲基丙烯酸酯、六氟異丙基甲基丙烯酸酯、丁基甲基丙烯酸酯、異丁基甲基丙烯酸酯、二級丁基甲基丙烯酸酯、三級丁基甲基丙烯酸酯、2-乙氧基乙基甲基丙烯酸酯、二乙二醇甲基丙烯酸酯、九氟-三級丁基甲基丙烯酸酯、2,2,3,3,4,4,4-七氟丁基甲基丙烯酸酯、戊基甲基丙烯酸酯、環戊基甲基丙烯酸酯、2,2-二乙基丙基甲基丙烯酸酯、1-甲基丁基甲基丙烯酸酯、異戊基甲基丙烯酸酯、2,2,3,3,4,4,5,6-八氟戊基甲基丙烯酸酯、己基甲基丙烯酸酯、環己基甲基丙烯酸酯、苯基甲基丙烯酸酯、3,3-二甲基丁基甲基丙烯酸酯、2-乙基丁基甲基丙烯酸酯、1-甲基環己基甲基丙烯酸酯、2-甲基環己基甲基丙烯酸酯、3-甲基環己基甲基丙烯酸酯、4-甲基環己基甲基丙烯酸酯、1,1-二乙基丙基甲基丙烯酸酯、2-甲基苯基甲基丙烯酸酯、3-甲基苯基甲基丙烯酸酯、4-甲基苯基甲基丙烯酸酯、苄基甲基丙烯酸酯、2-甲氧基苯基甲基丙烯酸酯、2,2,3,3,4,4,5,5,6,6,7,7-十二氟庚基甲基丙烯酸酯、辛基甲基丙烯酸酯、2-乙基己基甲基丙烯酸酯、2-苯基乙基甲基丙烯酸酯、2,4-二甲基苯基甲基丙烯酸酯、2,5-二甲基苯基甲基丙烯酸酯、2,6-二甲基
苯基甲基丙烯酸酯、3,5-二甲基苯基甲基丙烯酸酯、壬基甲基丙烯酸酯、癸基甲基丙烯酸酯、異癸基甲基丙烯酸酯等的甲基丙烯酸酯。
但是,共聚單體方面,使用含有芳香環之(甲基)丙烯酸酯並不佳。又,聚合物中共聚單體單位的含量以50莫耳%以下為佳,更佳為30莫耳%以下。若超過50莫耳%,折射率或耐熱性,耐光性的均衡性會惡化。
此外,上述脂環式烴基所含有的三級碳數以8以下為佳,更佳為5以下。酯部分所含有的三級碳數若超過8以上,易有變黃的情形
本發明的光電半導體封閉材料中,自由基聚合所使用之自由基聚合引發劑方面,可以例舉甲基乙基酮過氧化物、甲基異丁基酮過氧化物、乙醯基丙酮過氧化物、環己酮過氧化物、甲基環己酮過氧化物等的酮過氧化物類、1,1,3,3-四甲基丁基氫過氧化物、氫過氧化物、三級丁基氫過氧化物等的氫過氧化物類、二異丁醯基過氧化物、雙-3,5,5-三甲基己醇過氧化物、月桂醯基過氧化物、苯醯基過氧化物,間甲苯甲醯基苯醯基過氧化物等的二醯基過氧化物類、二基過氧化物、2,5-二甲基-2,5-二(三級丁基過氧)己烷、1,3-雙(三級丁基過氧異丙基)己烷、三級丁基基過氧化物、二-三級丁基過氧化物、2,5-二甲基-2,5-二(三級丁基過氧)己烯等的二烷基過氧化物類、1,1-二(三級丁基過氧-3,5,5-三甲基)環己烷、1,1-二-三級丁基過氧環己烷、2,2-二(三
級丁基過氧)丁烷等的過氧縮酮類、1,1,3,3-四甲基丁基過氧新二碳酸酯、α-基過氧新二碳酸酯、三級丁基過氧新二碳酸酯、三級己基過氧三甲基乙酸酯、三級丁基過氧三甲基乙酸酯、1,1,3,3-四甲基丁基過氧-2-乙基己酸酯、三級戊基過氧-2-乙基己酸酯、三級丁基過氧-2-乙基己酸酯、三級丁基過氧異丁酸酯、二-三級丁基過氧六氫對酞酸酯、1,1,3,3-四甲基丁基過氧-3,5,5-三甲基己酸酯(hexanate)、三級戊基過氧3,5,5-三甲基己酸酯、三級丁基過氧3,5,5-三甲基己酸酯、三級丁基過氧乙酸酯、三級丁基過氧苯甲酸酯、二丁基過氧三甲基己二酸酯等的烷基過酯類(perester)、二-3-甲氧基丁基過氧二碳酸酯、二-2-乙基己基過氧二碳酸酯、雙(1,1-丁基環己氧二碳酸酯)、二異丙基氧二碳酸酯、三級戊基過氧異丙基碳酸酯、三級丁基過氧異丙基碳酸酯、三級丁基過氧-2-乙基己基碳酸酯、1,6-雙(三級丁基過氧羧基)己烷等的過氧碳酸酯類等。
自由基聚合引發劑的使用量,相對於該單體全量100質量份,通常為0.01~5質量份,更佳為0.05~1.0質量份。上述自由基聚合引發劑可各自單獨使用,又複數併用亦無妨。
除了上述的自由基聚合引發劑之外,為了能夠獲得高強度,亦可使用交聯性單體。交聯性單體方面,可以例舉1,4-丁烷二醇(甲基)丙烯酸酯、1,6-己烷二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、新戊
基二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、氧化伸乙基變性雙酚A二(甲基)丙烯酸酯、環氧丙烷變性雙酚A二(甲基)丙烯酸酯、表氯醇變性雙酚A二(甲基)丙烯酸酯、環氧丙烷變性甘油三(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、二三羥甲基丙烷四(甲基)丙烯酸酯、二新戊四醇六(甲基)丙烯酸酯、三(丙烯醯氧乙基)三聚異氰酸酯等。該等的交聯性單體,可以單獨使用,也可以使用2種以上的組合。交聯性單體的含量,在全單體中,較佳為0.1~80質量%。更佳為1~70質量%,再更佳為2~50質量%。交聯性單體若比0.1質量%少,無法獲得因交聯而產生的高強度化效果。
在本發明的光電半導體封閉材料中,為了提高耐熱性,亦可含有熱塑性樹脂。該熱塑性樹脂方面,以透明性高,玻璃轉移溫度在120℃以上之物較佳。玻璃轉移溫度若比120℃低時,耐熱性的提高效果會變小。
此種熱塑性樹脂方面,可以例舉聚甲基丙烯酸酯、聚苯乙烯、聚碳酸酯、聚芳基酯、聚醚碸、環氧基丙烯酸酯、烯烴-順丁烯二醯亞胺共聚合物、ZEONEX(日本Zeon公司製,環烯烴系聚合物)、ZEONOR(日本Zeon公司製,環烯烴系聚合物)、ARTON(JSR公司製,環烯烴系聚合物)、TOPAS(Ticona公司製,環烯烴系聚合物)、透明ABS、透明丙烯、MS(甲基丙烯酸苯乙烯)樹脂、聚芳基化物、聚碸、透明耐綸、透明聚對苯二甲酸丁二醇
酯(PBT)、透明氟樹脂、聚-4-甲基戊烯-1,透明苯氧基樹脂等。
該等熱塑性樹脂可以使用2種以上的組合。熱塑性樹脂於半導體封閉材料中,以含有0.5~20質量%為佳。以熱塑性樹脂在0.5質量%以上,可以獲得耐熱性提高的效果,以在20質量%以下,可成為流動性優異之物。
又,本發明的光電半導體封閉材料方面,可恰當使用含有碳數7以上的含脂環式烴基之甲基丙烯酸酯與含有丙烯酸酯之羥基,自由基聚合所成的聚合物者。
本發明的光電半導體封閉材料所使用之含羥基丙烯酸酯方面,例如可以例舉2-羥基乙基甲基丙烯酸酯、2-羥基丙基甲基丙烯酸酯、2-羥基乙基丙烯酸酯、2-羥基丙基丙烯酸酯、2-羥基丁基甲基丙烯酸酯、甘油二甲基丙烯酸酯、2-羥基-3-丙烯醯氧丙基甲基丙烯酸酯、2-羥基丁基丙烯酸酯、2-羥基-3-苯氧基丙基丙烯酸酯、2-羥基-3-丙烯醯氧丙基丙烯酸酯、2-羥基-3-苯氧基丙基丙烯酸酯、六氫酞酸二環氧丙基酯的丙烯酸變性物、乙二醇二環氧丙基醚的甲基丙烯酸變性物、聚乙二醇環氧丙基醚的甲基丙烯酸變性物、二乙二醇二環氧丙基醚的甲基丙烯酸變性物、1,4-丁烷二醇二環氧丙基醚二丙烯酸酯等。該等中,特別以六氫酞酸二環氧丙基酯的丙烯酸變性物、乙二醇二甘胺醯醚的甲基丙烯酸變性物、聚乙二醇環氧丙基醚的甲基丙烯酸變性物、二乙二醇二環氧丙基醚的甲基丙烯酸變性物、1,4-丁烷二醇二環氧丙基醚
二丙烯酸酯為佳。
此種本發明的光電半導體封閉材料中,碳數7以上的含脂環式羥基之甲基丙烯酸酯與含羥基之丙烯酸酯的組合中,碳數7以上的含脂環式羥基之甲基丙烯酸酯的含量為50~97質量%,較佳為60~95質量%,含羥基之丙烯酸酯的含量為3~50質量%,較佳為5~40質量%。碳數7以上的含脂環式羥基之甲基丙烯酸酯與含羥基之丙烯酸酯的含量,在此種範圍內,對紫外線安定、也不會變黃,而且能成為賦予在耐熱性,黏接性的均衡性優異之硬化物的熱硬化性樹脂組成物。
上述熱硬化性樹脂組成物,對於塑膠成形品顯示出十分高的黏接性,亦可恰當使用黏接劑,預先在塑膠成形品的表面以紫外線照射處理、臭氧處理、電漿處理、電暈放電處理、高壓放電處理等的方法活性化處理,更能提高黏接性。
此外,本發明中熱硬化性樹脂組成物僅指以熱聚合之樹脂組成物者。聚合後所得之樹脂未必具有3次元交聯構造,亦可為直鏈酚狀樹脂。又,非不溶不融也可,熱塑性亦可。
紫外線照射處理係為在空氣中於塑膠成形品的表面照射紫外線的方法。照射紫外線的光源方面,可以使用低壓水銀燈、高壓水銀燈、超高壓水銀燈、氙照射燈、金屬鹵素照射燈等。藉由紫外線照射,塑膠內產生了自由基,進而產生來自空氣中的氧而致之活性氧,於兩者反應後之成
形品表面,導入極性基(-COOH,-COH,-C=O等)。其結果,可知提高了黏接性。在塑膠成形品所照射之紫外線的能量依據塑膠種類、形狀、照射燈的種類而有所不同,但是為了使與本發明的熱硬化性樹脂組成物之黏接性提高,以10~20000 mJ/cm2
的範圍,更佳為100~10000 mJ/cm2
。照射能量若超過20000 mJ/cm2
時,塑膠成形品的表面會劣化。若不足10 mJ/cm2
時,因為能量不完全,無法獲得充分的黏接力。照射能量依照成形品與照射燈的距離及照射時間而控制。例如,成形品與照射燈的距離在1~50 cm左右,更佳為5~30 cm的範圍。照射時間為5秒~10分左右,較佳為10秒~5分左右。成形品與照射燈的距離若不足1 cm或超過50 cm,照射時間不足5秒或超過10分時,照射能量將無法控制在10~20000 mJ/cm2
。
臭氧處理係使塑膠成形品的表面與臭氧分子接觸,進行以氧化反應為主之改質反應為目的。臭氧處理係藉由將塑膠成形品暴露於臭氧中而進行。暴露方法為在臭氧存在的氛圍下,保持設定時間的方法,在臭氧氣流中可以藉由保持設定時間的方法等適宜的方法進行。臭氧藉由在臭氧發生裝置供給空氣,氧氣體或氧添加空氣等的含有氧的氣體可以使其產生。將所得之含臭氧氣體,導入保持塑膠成形品之容器、槽等,可以進行臭氧處理。藉由臭氧處理在塑膠成形品的表面進行以氧化為主之反應,使氫過氧基等導入,可以推斷其一部份之羥基或羰基等的官能基產生變
化。
電漿處理係將塑膠成形品放置於含有氬、氖、氦、氮、二氧化氮、氧或空氣等的容器內,在藉由輝光放電(glow discharge)而產生之電漿暴露,於成形品的表面導入含有氧、氮等的官能基為目的。電漿發生的放電方式有(1)直流放電及低周波放電(2)無線電波放電(3)微波放電等。
電暈放電處理係於所設置的金屬輥與其上以數mm的間隔所設置的刀狀電極之間,施予數千伏特的高壓電,使電暈發生放電,在該放電中的電極-輥間使塑膠成形品通過的方法。
高壓放電處理係在通道(tunnel)狀的處理裝置內,設置可以使被處理之塑膠成形品移動之輸送帶,一面移動塑膠成形品,一面在處理裝置內側的壁面所安裝的多數電極間施予數十萬伏特的高壓電,於空氣中放電處理的方法。藉由放電可知空氣中的氧與塑膠成形品的表面可以活性化,在塑膠的表面取得了氧,產生了極性基。
又,在本發明的光電半導體封閉材料中,添加劑方面,進而可以使用防氧化劑及光穩定劑等。防氧化劑方面,有苯酚系防氧化劑、磷系防氧化劑、硫系防氧化劑、維生素系防氧化劑、內酯系防氧化劑、胺系防氧化劑等。
苯酚系防氧化劑方面,可以例舉Irganox 1010(千葉特用化學品公司,商標)、lrganox 1076(千葉特用化學品公司,商標)、Irganox 1330,千葉特用化學品公司,
商標)、Irganox 3114(千葉特用化學品公司,商標)、Irganox 3125(千葉特用化學品公司,商標)、Irganox 3790(千葉特用化學品公司,商標)BHT、Cyanox 1790(氰胺公司,商標)、SumilizerGA-80(住友化學公司,商標)等的市售品。
磷系防氧化劑方面,可以例舉lrgafos 168(千葉特用化學品公司,商標)、Irgafos 12(千葉特用化學品公司,商標)、Irgafos38(千葉特用化學品公司,商標)、ADKSTAB329K(旭電化公司,商標)、ADKSTAB PEP36(旭電化公司,商標)、ADKSTAB PEP-8(旭電化公司,商標)、Sardstab P-EPQ(Clariant公司,商標)、Weston 618(GE公司,商標)、Weston 619G(GE公司,商標)、Weston-624(GE公司,商標)等的市售品。
硫系防氧化劑方面,可以例舉例如DSTP(Yoshitomi)(吉富公司,商標)、DLTP(Yoshitomi)(吉富公司,商標)、DLTOIB(吉富公司,商標)、DMTP(Yoshitomi)(吉富公司,商標)、Seenox 412S(shipro化成公司,商標)、Cyanox 1212(氰胺公司,商標)等的市售品。
維生素系防氧化劑方面,有生育醇、lrganox E201(千葉特用化學品公司,商標,化合物名;2,5,7,8-四甲基-2(4',8',12'-三甲基三癸基)香豆酮(coumarone)-6-醇)等的市售品。
內酯系防氧化劑方面,可以使用特開平7-233160號
公報,特開平7-247278號公報所記載之物。又,有HP-136(千葉特用化學品公司,商標,化合物名;5,7-二-三級丁基-3-(3,4-二甲基苯基-3H-苯并呋喃-2-酮)等。
胺系防氧化劑方面,可以例舉IRGASTAB FS042(千葉特用化學品公司,商標)、GENOX EP(Crompton公司,商標,化合物名;二烷基-N-甲基胺氧化物)等的市售品。
該等添加劑的使用量,相對於樹脂成分全量100質量份,通常為0.005~5質量份,較佳為0.02~2質量份。該等添加劑可以使用2種以上的組合。
進而,在本發明的光電半導體封閉材料中,可以添加光穩定劑。光穩定劑方面可以使用一般所知之物,較佳為受阻胺系光穩定劑。具體言之,可以例舉商品名方面,旭電化公司製的ADKSTAB LA-52、LA-57、LA-62、LA-53、LA-67、LA-68、LA-77、LA-82、LA-87、LA-94、CSC公司製的Tinuvin 123、144、440、662、Chimassorb 2020、119、944、Hoechst公司製的Hostavin N30、Cytec公司製的Cyasorb UV-3346、UV-3526、GLC公司製的Uval 299、Clariant公司製的Sanduvor PR-31等。
光穩定劑的添加量,相對於樹脂成分全量100質量份,通常為0.005~5重量份,較佳為0.002~2重量份,該等光穩定劑亦可組合2種以上。又,亦可添加各種螢光體
。
以本發明的光電半導體封閉材料封閉的元件並無特別的限制,例如可以例舉發光二極體(LED)晶片、半導體雷射、光二極體、光斷續器(photointerrupter)、光電耦合器(photocoupler),光電晶體、電激發光元件、CCD、太陽電池等。有關本發明的光電變換元件方面,可以例舉以本發明的光電半導體封閉材料封閉的LED等,有關本發明的光電變換裝置方面,可以例舉使用該LED之照明裝置或信號機等的各種半導體裝置。
接著,以本發明的實施例,進而更詳細地說明,本發明並不限定於該等例。
此外,各實施例及比較例中,所得之光電半導體封閉材料(硬化物)的物性評價方法如下。
使用差式掃描型熱量計(Perkin.Elmer公司製,DSC-7),藉由將試料10 mg在氮氛圍下,以50℃保持5分鐘後,以20℃/分加溫,在所得之熱流束曲線所觀測的不連續點為玻璃轉移溫度Tg。
使用壁厚3 mm的試驗片作為試料,準照JIS K7105進行測定(單位%)。測定裝置係使用HGM-2DP(Suga試驗機公司)。
又,將樣本在140℃的恆溫槽中放置100小時,其前後全光線透過率的差(%)為△全光線透過率。
使用UV可視分光計(島津製作所製UV-2400PC),測定在200 nm至700 nm波長範圍內的透過率。
黃變度(YI)的測定係使用作為試料的厚壁3 mm之試驗片,準照JIS K7105而測定。測定裝置係使用SZ-optical SENSOR(日本電色工業公司製),進行如次的耐候性試驗。
△YI1
:使用耐候性試驗機(Jasco international製solarbox 1500e),以500W/m2
的輸出,在試料上照射紫外光100小時,測定紫外光照射前後的YI,其差為△YI1
。
△YI2
:將樣本放置於140℃的恆溫槽100小時,其前後的YI差為△YI2
。
使用長度10 mm,一邊長度3 mm的圓柱形,使用熱物性測定機(TMA/SS6100,精工儀器公司),在加溫速度為5℃/min,荷重為49 mN的條件下測定。
使用Elmer公司製的折射率計,在25℃下測定。
黏接強度:自64 mm×13 mm×3 mm的聚醯胺複合材料試驗片a)
之一端至20 mm止的區域(面積=20 mm×13 mm)內,塗佈熱硬化性樹脂組成物(液狀),而且在其上重疊相同尺寸的試驗片,在設定的條件下,將熱硬化的兩試驗片相黏接(參照第1圖)。其後,以20 mm/分的拉伸速度,進行拉伸試驗。試驗時最大點負重(N)為黏接強度的指標。
與反射器的黏接數:聚醯胺複合材料b)
與引導框架(lead frame)一體成形,準備如第2圖所示已製成的零件10個。在零件的凹部充填熱硬化性樹脂組成物(液狀),在設定的條件下熱硬化。一個一個的觀察零件,觀察硬化物與反射器之間的黏接狀態。依據10個零件內,不剝離的零件有幾個,來評價其黏接性。
a):b)的聚醯胺系複合材料顆粒物,係以70℃經一
晝夜的乾燥後,在桶溫度280℃,模具溫度120℃下射出成形之試驗片。
b)半芳香族聚醯胺(Amodel A4000,Solvay Advanced Polymers)/氧化鈦(PF-726,石原產業)/玻璃纖維(JAFT164G,旭纖維玻璃)=70/10/20(質量比)的比率配合,予以乾摻合後,投入內徑為30 mm的二軸擠壓機之送料斗,以桶(barrel)溫度285℃熔融捏合,成型為丸狀者。
c)上述黏接性試驗係在聚醯胺複合材料試驗片或引導框架(lead frame)一體零件上,照射紫外線與不照射的兩種情形均予以實施。紫外線照射裝置方面,係使用高壓水銀照射燈(3kW IgrantageECS-301G1,Igraphic公司製,120W,照射距離15 cm),以1000 mJ/cm2
的照射能量照射紫外線。
在1-金剛烷基甲基丙烯酸酯(出光興產公司製)單體21 g,加入作為自由基聚合引發劑的1,1-雙(三級丁基過氧)-3,3,5-三甲基環己烷(日本油脂公司製Perhexa 3M-95)0.021 g,成為硬化性組成物。將該組成物流過以3 mm厚度鐵氟龍製的間隔片夾入2片的玻璃板間所製成的胞室(cell),在烤箱內以100℃/1小時,110℃/1小時,120℃/1小時,130℃/30分進行加熱後,藉由在室溫慢慢冷卻獲得無色透明的板狀硬化物。所得
硬化物的物性評價結果如第1表所示。
實施例1中,除了將單體變更為二環戊基甲基丙烯酸酯(日立化成工業公司製FANCRYL FM-513)單體,自由基聚合引發劑變更為偶氮雙異丁腈(東京化成工業公司製)以外,以與實施例6同樣的方法獲得硬化物。所得硬化物的物性評價結果如第1表所示。
實施例6中,除了將單體變更為異基(isobornyl)甲基丙烯酸酯單體(和光純藥工業公司製)以外,以與實施例6同樣的方法獲得硬化物。所得硬化物的物性評價結果如第1表所示。
實施例1中,除了將單體變更為降基甲基丙烯酸酯(和光純藥工業公司製)以外,以與實施例1同樣的方法獲得硬化物。所得硬化物的物性評價結果如第1表所示。
實施例1中,除了進而添加交聯性單體的乙二醇二甲基丙烯酸酯(和光純藥工業公司製)0.42 g以外,以與實施例6同樣的方法獲得硬化物。所得硬化物的物性評價結
果如第1表所示。
實施例5中,除了進而將熱塑性樹脂的Topas 8007(Ticona公司製)2.1 g一面於室溫攪拌,一面平均溶解以外,以與實施例5同樣的方法獲得硬化物。所得硬化物的物性評價結果如第1表所示。
在1-金剛烷基甲基丙烯酸酯(出光興產公司製)單體21 g中,加入作為自由基聚合引發劑之1,1-雙(三級丁基過氧)-3,3,5-三甲基環己烷(日本油脂公司製Perhexa 3M-95)0.021 g及二異丙基苯氫過氧化物(日本油脂公司製percumyl P)0.021 g,成為硬化性組成物。將該組成物流過以3mm厚度鐵氟龍製的間隔片夾入2片的玻璃板間所製成的胞室(cell),在烤箱內以100℃/1小時,110℃/1小時,120℃/1小時,130℃/30分進行加熱後,以2℃/分加溫至200℃止,熱處理1小時,藉由在室溫慢慢冷卻的方式,獲得無色透明的板狀硬化物。所得之硬化物的物性評價結果如第1表所示。
在1-金剛烷基甲基丙烯酸酯(出光興產公司製)單體22 g中,加入甲基甲基丙烯酸酯單體(日本Sigma
Aldrich公司製)2.5 g,加入作為自由基聚合引發劑的雙(4-三級丁基環己基)過氧二碳酸酯(Peroyl TCP,日本油脂公司製)0.068 g,成為硬化性組成物。將該組成物流過以3 mm厚度鐵氟龍製的間隔片夾入2片的玻璃板間所製成的胞室(cell),在烤箱內以60℃/3小時,200℃/30分進行加熱後,藉由在室溫慢慢冷卻的方式,獲得無色透明的板狀硬化物。所得之硬化物的物性評價結果如第2表所示。
在1-金剛烷基甲基丙烯酸酯(出光興產公司製)單體21 g中,加入交聯性單體的聚乙二醇二甲基丙烯酸酯(新中村化學工業公司製NK ESTER 9G)7 g,加入作為自由基聚合引發劑之雙(4-三級丁基環己基)過氧二碳酸酯(Peroyl TCP,日本油脂公司製)0.12 g,成為硬化性組成物。將該組成物流過以3 mm厚度鐵氟龍製的間隔片夾入2片的玻璃板間所製成的胞室(cell),在烤箱內以70℃/3小時,160℃/1小時進行加熱後,藉由在室溫慢慢冷卻的方式,獲得無色透明的板狀硬化物。所得之硬化物的物性評價結果如第1表所示。
在雙酚A型液狀環氧基樹脂(日本環氧樹脂公司製Epicoat 828)單體14 g中,加入甲基六氫酞酸酐(和光
純藥工業公司製)14 g,配合1,8-二氮雜雙環[5,4,0]十一-7-烯(日本Sigma Aldrich公司製)0.028 g,將已平均混合之物注入密閉的鐵氟龍製間隔片中,在烤箱內以130℃ 3小時慢慢地加溫後,以室溫慢慢冷卻的方式獲得板狀試料。所得硬化物的物性評價結果如第1表及第2表所示。
在1-金剛烷基甲基丙烯酸酯(出光興產公司製)18.9 g,1,4-丁烷二醇環氧丙基醚二丙烯酸酯(新中村化學工業公司製)2.1 g中,加入作為聚合引發劑的Perhexa 3M-95(日本油脂公司製)0.021 g,成為硬化性組成物。
將該組成物流過以3 mm厚度鐵氟龍製的間隔片夾入2片的玻璃板間所製成的胞室(cell),在烤箱內以100℃ 1小時,110℃ 1小時,120℃ 1小時,130℃ 30分進行加熱後,以室溫慢慢冷卻的方式獲得無色透明的板狀硬化物。所得之硬化物(樹脂)的物性評價結果如第2表所示。
實施例1中,除了以二環戊二烯基甲基丙烯酸酯(日立化成工業公司製,FANCRYL FM-513)取代1-金剛烷基甲基丙烯酸酯之變更外,其他以與實施例10同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
實施例10中,除了以降基(norbonyl)甲基丙烯酸酯(和光純藥工業公司製)取代1-金剛烷基甲基丙烯酸酯的變更以外,其他以與實施例10同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
實施例10中,除了1-金剛烷基甲基丙烯酸酯14 g,1,4-丁烷二醇環氧丙基醚二丙烯酸酯7 g以外,其他以與實施例1同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
實施例1中,除了1-金剛烷基甲基丙烯酸酯的配合量為15.8 g,進而加入交聯性單體的乙二醇二甲基丙烯酸酯(和光純藥公司製)3.1 g以外,其他以與實施例10同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
實施例10中,除了1-金剛烷基甲基丙烯酸酯的量為21 g,1,4-丁烷二醇環氧丙基醚二丙烯酸酯為0 g以外,其他以與實施例10同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
實施例14中,除了1,4-丁烷二醇環氧丙基醚二丙烯酸酯為0 g,乙二醇二甲基丙烯酸酯為5.2 g以外,其他以與實施例14同樣的方法獲得硬化物。所得硬化物的物性評價結果如第2表所示。
本發明的光電半導體封閉材料,透明性優異,對紫外光安定,不會變黃,耐熱性、折射率的平衡優異,又,回流銲接等的加熱步驟中,有不會變形或破裂之加工性亦優異的特性,可恰當使用於光電半導體裝置(半導體發光裝置)中的發光元件或受光元件等的封閉材料。
[第1圖]實施例的黏接性試驗中,表示測定黏接強度時,試驗片的黏接狀況之說明圖。
[第2圖]實施例的黏接性試驗中,測定與反射器的黏接數時之測定裝置說明圖。
Claims (5)
- 一種光電半導體封閉材料,其特徵為,含有金剛烷基之甲基丙烯酸酯予以自由基聚合所成的聚合物。
- 如申請專利範圍第1項記載的光電半導體封閉材料,其進而含有熱塑性樹脂0.5~20質量%。
- 一種光電半導體封閉材料,其特徵為,含有金剛烷基之甲基丙烯酸酯50~97質量%,與含羥基之丙烯酸酯3~50質量%,予以自由基聚合所成的聚合物。
- 一種使用如申請專利範圍第1~3項中任一項記載的光電半導體封閉材料所封閉的LED晶片。
- 一種光電變換裝置,其特徵為,使用如申請專利範圍第4項記載的LED晶片。
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US20120305982A1 (en) | 2012-12-06 |
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JP2012117079A (ja) | 2012-06-21 |
KR101270821B1 (ko) | 2013-06-05 |
KR20070083920A (ko) | 2007-08-24 |
CN101056900B (zh) | 2011-09-07 |
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