TW201406864A - 含有聚碳矽烷和水合矽膠之用於led密封劑可固化組成物 - Google Patents
含有聚碳矽烷和水合矽膠之用於led密封劑可固化組成物 Download PDFInfo
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- TW201406864A TW201406864A TW102121024A TW102121024A TW201406864A TW 201406864 A TW201406864 A TW 201406864A TW 102121024 A TW102121024 A TW 102121024A TW 102121024 A TW102121024 A TW 102121024A TW 201406864 A TW201406864 A TW 201406864A
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- 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
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- 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
- C08L83/16—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 in which all the silicon atoms are connected by linkages other than oxygen atoms
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Abstract
本發明提供一種可固化組成物,包含:(A)至少一種下式(1)代表之聚碳矽烷A:[R1R2 R3SiX1/2]M[R4R5SiX2/2]D[R6SiX3/2]T[SiX4/2]Q (1),其中R1、R2、R3、R4、R5和R6各獨立地指定為甲基、乙基、乙烯基或苯基,其條件為各分子含有至少2個乙烯基;各X獨立地指定為雙價C2H4羥基或亞苯基;以及M、D、T和Q各自代表範圍從0至小於1之數目,其假設M+D+T+Q為1,(B)至少一種下式(2)代表之有機聚矽氧烷B:[R7R8 R9SiO1/2]M’[R10R11SiO2/2]D’[R12SiO3/2]T’[SiO4/2]Q’, (2),其中R7、R8、R9、R10、R11和R12各獨立地指定為甲基、乙基、乙烯基、苯基或氫,其條件為各分子含有至少2個直接鍵結至矽之氫原子;以及M’、D’、T’和Q’各自代表範圍從0至小於1之數目,其假設M’+D’+T’+Q’為1,以及(C)至少一種催化劑,以及藉由加熱該組成物所獲得之經固化產品,以及使用該組成物作為半導體封裝材料及/或電子元件包裝材料。
Description
本發明係關於含有組合至少一聚碳矽烷含乙烯基官能度和至少一有機聚矽氧烷含氫官能度之可固化組成物,以及包覆固化該組成物所製成產品之發光裝置。更明確而言,本發明係關於固化矽氫化-固化組成物所形成具有光學澄清度、抗高溫,及極佳濕度和阻氣性之聚碳矽烷/聚矽烷產品。本發明進一步係關於包覆這些組成物之可靠發光裝置。
發光二極體(LED)具有許多有益性質包括壽命長、亮度高、電壓低,和體積小、使用時幾乎完全無熱射線,以及即使於低溫下具有良好發光滯留效率。
發光裝置例如發光二極體(LED)中,用於密封發光元件之組成物不僅需要防止外界影響,亦能提供發光元件對支撐發光元件之支承基板如聚鄰苯二甲醯胺、陶瓷等之滿意和安定黏性。該組成物亦具有高透明度以不降低發光元件之亮度。
通常已使用此類密封組成物,例如環氧樹脂等。然而,近來由於LED已變得更加有效率,導致提高光度、於使用和發射短波光線時增加熱產生,以及因而造成環氧樹脂之龜裂和黃化。
因此,已使用具有極佳耐熱性和抗紫外線之有機聚矽氧烷組成物(矽氧組成物)。明確而言,由於其快速加熱可固性及固化時不形成任何
副產物,而因此已廣泛地使用經由矽氫化反應固化且具有極佳產率之加成反應型矽氧組成物。
已有許多有關此類矽氧組成物及其於製造LED用途之參考文獻。
WO 2008023537 A1描述一種含有至少下列成分之可固化有機聚矽氧烷組成物:(A)具有至少3,000量平均分子量之直鏈二有機聚矽氧烷,(B)分支有機聚矽氧烷,(C)一分子內具有平均至少兩個矽鍵合芳基及平均至少兩個矽鍵合氫原子之有機聚矽氧烷,以及(D)矽氫化反應催化劑;此組成物具有極佳可固性以及,當固化時可形成具有高折射率、光透射係數、對各種基板黏性極佳、高硬度和些微表面黏性之軟性固化產品。
EP 2032653 B1揭露一種含有至少下列成分之可固化有機聚矽氧烷組成物:下列通式:R1 3SiO(R1 2SiO)mSiR1 3(其R1係單價羥基,以及「m」係從0至100整數)代表之有機聚矽氧烷組成物(A);下列平均單位化學式:(R2SiO3/2)a(R2 2SiO2/2)b(R2 3SiO1/2)c(其R2係單價羥基,以及「a」、「b」,和「c」係特定數目)代表之有機聚矽氧烷組成物(B);具有一分子內平均至少兩個矽鍵合芳基和平均至少兩個矽鍵合氫原子之有機聚矽氧烷組成物(C);以及矽氫化反應催化劑(D);此組成物以良好間隙充填性和可固化性及於固化時形成具有高折射率固化體、高透光率,以及對各種基板黏性強之特徵。
US 20070249790 A1描述一種無色透明矽透鏡,其製造自熱固化矽膠樹脂組成物,包含(A)具有含R1SiO1.5單位、R2 2SiO單位,和R3 aR4 bSiO(4-a-b)/2單位樹脂構造物之有機聚矽氧烷,其中R1、R2和R3係獨立為甲基、乙基、丙基、環己基或苯基,R4係乙烯基或丙烯基,a係0、1或2,b係1或2,及a+b係2或3,以及其中R2 2SiO單位之重複次數為5至300;(B)具有含R1SiO1.5單位、R2 2SiO單位和R3 cHdSiO(4-c-d)/2單位樹脂構造物之有機氫
聚矽氧烷,其中c係0、1或2,d係1或2,及c+d係2或3,以及其中R2 2SiO單位之重複次數為5至300;以及(C)鉑族催化劑。此組成物呈現極佳撓性、透明度和可塑性,以及降低表面黏性。
US 20080160322 A1描述一種用於密封發光元件之矽氧組成物,包括(A)含乙烯基有機聚矽氧烷具有平均單位化學式(SiO4/2)a(ViR2SiO1/2)b(R3SiO1/2)c代表之三維網絡結構,其中Vi代表乙烯基,R's係除了鏈烯基外之相同或不同經取代或未經取代單價羥基,以及a、b和c係滿足a/(a+b+c)為0.2至0.6和b/(a+b+c)為0.001至0.2之正數;(B)每分子含有至少兩個氫原子之有機氫聚矽氧烷,各氫原子鍵合至一矽原子,該有機氫聚矽氧烷含量能使氫原子鍵合至矽原子之數量為成分(A)內每1 mol乙烯基鍵合至矽原子之0.3至3.0;以及(C)催化量之氫化矽烷化催化劑,其中固化後組成物之線性膨脹係數為10×10-6至290×10-6/℃。可獲得降低其與支承基板殘留應力並且具有長期滿意和穩定黏性之固化產品。
EP 1767580 A1揭露一種含有機聚矽氧烷之加成反應固化矽組成物,其中一些矽原子可經由2至10個碳原子之雙價羥基被連接。然而,至少80 mol-%之全部橋連兩個矽原子必需為氧原子,亦即主要由矽氧烷單位構成聚合主鏈而僅容許少數矽烯烴基或矽亞芳基單位。據稱該組成物特別適合用作為光學裝置例如LED以及透鏡材料或硬塗佈劑等之密封材料。
KR 20100030959 A中教導用於密封材料或LED透鏡之聚矽氧烷。該聚矽氧烷含有[--Si(R1)(R2)-X1-C6H4-Y1-]m之重複單位,其中R1和R2係獨立為氫、甲基、乙基、苯基或C2-C6烯基;X1和Y1係獨立為C0-C6伸烷基、C2-C6伸烯基、C2-C6亞炔基、胺基或氧;以及m係1以上。不排除存在矽氧烷單位。
從WO 2009/131023 A1已知含矽聚合物含有橋連鄰近矽原
子之-R2-C6H4-R2-單位,其中R2指定為相同或不同、經取代或未經取代伸烷基。該含矽聚合物進一步含有矽氧烷單位。含矽聚合物內含有該-R2-C6H4-R2-橋單位之克分子量係低於10%。該聚合物可用於適合於獲得具有高折射率特性固化產品之可固化高分子組成物。此類組成物適合被用作為光學裝置例如LED以及用於光學儀器之密封劑。
從上述文件可看出矽氧組成物已廣泛被用作為LED封裝材料。然而,由於矽氧組成物具有大自由體積作為固有性質,其氣體和濕氣阻隔性較環氧基材料更差。因此,水份更易穿透封裝材料而造成LED晶片腐蝕,其大為影響LED之耐用性。
因此,發展一種具有極佳氣體和濕氣阻隔性以及同時熱安定性等於矽氧組成物安定性之LED密封劑為一項極大挑戰。
本發明之目的係提供一種組成物,其經由矽氫化反應被固化以及固化後呈現高透明度、熱安定性,及極佳氣體和濕氣阻隔性。發明人發現Si-[雙價羥基]-Si鍵,及特別指Si-C2H4-Si鍵和Si-C6H4-Si鍵甚至在高溫下仍極為安定,以及因而此類鍵結被用於建構本發明聚合物之主鏈。此類聚合物內包含單獨經由該雙價羥基被連接之矽原子主鏈,以及因而此類聚合物在下文中被稱為聚碳矽烷。本發明之目的可藉由以下提供之組成物而達成。
本發明第一態樣中係關於一種可固化組成物,其特別指一種透明LED封裝組成物,包含:(A)至少一種下式(1)代表之聚碳矽烷A:[R1R2 R3SiX1/2]M[R4R5SiX2/2]D[R6SiX3/2]T[SiX4/2]Q (1),
其中R1、R2、R3、R4、R5和R6各獨立地指定為甲基、乙基、乙烯基或苯基,其條件為各分子含有至少2個乙烯基;各X獨立地指定為雙價C2H4羥基或亞苯基;以及M、D、T和Q各自代表範圍從0至小於1之數目,其假設M+D+T+Q為1,(B)至少一種下式(2)代表之有機聚矽氧烷B:[R7R8 R9SiO1/2]M’[R10R11SiO2/2]D’[R12SiO3/2]T’[SiO4/2]Q’, (2),其中R7、R8、R9、R10、R11和R12各獨立地指定為甲基、乙基、乙烯基、苯基或氫,其條件為各分子含有至少2個直接鍵結至矽之氫原子;以及M’、D’、T’和Q’各自代表範圍從0至小於1之數目,其假設M’+D’+T’+Q’為1,以及(C)至少一種催化劑。
該有機聚矽氧烷B含有直接鍵結至矽之氫原子以及,因此亦可被稱為有機氫聚矽氧烷或水合矽膠。
此外,本發明係關於一種藉由加熱根據本發明組成物所獲得之經固化組成物,以及使用該根據本發明之組成物作為半導體封裝材料及/或電子元件包裝材料。
根據本發明之組成物含有式(1)代表之聚碳矽烷A以及式(2)代表之有機聚矽氧烷B。在這兩種情況下該聚合物含有不同「單位」,其中一單位被認為是一種結構單元,其由1個矽原子和一根據矽原子價數一分別為直接鍵結至該矽原子之4個橋連基X或O以及其餘基R所形成。僅具有一個橋連基之單位亦被稱為單官能或M-單位。具有兩個橋連基之單位被稱為雙官能或D-單位,具有三個橋連基之單位被稱為三官能或T-單位,以及具有四個橋連基之單位被稱為四官能或Q-單位。存在一特定聚合物內之特定單位數以M和M’、D和D’、T和T’,及Q和Q’代表其指數。
已認為不僅在一特定聚碳矽烷之各種單位類型內,並且在一和相同類型之各種單位及甚至單一單位內亦可具有不同橋連單位X。因此,例如,含有兩個橋連基如式(1)中[R4R5SiX2/2]單位之D-單位可含兩個相同橋連基,亦即2/2雙價C2H4基或2/2亞苯基。然而,其單位也可含1/2雙價C2H4基及1/2亞苯基,其可應用於T-和Q-單位內之對應橋連基。
該聚碳矽烷A實質上係一種以上述說明平均複合式(1)代表直鏈或支鏈結構之液體或固體聚碳矽烷。
該聚碳矽烷A較佳為具有支鏈結構,即對應式(1),其中T+Q係大於0。
根據本發明聚碳矽烷之重均分子量較佳為100-300,000 g/mol,較佳為1,000-50,000 g/mol(GPC,標準:聚苯乙烯)。其黏度於25℃較佳為0.1-100 Pa.s以及於25℃更佳為0.5-50 Pa.s(布氏DV-+數字黏度計/LV(轉軸S64,轉速50 rpm))。
式(1)中X較佳為一雙價C2H4羥基。
「可固化組成物」被認為係二或多種物質藉由物理或化學作用從軟性狀態轉變成硬性狀態之一種混合物。這些物理或化學作用包括,例如藉由熱、光或其他電磁幅射所傳遞能量,但亦可單純地藉由接觸大氣濕度、水或反應性組分。本發明之組成物較佳為熱可固化。
本發明之可固化組成物進一步含有至少一種式(2)代表之有機聚矽氧烷B。此類有機聚矽氧烷每分子內含有至少兩個直接鍵結至矽之氫原子。
該有機聚矽氧烷B實質上係一種具有直鏈或支鏈結構之液體或固體聚碳矽烷。其較佳為具有直鏈結構,即對應式(2),其中T’+Q’係0,以及D’係大於0。
該有機聚矽氧烷B之重均分子量較佳為1,000-300,000 g/mol,以及更佳為10,000-100,000 g/mol(GPC,標準:聚苯乙烯)。其黏度於25℃較佳為0.1-100 Pa.s以及於25℃更佳為0.5-50 Pa.s(布氏DV-+數字黏度計/LV(轉軸S64,轉速50 rpm))。
該可固化組成物較佳為含有0.8-8 mmol/g矽鍵合氫原子之有機聚矽氧烷B。
該可固化組成物較佳為含有各別量之聚碳矽烷A和有機聚矽氧烷B以供應形成自任何存在有機聚矽氧烷B之矽鍵合氫原子(即SiH基)對形成自任何存在聚碳矽烷A之矽鍵合乙烯基之克分子比在0.5至10範圍內,更佳為0.8至4,以及最佳為1至3。換言之該Si-H/Si-乙烯基比例較佳為0.5-10,更佳為0.8-4.0,以及最佳為1.0-3.0。
該可固化組成物更含有至少一種催化劑。催化劑係能促進聚碳矽烷A內乙烯基及/或和丙烯基與有機聚矽氧烷B內Si-H基間之矽氫化加成反應可被使用之任何化合物。典型加成反應催化劑為鉑基金屬催化劑包括鉑催化劑,例如氯鉑酸與一元醇之反應產物、氯鉑酸與烯烴和雙乙醯乙酸鉑之複合物,以及鈀催化劑和銠催化劑。
該催化劑較佳為一或多種選自由鉑基金屬催化劑所構成群組之化合物。
該催化劑只要足以加速所欲矽氫化反應,其加入量並無特殊限制。加成反應催化劑之用量較佳為根據該可固化組成物之總重量約1至500 ppm,特別指約2至100 ppm之金屬,其特別指鉑基金屬。即使該金屬以複合物存在於可固化組成物內,該「金屬」或「鉑基金屬」一詞僅分別指金屬本身之含量。
可單純藉由混合全部成分之方法製備本發明之可固化組成
物。因此製成之混合物可立即被塗佈及被固化,例如藉由加熱。
然而,在本發明一具體實施例中,該組成物係一種由成分1和成分2所組成之雙組分製備物,其中該成分1含有聚碳矽烷A及存在之全量催化劑以及該成分2含有存在有機聚矽氧烷B之全量以及其他任選聚碳矽烷A。各成分可被充填入不同容器,例如管或瓶,或雙組分容器之不同室,例如雙室管。此可安全地儲存組成物而不導致過早固化。成分1和成分2在使用前被分開保存。使用組成物時,混合成分1和成分2以及將混合物塗佈於所欲位置。
除了上述成分(A)至(C)之外,根據本發明之組成物只要能達成本發明之目的可進一步含有其他任選成分。
可用任選成分包括用於調節固化時間和賦予保存期限之加成反應抑制劑,以及助黏劑以改善該組成物之黏性。
適當反應抑制劑包括乙炔基環已醇、2-甲基-3-丁炔-2-醇、3,5-二甲基-1-己炔-3-醇、2-苯基-3-丁炔-2-醇,或類似炔醇;3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔,或類似烯炔化合物;1,3,5,7-四甲基-1,3,5,7-四乙烯基-環四矽氧烷、1,3,5,7-四甲基-1,3,5,7-四己烯基-環四矽氧烷;苯并***等。這些抑制劑之加入量並無特殊限制,但是以重量單位而言,這些抑制劑加入量每組成物重量較佳為10至1,000 ppm。
助黏劑意指可改善組成物表面黏性之物質。可個別使用熟知本領域技術者所習知助黏劑(增黏劑)或混合數種化合物。適當實例包括樹脂、萜烯低聚物、苯并呋喃/茚樹脂、脂肪族石化樹脂以及改性酚醛樹脂。適用於本發明架構內者為例如,藉由聚合主要為α-或β-蒎烯之萜烯、茴香萜(dipentene)或檸檬烯(limonene)所獲得之碳氫樹脂。這些單體通常利用費克氏觸媒(Friedel-Crafts catalysts)引發陽離子之聚合作用。萜烯樹脂亦包括
萜烯和其他單體之共聚物,例如苯乙烯、α-甲基苯乙烯、異戊二烯等。上述樹脂被用作為,例如壓敏黏著劑和塗料之助黏劑。亦適用於萜烯酚樹脂,其係製造自將酚加至萜烯或松香之酸性催化反應。萜烯酚樹脂被溶解於大部分有機溶劑和油類內以及互溶於其他樹脂、石蠟和橡膠。亦適用於本發明架構之助黏劑於上述松香及其衍生物,例如其酯或醇內。尤其為適用於矽烷助黏劑,其特別指胺基矽烷和環氧矽烷,例如3,4-環氧環己基乙基三甲氧基矽烷。
根據本發明之可固化組成物一特定具體實施例中,該組成物包含通式(3)之胺基矽烷R’R”N-R-SiX’Y’Z’ (3)作為助黏劑,其中R'和R"為相互獨立之氫或C1-C8烷基殘基,R為具有1-12個碳原子含有任選雜原子之雙價烴殘基,以及X’、Y’、Z’為相互獨立之C1-C8烷基、C1-C8烷氧基或C1-C8醯氧基殘基,其至少一殘基為C1-C8烷氧基或C1-C8醯氧基。此類化合物對根據本發明可固化組成物之鍵結聚合物成分具有高親和力,並且亦具有廣泛極性和非極性表面及因此有助於固化組成物與被黏合基材間或分別被塗覆於其上之處形成極安定黏性。
聯結基R可為,例如直鏈或支鏈或環狀、經取代或未經取代伸烷基殘基。作為雜原子之氮(N)或氧(O)可任選地被含於其中。若X’、Y’及/或Z’為醯氧基時,其可為例如乙醯氧基-OCO-CH3。
只要不損及透明度,其可滲合無機填料以增加該組成物之強度。
用於根據本發明組成物之適當填料為,例如白堊、石灰粉、
沈澱及/或熱解矽石、沸石、膨潤土、碳酸鎂、矽藻土(kieselguhr)、氧化鋁、黏土、滑石粉、氧化鈦、氧化鐵、氧化鋅、沙石、石英、燧石(flint)、雲母、玻璃粉末及其他研磨礦粉。此外,亦可使用有機填料,特別指碳黑、石墨、木質纖維、木粉、鋸木屑、木漿、棉花、紙漿、碎木、切碎秸杆、糠(chaff)、磨碎桃殼及其他切碎纖維。此外,亦可加入短纖維例如玻璃纖維、玻璃絲、聚丙烯晴、碳纖維、克維拉纖維(Kevlar fiber)或聚乙烯纖維。亦可使用鋁粉作為填料。另外,具有礦殼或塑膠殼之中空球亦適合作為填料。這些可為例如中空玻璃球,其市售商品名稱為Glass Bubbles®。塑膠基質中空球可供應自例如市售商品Expancel®或Dualite®。這些係由無機或有機物質所組成,其各具有直徑1 mm或以下,較佳為500 μm或以下。在一些應用上,填料於製備時較佳為賦予黏流性(thixotropy)。此類填料亦可被稱為流變輔助劑,例如氫化蓖麻油、脂肪酸醯胺或可膨脹塑膠如PVC。只要其可從適當計量裝置(如管件)輕易地被擠出,此類製品具有3,000至15,000之黏度,較佳為4,000至8,000 mPas或5,000至6,000 mPas。
根據該組成物總重量,填料之用量為1至80 wt.%。可使用單一種填料或組合使用數種填料。
在一根據本發明組成物之較佳具體實施例中,該填料係具有BET表面積從10至90 m2/g之高分散矽,特別指從35至65 m2/g。當使用此類氧化矽時,根據本發明組成物之黏度其實質上不增加但有助於強化其經固化組成物。藉由此強化,可改善使用根據本發明組成物之密封劑或塗佈組成物,例如初始強度、剪力強度和黏著劑之黏性。
較佳為使用具有BET表面積45至55 m2/g之高分散矽,最佳為具有BET表面積約50 m2/g。此類氧化矽與具有較高BET表面積之氧化矽
相比,其優點為可縮短30至50%之混合時間。該高分散矽之另一優點為其可在極高濃度下進行混合而不損及組成物之透明度和流動性。在一根據本發明組成物之具體實施例中,該填料藉由雷射繞射測量最佳為低於25 μm之具有平均粒徑d50高分散矽,特別指從5至20 μm。此類型填料特別適合用於當在特定用途下需要高透明、清澈組成物時。亦可使用具有極高BET表面積之燻矽(pyrogenic)及/或沈澱矽,其較佳為100-250 m2/g,特別指110-170 m2/g作為填料。然而,混合此類氧化矽需時極長而因此更加耗費成本。此外,產品內被導入大量空氣而需要以複雜和耗時之方式再一次被移除。另一方面,以較小比例氧化矽重量比可達到加強較高BET表面積經固化組成物之效果。依此方式,可導入附加物質以針對其他需求改善根據本發明之製品。
在使用鹼性填料代替酸性填料時,例如可使用立方、非立方、無晶形及其他修飾之碳酸鈣(白堊)。該白堊較佳為用於表面處理或塗佈。作為塗佈劑時,較佳為使用脂肪酸、脂肪酸皂和脂肪酸酯,例如月桂酸、棕櫚酸或硬脂酸,此類酸或其烷基酯之鈉或鉀鹽。此外,然而亦可使用其他表面活性物質,例如長鏈醇或烷基苯磺酸之硫酸酯或其鈉或鉀鹽,或基於矽烷或鈦酸酯之偶合劑。白堊之表面處理時通常需同時改善其可加工性和黏著強度以及該組成物之耐候性。根據粗白堊之總重量,該塗佈組成物內之用量比例通常為0.1至20 wt%,較佳為1至5 wt%。
視所欲性能特徵,可使用沈澱或重質碳酸鈣(ground chalks)。可藉由乾或濕機械研磨法製造重質碳酸鈣,例如從天然石灰、石灰石或大理石。視研磨法可獲得具有不同分級之平均粒徑。特定表面積值(BET)較佳為介於1.5 m2/g和50 m2/g之間。
需要時,亦可加入磷和抗分解劑。
其他輔助物質和添加劑包括增塑劑、安定劑、抗氧化劑、活
性稀釋劑、乾燥劑、紫外線安定劑、抗老化劑、流變輔助劑、防黴劑及/或阻燃劑。
固化根據本發明之組成物一般為於50至200℃,較佳為70至160℃加熱1至60分鐘,以及更佳為加熱2至30分鐘。此外,固化後亦可於50至200℃,以及較佳為於70至160℃加熱0.1至10小時,以及較佳為1至4小時。
此外,本發明係關於藉由加熱根據本發明可固化組成物所獲得之經固化產品。
本發明進一步申請標的係使用根據本發明之可固化組成物於封裝、密封、保護、黏合及/或透鏡形成材料,其特別指作為半導體封裝材料及/或電子元件包裝材料。本發明之組成物對水分和空氣具有增強阻隔性。明確而言,根據本發明之組成物有利地被用於作為包覆半導體之封裝材料,其特別指用於發光裝置(LED)。
在下列特定態樣中利用一系列實例進一步說明本發明,然而,本發明非僅侷限於這些實例。
依照下列所述方法進行評估。
下列實例中,利用膠體滲透層析法(GPC)以聚苯乙烯-等值測定重均分子量值(g/mol)。
根據中國化學工業標準HG/T 3312-2000滴定乙烯含量。
氫含量之滴定法已揭露於Feng S.Y.、Zhang,J.、Li,M.J.、Zhu,Q.Z.;有機矽聚合物及其應用,第400-401頁;化學工業出版社。
藉由製造自PerkinElmer公司之紫外線可見光譜分析儀Lambda 650S測量透光率。從300 nm至800 nm範圍測量透光率,以及記錄其在450 nm之透光率。
藉由Mocon Permatran-W®型3/33於50℃/100% RH(RH=相對濕度)測定滲透作用。
各種組成物使用3個樣本測試其龜裂和層合行為。藉由於LED杯內在下述條件下固化組成物以製備各樣本。固化期間若一個以上樣本龜裂,則該組成物被視為「劣」,若無樣本龜裂,則該組成物被視為「優」。若一個以上測試件發現從LED杯剝離,則該組成物被視為「分層」,若無測試件剝離,則該組成物被視為「未分層」。
二乙烯基二甲基矽烷(CAS 10519-87-6)係購自Ruilijie化學公司。二苯基矽烷(CAS:775-12-2)和三乙烯甲基矽烷(CAS:18244-95-6)係購自Gelest。鉑催化劑SIP 6832.2(環狀甲基乙烯基矽氧烷內2.0-2.3%鉑濃度,CAS:68585-32-0)係購自Gelest。HPM-502(一種具有100 mPa*S黏度及1359 g/mol重均分子量,6.06 mmol/g氫含量和35.4重量%苯基含量之氫封端甲基氫矽氧烷-苯基甲基矽氧烷共聚物)係購自Gelest。
將9.22 g二苯基矽烷、6.16 g二乙烯基二甲基矽烷、0.008 g鉑催化劑SIP 6832.2和6.28 g二甲苯加入100 mL之乾燥和潔淨雙頸圓底燒瓶內。裝上電磁攪拌器及以塞子蓋上燒瓶以及配備一冷凝器。在攪拌下將混
合物加熱至75℃然後於此溫度維持1小時,接著再於130℃加熱6小時。於115℃和20 mbar旋轉蒸發1小時及接著於135℃和5 mbar再一小時以移除未反應單體。獲得液體具有3072 g/mol之重均分子量,以及其乙烯基含量為0.65 mmol/g。
獲得之聚合物具有下列平均分子式:[Vi(CH3)2Si(C2H4)1/2]0.095[Ph2Si(C2H4)2/2]0.476[(CH3)2Si(C2H4)2/2]0.429
將9.22 g二苯基矽烷、7.44 g三乙烯基甲基矽烷、0.016 g鉑催化劑SIP 6832.2和6.28 g甲苯加入100 mL之乾燥和潔淨雙頸圓底燒瓶內。裝上電磁攪拌器及以塞子蓋上燒瓶以及配備一冷凝器。在攪拌下將混合物加熱至75℃然後於此溫度維持1小時,接著再於130℃加熱6小時。於115℃和20 mbar旋轉蒸發1小時及接著於135℃和5 mbar再一小時以移除未反應單體。獲得液體聚合物具有分支結構,其重均分子量為1662 g/mol,以及乙烯基含量為3.6 mmol/g。
混合100 g合成實例1之乙烯基聚碳矽烷、21.5 g有機氫聚矽氧烷HPM-502、0.001 g鉑催化劑SIP 6832.2,以及0.001 g之抑制劑3,5-二甲基-1-己炔-3-醇。獲得之混合物於150℃加熱2小時以產生固化產品。評估產品之滲透性、龜裂度、黏度/層合度、於450 nm初始透明度(T@450nm(初始)),以及產品在150℃熱處理100小時之後於450 nm之透明度(T@450nm(150℃,100小時))。其結果示於表1。
混合100 g合成實例2之乙烯基聚碳矽烷、2,55 g有機氫聚矽氧烷HPM-502、0.001 g鉑催化劑SIP 6832.2,以及0.001 g之抑制劑3,5-二甲
基-1-己炔-3-醇。獲得之混合物於150℃加熱2小時以產生固化產品。評估產品之滲透性、龜裂度、黏度/層合度、於450 nm初始透明度(T@450nm(初始)),以及產品在150℃熱處理100小時之後於450 nm之透明度(T@450nm(150℃,100小時))。其結果示於表1。
以A:B=1:2重量比例混合市面購自道康寧公司(Dow Corning)商品6636之高折射率(RI)兩種成分A和B封裝材料,然後於70℃加熱1小時,於120℃加熱1小時以及最後於150℃加熱1小時。評估形成經固化產品之滲透性、龜裂度、黏度/層合度、於450 nm初始透明度(T@450nm(初始)),以及產品在150℃熱處理100小時之後於450 nm之透明度(T@450nm(150℃,100小時))。其結果示於表1。
從表1結果可看出根據本發明之經固化產品與獲得自單獨使用有機聚矽氧烷之市售封裝材料比較顯示可改善其滲透行為。其熱安定性則相若。
Claims (11)
- 一種可固化組成物,包含:(A)至少一種下式(1)代表之聚碳矽烷A:[R1R2 R3SiX1/2]M[R4R5SiX2/2]D[R6SiX3/2]T[SiX4/2]Q (1),其中R1、R2、R3、R4、R5和R6各獨立地指定為甲基、乙基、乙烯基或苯基,其條件為各分子含有至少2個乙烯基;各X獨立地指定為雙價C2H4羥基或亞苯基;以及M、D、T和Q各自代表範圍從0至小於1之數目,其假設M+D+T+Q為1,(B)至少一種下式(2)代表之有機聚矽氧烷B:[R7R8 R9SiO1/2]M’[R10R11SiO2/2]D’[R12SiO3/2]T’[SiO4/2]Q’, (2),其中R7、R8、R9、R10、R11和R12各獨立地指定為甲基、乙基、乙烯基、苯基或氫,其條件為各分子含有至少2個直接鍵結至矽之氫原子;以及M’、D’、T’和Q’各自代表範圍從0至小於1之數目,其假設M’+D’+T’+Q’為1,以及(C)至少一種催化劑。
- 根據申請專利範圍第1項所述之組成物,包含式(1)代表之聚碳矽烷A,其中T+Q係大於0。
- 根據申請專利範圍第1項所述之組成物,其中該聚碳矽烷A之重均分子量為100-300,000 g/mol,較佳為1,000-50,000 g/mol。
- 根據申請專利範圍第1項所述之組成物,含有式(2)代表之有機聚矽氧烷B,其中D’係大於0。
- 根據申請專利範圍第1項所述之組成物,其中存在各別量之聚碳矽烷A和有機聚矽氧烷B以提供0.5-10之Si-H/Si-乙烯基克分子比,較佳為1.0-3.0。
- 根據申請專利範圍第1項所述之組成物,其中該有機聚矽氧烷B之重均分子量為1,000-300,000 g/mol,較佳為10,000-100,000 g/mol。
- 根據申請專利範圍第1項所述之組成物,其中該催化劑係一或多種選自由鉑基金屬催化劑所構成之群組。
- 根據申請專利範圍第1項所述之組成物,其中根據該可固化組成物總重量該催化劑之催化金屬用量範圍為1至500 ppm,較佳為2至100 ppm。
- 根據申請專利範圍第1項所述之組成物,其中該組成物係一種由成分1和成分2所組成之雙組分製備物,其中該成分1含有聚碳矽烷A及存在之全量催化劑以及該成分2含有存在有機聚矽氧烷B之全量以及其他任選聚碳矽烷A。
- 一種藉由加熱根據申請專利範圍第1項至第9項中任一項所述可固化組成物獲得之經固化產品。
- 一種根據申請專利範圍第1項至第9項中任一項所述組成物作為半導體封裝材料及/或電子元件包裝材料之用途。
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