TW201512293A - 樹脂組合物及閘極絕緣膜 - Google Patents
樹脂組合物及閘極絕緣膜 Download PDFInfo
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- TW201512293A TW201512293A TW103125963A TW103125963A TW201512293A TW 201512293 A TW201512293 A TW 201512293A TW 103125963 A TW103125963 A TW 103125963A TW 103125963 A TW103125963 A TW 103125963A TW 201512293 A TW201512293 A TW 201512293A
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Classifications
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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
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1515—Three-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
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Abstract
提供一種樹脂組合物,包含:含有羥基以及氰基烷基的樹脂(A)、分子內具有2個以上環氧基的環氧化合物(B)、分子內具有2個以上羥基、且羥基值為150~300mgKOH/g的硬化劑(C)、以及具有下述一般式(1)所表示結構的交聯劑(D),
□(上述一般式(1)中,R1、R2為碳數1~20的烷基,R1與R2可彼此相同或是不同)。
Description
本發明是關於樹脂組合物及閘極絕緣膜,更詳細而言是有關於一種樹脂組合物,能夠提供即使膜成形後進行高溫處理,亦能夠適當的防止密著性降低的樹脂膜,以及使用該樹脂組合物所得的閘極絕緣膜。
近年來,關於使用有機材料或非晶質氧化物的TFT(薄膜電晶體)之研究正在盛行。薄膜電晶體是在基板上具有半導體層、閘極電極、源極電極、汲極電極以及閘極絕緣膜的電晶體,可區分為底閘極(bottom gate)型與頂閘極(top gate)型。底閘極型的構成為:在基板上具有閘極電極,於其上具有經由閘極絕緣膜而連接於半導體層的源極電極以及汲極電極。另一方面,頂閘極型構成為:在基板上具有與半導體層相接的源極電極與汲極電極,於其上經由絕緣膜而具有閘極電極。
於構成此種薄膜電晶體的閘極絕緣膜中,要求優良的絕緣性、電特性。高介電常數的閘極絕緣膜能夠以低電壓進行電晶體的驅動,而有助於元件的低電力消耗化。而且,例如底閘極型的話,在絕緣膜上以規定形狀形成半導體層、閘極電極、汲極電極,例如具有使用微影法與蝕刻法的情形。於此
情形,為了使閘極絕緣膜得以接觸顯影液或蝕刻液,對絕緣膜要求耐藥品性。而且,如此形成的閘極絕緣膜上,其後會進行半導體層、閘極電極、汲極電極的形成,但是在形成此些半導體層、閘極電極、汲極電極時,由於會進行高溫處理,對閘極絕緣膜要求即使在經由如此的高溫處理之後,亦能夠保持高的密著性。
作為用以形成此種閘極絕緣膜的樹脂,例如專利文獻1揭示使用聚乙烯苯酚(PVP)形成閘極絕緣膜的技術。然而,如同此專利文獻1的使用聚乙烯基苯酚的情形,雖然能夠得到耐藥品性優良至某程度的閘極絕緣膜,但有所得的閘極絕緣膜的介電常數顯著降低之問題。而且,在非專利文獻1中揭示有形成由氰基乙基普魯蘭多醣(Pullulan)與具有三嗪環的交聯劑所構成的閘極絕緣膜的技術,但此種的閘極絕緣膜成膜後暴露於高溫的話,與基材的密著性顯著降低。
專利文獻1:日本專利公開第2010-56115號公報
非專利文獻1:Organic Electronics 11(2010)966-1004
本發明的目的在於提供一種樹脂組合物,該樹脂
組合物能夠提供介電常數高、耐藥品性以及密著性優良、且能夠適當防止膜成形後進行高溫處理時之密著性降低的樹脂膜,以及提供使用該樹脂組合物所得的閘極絕緣膜。
本發明人們為了達成上述目的而努力研究的結果,發現使用含有羥基以及氰基烷基的樹脂作為基質的樹脂,使其與特定的環氧化合物、特定的硬化劑及特定的具有含有烷氧基甲基結構的交聯劑調配而成的樹脂組合物,藉此能夠達成上述目的,進而完成本發明。
亦即是,根據本發明,提供〔1〕一種樹脂組合物,包括:含有羥基以及氰基烷基的樹脂(A)、分子內具有2個以上環氧基的環氧化合物(B)、分子內具有2個以上羥基、且羥基值為150~300mgKOH/g的硬化劑(C)、以及具有下述一般式(1)所表示結構的交聯劑(D),
(上述一般式(1)中,R1、R2為碳數1~20的烷基,R1與R2可彼此相同或是不同。)
〔2〕如前述〔1〕記載的樹脂組合物,其中前述樹脂(A)是將具有複數羥基的含羥基的有機化合物所含的羥基的一部份氰基烷基化而得者,〔3〕如前述〔2〕記載的樹脂組合物,其中前述含羥基的
有機化合物為普魯蘭多醣(Pullulan)或聚乙烯醇,〔4〕如前述〔1〕~〔3〕的其中一項記載的樹脂組合物,其中前述環氧化合物(B)為分子內具有2個以上環氧基之含芳香族烴結構的環氧化合物,〔5〕如前述〔1〕~〔4〕的其中一項記載的樹脂組合物,其中前述硬化劑(C)具有酚性羥基作為前述羥基,〔6〕如前述〔1〕~〔5〕的其中一項記載的樹脂組合物,其中進一步含有分子內具有酚性的羥基、且羥基值未滿150mgKOH/g的酚類化合物(E),〔7〕如前述〔1〕~〔6〕的其中一項記載的樹脂組合物,其中進一步含有硬化觸媒(F),〔8〕如前述〔1〕~〔7〕的其中一項記載的樹脂組合物,其中前述樹脂(A)所含有的羥基與氰基烷基的比率,以「羥基:氰基烷基」的莫耳比為30:70~2:98,〔9〕如前述〔1〕~〔8〕的其中一項記載的樹脂組合物,其中前述交聯劑(D)為下述式(2)~(4)所表示的至少一種化合物,
(上述一般式(2)~(4)中,R1、R2與前述一般式(1)相同,上述一般式(3)中,R3、R4為碳數1~20的烷基,上述一般式(3)中,R1、R2、R3、R4的全部或是任一可為相同,亦可以全部不同。),以及〔10〕一種閘極絕緣膜,使用前述〔1〕~〔9〕的其中一項記載的樹脂組合物而獲得。
根據本發明,提供一種樹脂組合物,該樹脂組合物能夠提供介電常數高、耐藥品性以及密著性優良、且能夠適當防止膜成形後進行高溫處理時之密著性降低的樹脂膜,以及提供使用該樹脂組合物所得的閘極絕緣膜。
1、1a、1b‧‧‧薄膜電晶體
2‧‧‧基板
3‧‧‧閘極電極
4‧‧‧閘極絕緣膜
5‧‧‧半導體層
6‧‧‧源極電極
7‧‧‧汲極電極
8‧‧‧保護層
9‧‧‧蝕刻終止層
10‧‧‧通道部
第1圖所示為具備本發明的樹脂組合物所構成的閘極絕緣膜的薄膜電晶體的一例的剖面圖。
第2圖所示為第1圖所示的薄膜電晶體的製造方法的圖。
第3圖所示為具備本發明的樹脂組合物所構成的閘極絕緣膜的薄膜電晶體的其他例(第2例)的剖面圖。
第4圖所示為具備本發明的樹脂組合物所構成的閘極絕緣膜的薄膜電晶體的其他例(第3例)的剖面圖。
本發明的樹脂組合物包括:含有羥基以及氰基烷基的樹脂(A)、分子內具有2個以上環氧基的環氧化合物(B)、分子內具有2個以上羥基、且羥基值為150~300mgKOH/g的硬化劑(C)、以及具有後述一般式(1)所表示結構的交聯劑(D)。
作為含有羥基以及氰基烷基的樹脂(A)(以下稱為「含羥基-氰基烷基的樹脂(A)」。),只要是含有羥基以及氰基烷基即可,並沒有特別的限制,例如可舉出使用具有複數羥基的含羥基的有機化合物作為起始原料,藉由其與丙烯腈反應,將含羥基的有機化合物所含的羥基中的一部份,加以氰基烷基化而得者。
作為含羥基的有機化合物,例如可舉出葡萄糖、果糖、半乳糖等單糖類;麥芽糖、蔗糖、乳糖等的二糖類;山梨糖醇、木糖醇等的糖醇、纖維素、澱粉、普魯蘭多醣(Pullulan)等的多糖類;甲基纖維素、羧基甲基纖維素等的烷基纖維素、羥基丙基纖維素、羥基乙基纖維素、二羥基丙基纖維素等的羥基烷基纖維素;羥基丙基甲基纖維素、羥基乙基甲基纖維素等
的羥基烷基烷基纖維素;二羥基丙基普魯蘭多醣(Pullulan)等的多醣類衍生物;聚乙烯醇等;聚乙烯苯酚;酚醛清漆樹脂;聚乙烯苯酚等。
這些之中,於作為閘極絕緣膜的情形,由介電常數的提升效果高的觀點來看,較佳為普魯蘭多醣(Pullulan)、聚乙烯醇。
而且,作為用以取代含羥基的有機化合物之氰基烷基並沒有特別的限定,可舉出一般式:-R-CN(R為碳數2~6的伸烷基)所表示的基,例如氰基乙基、1-氰基丙基、1-氰基丁基、1-氰基己基等。這些之中,由比較容易導入至含羥基的有機化合物、泛用性能高的觀點,較佳為羥基乙基。而且,本發明所使用的含羥基-氰基烷基的樹脂(A),亦可以使用兩種以上的氰基烷基。尚且,這種的氰基烷基可以藉由使用對應的含氰基的化合物,將其與含羥基的有機化合物反應而導入。氰基烷基化率可藉由NMR或元素分析所得的含氮率以計算。
本發明所使用的含羥基-氰基烷基的樹脂(A)中,羥基與氰基烷基的比例,以「羥基:氰基烷基」的莫耳比,較佳為50:50~2:98,更佳為30:70~2:98,再更佳為15:85~2:98。羥基的比例過低的話(氰基烷基化率過高的話),所得的閘極絕緣膜的耐藥品性具有降低的傾向。另一方面,羥基的比例高的話(氰基烷基化率過低的話),所得的閘極絕緣膜具有介電常數下降的傾向。
分子內具有2個以上環氧基的環氧化合物(B)(以下僅稱
為「環氧化合物(B)」),只要是具有2個以上環氧基的化合物即可,並沒有特別的限定。而且,作為環氧基,可為末端環氧基或脂環式環氧基的其中之一。
作為此種的環氧化合物(B),例如雙酚A型環氧化合物、雙酚F型環氧化合物、苯酚酚醛清漆型環氧化合物、甲酚酚醛清漆型環氧化合物、聚苯酚型環氧化合物、環狀脂肪族環氧化合物、環氧丙基醚基化合物、含環氧基的丙烯酸酯聚合物等。這些之中,由更為提升所得的閘極絕緣膜的耐蝕刻性的觀點,較佳是具有芳香族烴結構的環氧樹脂,更佳為具有2-[4-(2,3-環氧基丙氧基)苯基]-2-[4-[1,1-雙[4-([2,3-環氧基丙氧基]苯基)]乙基]苯基]丙烷、肆(環氧丙基氧基苯基)乙烷、萘結構、或茀結構的環氧化合物。尚且,這些可單獨使用1種或併用2種以上。
作為環氧化合物(B)的具體例,可舉出:雙酚A型環氧化合物(商品名「jER827、jER828、jER828EL、jER828XA、jER834、jER1001、jER1002、jER1003、jER1007、jER1009、jER1010、jER980U」(以上三菱化學公司製))、雙酚F型環氧化合物(商品名「jER806、jER806H、jER4004P、jERYL983U」(以上三菱化學公司製))、具有萘骨架的環氧化合物(商品名「Epiclon HP-4032、HP-4032D、HP-4700、HP-4710、HP-4770、HP-5000」(以上DIC公司製))、聯苯二亞甲基型的環氧化合物(商品名「NC-3000」,日本化藥公司製)、芳香族胺型的環氧化合物(商品名「H-434」,東都化成工業公司製)、甲酚酚醛清漆型環氧化合物(商品名
「ECON-1020」,日本化藥公司製)、苯酚酚醛清漆型環氧樹脂(商品名「Epicoat152、154」(以上、三菱化學公司))、苯酚芳烷基型環氧化合物(商品名「NC-2000」,日本化藥公司製)、雙酚A酚醛清漆型環氧化合物(商品名「jER157S」,三菱化學公司製)、2-[4-(2,3-環氧基丙氧基)苯基]-2-[4-[1,1-雙[4-([2,3-環氧基丙氧基]苯基)]乙基]苯基]丙烷(商品名「NC-6000」,日本化藥公司製)、肆(環氧丙基氧基苯基)乙烷(商品名「jER1030S」,三菱化學公司製,「TEP-G」旭有機材工業公司製)二氫蒽型環氧化合物(商品名「XY8800」,三菱化學公司製)等的具有芳香族烴結構的環氧化合物。
以二環戊二烯結構作為骨架的3官能性的環氧化合物(上品名「XD-1000」,日本化藥公司製)、2,2-雙(羥基甲基)1-丁醇的1,2-環氧基-4-(2-環氧乙烷基)環己烷加成物(具有環己烷骨架以及末端環氧基的15官能性的脂環式環氧樹脂,商品名「EHPE3150」,Daicel化學工業公司製)、環氧化3-環氧己烷-1,2-二羧酸雙(3-環己烯基甲基)修飾ε-己內酯(脂肪族環狀3官能性的環氧樹脂,商品名「Epilead-GT301」,Daicel化學工業公司製)、環氧化丁烷四羧酸肆(3-環己烯基甲基)修飾ε-己內酯(具有脂環式環氧基的脂肪族環狀4官能性的環氧樹脂、商品名「Epilead-GT401」,Daicel化學工業公司製)、鏈狀烷基多官能環氧化合物(商品名「SR-TMP」,阪本藥品工業股份有限公司製)、(3',4'-環氧基環己烷)甲基-3,4-環氧基環己烷羧酸酯(商品名「Celloxide 2021P」,Daicel化學工業公司製)等的不具有芳香族烴結構的環氧樹脂等。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的環氧樹脂(B)的含量,較佳為1~100重量份,更佳為5~80重量份,更佳為10~50重量份。藉由使環氧樹脂(B)的含量於上述範圍,能夠適當的提高所得的閘極絕緣膜的耐藥品性以及耐蝕刻性。
作為本發明所使用的分子內具有2個以上羥基、且羥基值為150~300mgKOH/g的硬化劑(C)(以下僅稱為「硬化劑(C)」),只要是具有2個以上羥基化合物即可,並沒有特別的限制,但較佳為具有酚性羥基作為羥基的化合物。作為硬化劑(C),藉由使用與環氧基反應的羥基為酚性羥基的化合物,能夠提升所得的閘極絕緣膜的耐乾蝕刻性。硬化劑(C)藉由其羥基,與上述環氧化合物(B)所含有的環氧基反應,藉此對於環氧化合物(B)作用為硬化劑,而且,藉由與後述的交聯劑(D)所含有的烷氧基甲基反應,對於交聯劑(D)亦作用為硬化劑。
作為硬化劑(C),只要是分子內具有2個以上羥基、且羥基值為150~300mgKOH/g之範圍的化合物即可,並沒有特別的限制,例如可舉出:苯酚、甲酚、間苯二酚、鄰苯二酚、雙酚A、雙酚F、苯基苯酚、胺基苯酚等的苯酚類以及/或是α-萘酚、β-萘酚、二氫萘等的萘酚類與甲醛、苯甲醛、水楊醛等的具有醛基的化合物於酸性觸媒下縮合或共縮合而得的酚醛清漆型苯酚樹脂、苯酚類以及/或是萘酚類與二甲氧基
對二甲苯或雙(甲氧基甲基)苯合成的苯酚.芳烷基樹脂、聯伸苯基型苯酚.芳烷基樹脂、萘酚.芳烷基樹脂等的芳烷基型苯酚樹脂、苯酚類以及/或是萘酚類與二環戊二烯共聚合而合成的二環戊二烯型苯酚酚醛清漆樹脂、二環戊二烯型萘酚酚醛清漆樹脂等的二環戊二烯型苯酚樹脂、三苯基甲烷型苯酚樹脂、萜烯改質苯酚樹脂、對二甲苯基以及/或是鄰二甲苯基改質苯酚樹脂、三聚氰胺改質苯酚樹脂、環戊二烯改質苯酚樹脂、聯苯型苯酚樹脂、這些2種以上共聚合所得的苯酚樹脂等。這些可單獨使用或組合2種以上使用。
而且,作為硬化劑(C),如為羥基值在150~300mgKOH/g之範圍的化合物即可,但此羥基值較佳為160~250mgKOH/g,更佳為175~220mgKOH/g。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的硬化劑(C)的含量,較佳為1~100重量份,更佳為3~80重量份,再更佳為5~50重量份。藉由使硬化劑(C)的含量於上述範圍,能夠使所得的閘極絕緣膜的強度適當。
本發明的樹脂組合物,除了上述的含羥基-氰基烷基的樹脂(A)、環氧化合物(B)、以及硬化劑(C)以外,含有下述一般式(1)所表示的結構的交聯劑(D)(以下僅稱為「交聯劑(D)」)
上述一般式(1)中,,R1、R2為碳數1~20的烷基,由對於上述含羥基-氰基烷基的樹脂(A)之溶解性的觀點,較佳為碳數1~10的烷基,更佳為碳數1~3的烷基。而且,R1與R2可彼此相同或是不同。
作為本發明所使用的交聯劑(D),只要是具有上述一般式(1)所表示的結構的交聯劑(D)即可,並沒有特別的限制,但例如較佳是下述一般式(2)~(4)所示的化合物。
(上述一般式(2)~(4)中,R1、R2與前述一般式(1)相同,上述一般式(3)中,R3、R4為碳數1~20的烷基,較佳為碳數1~10的烷基,更佳為碳數1~3的烷基。而且,上述一
般式(3)中,R1、R2、R3、R4的全部或是任一可為相同,亦可以全部不同。)
而且,作為本發明所使用交聯劑(D)的具體例,可舉出下述(5)~(10)所表示的化合物,這些之中,由使本發明的作用效果更為顯著的觀點,較佳為下述式(7)、(9)所示的化合物,更佳為下述式(9)所表示的化合物。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的交聯劑(D)的含量,較佳為0.1~100重量份,更佳為1~50重量份,再更佳為5~20重量份。藉由使交聯劑(D)的含量於上述範圍,能夠使所得的閘極絕緣膜的耐藥品性以及密著性更為提高,進而膜形成後進行高溫處理時的密著性更為提高。
而且,本發明的樹脂組合物,除了上述各成分之外,亦可以含有分子內具有酚性的羥基、且羥基值未滿150mgKOH/g的酚類化合物(E)(以下僅稱「酚類化合物(E)」)。藉由進一步含有羥基值未滿150mgKOH/g的酚類化合物(E),能夠抑制膜形成後的燒結所致的密著性降低,並提高耐藥品性。
作為本發明所用的酚類化合物(E),只要是羥基值未滿150mgKOH/g,且具有酚性的羥基者即可,並沒有特別的限制,例如可舉出:苯酚、甲酚、間苯二酚、鄰苯二酚、雙酚A、雙酚F、苯基苯酚、胺基苯酚等的苯酚類以及/或是α-萘酚、β-萘酚、二氫萘等的萘酚類與甲醛、苯甲醛、水楊醛等的具有醛基的化合物於酸性觸媒下縮合或共縮合而得的酚醛清漆型苯酚樹脂、苯酚類以及/或是萘酚類與二甲氧基對二甲苯或雙(甲氧基甲基)苯合成的苯酚.芳烷基樹脂、聯伸苯基型苯酚.芳烷基樹脂、萘酚.芳烷基樹脂等的芳烷基型苯酚樹脂、苯酚類以及/或是萘酚類與二環戊二烯共聚合而合成的二環戊二烯型苯酚酚醛清漆樹脂、二環戊二烯型萘酚酚醛清漆樹脂等的二環戊二烯型苯酚樹脂、三苯基甲烷型苯酚樹脂、萜烯改質苯酚樹脂、對二甲苯基以及/或是鄰二甲苯基改質苯酚樹脂、三聚氰胺改質苯酚樹脂、環戊二烯改質苯酚樹脂、聯苯型苯酚樹脂、這些2種以上共聚合所得的苯酚樹脂等。這些可單獨使用或組合2種以上使用。
而且,作為酚類化合物(E),只要是羥基值未滿150mgKOH/g即可,但其羥基值較佳為50~140mgKOH/g,更佳為80~120mgKOH/g。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的酚類化合物(E)的含量,較佳為0.1~100重量份,更佳為1~50重量份,再更佳為5~20重量份。藉由使酚類化合物(E)的含量於上述範圍,能夠進一步提高其添加效果。而且,相對於含羥基-氰基烷基的樹脂(A)100重量份,酚類化合物(E)的含量以與上述硬化劑(C)的合計量計(亦即酚類化合物(E)與硬化劑(C)的合計量),較佳為成為1~100重量份之範圍的量,更佳為5~50重量份,再更佳為10~40重量份。藉由使酚類化合物(E)與硬化劑(C)的含量於上述範圍,能夠使所得的閘極絕緣膜的耐藥品性以及密著性更為提高,進而膜形成後進行高溫處理時的密著性更為提高。酚類化合物(E)與硬化劑(C)相同,藉由其羥基,與上述環氧化合物(B)所含有的環氧基反應,藉此對於環氧化合物(B)作用為硬化劑,而且,藉由與後述的交聯劑(D)所含有的烷氧基甲基反應,對於交聯劑(D)亦作用為硬化劑。
而且,本發明的樹脂組合物除了上述各成分之外,亦可含有硬化觸媒(F)。作為硬化觸媒(F),例如可舉出具有酸性基或熱潛性酸性基的化合物,以及具有鹼性基或熱潛性鹼性基的化合物。具有酸性基或熱潛性酸性基的化合物,只要具有酸性基或是經由加熱或光產生酸的熱潛性酸性基即可,不特別限定,較佳為脂肪族化合物、芳香族化合物、雜環化合物,更佳為芳香族化合物、雜環化合物。具有鹼性基或熱潛性鹼性基的化合物,只要具有鹼性基或是經由加熱產生鹼的熱潛性鹼性基
即可,不特別限定,較佳為脂肪族化合物、芳香族化合物、雜環化合物,更佳為芳香族化合物、雜環化合物。藉由調配硬化觸媒(F),能夠降低使本發明的樹脂組合物硬化時之硬化所需的加熱能源(加熱時間以及加熱溫度)。
具有酸性基的化合物的酸性基之數目不特別限定,較佳為具有合計2個以上的酸性基。酸性基可彼此相同或不同。
作為酸性基只要是酸性官能基即可,其具體例,例如可舉出:磺酸基、磷酸基等強酸性基;羧基、硫醇基及羧基亞甲硫基等弱酸性基。這些之中,較佳為羧基、硫醇基或羧基亞甲硫基,特佳為羧基。而且,這些酸性基之中,較佳酸解離常數pKa為3.5以上5.0以下之範圍者。而且,具有2個以上酸性基時,第1解離常數pKa1作為酸解離常數,第1解離常數pKa1較佳為在上述範圍。又,pKa係於稀薄水溶液條件下,測定酸解離常數Ka=[H3O+][B-]/[BH],且pKa=-logKa而求得。此處的BH表示有機酸,B-表示有機酸之共軛鹼。
又,pKa之測定方法,例如使用pH計測定氫離子濃度,從該物質之濃度及氫離子濃度計算得到。
而且,具有酸性基或熱潛性酸性基的化合物可具有酸性基以及熱潛性酸性基以外的取代基。
作為此種取代基,例如可舉出:烷基、芳基等烴基;除此以外,例如:鹵素原子;烷氧基、芳氧基、醯氧基、雜環氧基;烷基、芳基或雜環基所取代之胺基、醯基胺基、脲基、胺磺醯基胺基、烷氧羰基胺基、芳氧基羰基胺基;烷硫基、芳硫基、
雜環硫基;等不具有質子的極性基、以此些不具有質子之極性基取代的烴基等。
這些具有酸性基或熱潛性酸性基的化合物中,具有酸性基的化合物的具體例,例如可舉出:甲酸、乙酸、丙酸、丁酸、戊酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、甘醇酸、甘油酸、乙二酸(也稱為草酸)、丙二酸(也稱為蘋果酸(malonic acid))、丁二酸(也稱為琥珀酸)、戊二酸、己二酸(也稱為adipic acid)、1,2-環己烷二羧酸、2-含氧丙酸、2-羥基丁二酸、2-羥基丙烷三羧酸、巰基琥珀酸、二巰基琥珀酸、2,3-二巰基-1-丙醇、1,2,3-三巰基丙烷、2,3,4-三巰基-1-丁醇、2,4-二巰基-1,3-丁二醇、1,3,4-三巰基-2-丁醇、3,4-二巰基-1,2-丁二醇、1,5-二巰基-3-硫雜戊烷等脂肪族化合物;
苯甲酸、對羥基苯羧酸、鄰羥基苯羧酸、2-萘羧酸、苯甲酸甲酯、苯甲酸二甲酯、苯甲酸三甲酯、丙酸3-苯酯、二羥基苯甲酸、二甲氧基苯甲酸、苯-1,2-二羧酸(也稱為鄰苯二甲酸)、苯-1,3-二羧酸(也稱為間苯二甲酸)、苯-1,4-二羧酸(也稱為對苯二甲酸)、苯-1,2,3-三羧酸、苯-1,2,4-三羧酸、苯-1,3,5-三羧酸、苯六羧酸、聯苯-2,2'-二羧酸、2-(羧基甲基)苯甲酸、3-(羧基甲基)苯甲酸、4-(羧基甲基)苯甲酸、2-(羧基羰基)苯甲酸、3-(羧基羰基)苯甲酸、4-(羧基羰基)苯甲酸、2-巰基苯甲酸、4-巰基苯甲酸、二酚酸、2-巰基-6-萘羧酸、2-巰基-7-萘羧酸、1,2-二巰基苯、1,3-二巰基苯、1,4-二巰基苯、1,4-萘二硫醇、1,5-萘二硫醇、2,6-萘二硫醇、2,7-萘二硫醇、1,2,3-三巰基苯、1,2,4-三巰基苯、1,3,5-三巰基苯、
1,2,3-參(巰基甲基)苯、1,2,4-參(巰基甲基)苯、1,3,5-參(巰基甲基)苯、1,2,3-參(巰基乙基)苯、1,2,4-參(巰基乙基)苯、1,3,5-參(巰基乙基)苯等芳香族化合物;
菸鹼酸、異菸鹼酸、2-呋喃甲酸、吡咯-2,3-二羧酸、吡咯-2,4-二羧酸、吡咯-2,5-二羧酸、吡咯-3,4-二羧酸、咪唑-2,4-二羧酸、咪唑-2,5-二羧酸、咪唑-4,5-二羧酸、吡唑-3,4-二羧酸、吡唑-3,5-二羧酸等含氮原子之五員雜環化合物;噻吩-2,3-二羧酸、噻吩-2,4-二羧酸、噻吩-2,5-二羧酸、噻吩-3,4-二羧酸、噻唑-2,4-二羧酸、噻唑-2,5-二羧酸、噻唑-4,5-二羧酸、異噻唑-3,4-二羧酸、異噻唑-3,5-二羧酸、1,2,4-噻二唑-2,5-二羧酸、1,3,4-噻二唑-2,5-二羧酸、3-胺基-5-巰基-1,2,4-噻二唑、2-胺基-5-巰基-1,3,4-噻二唑、3,5-二巰基-1,2,4-噻二唑、2,5-二巰基-1,3,4-噻二唑、3-(5-巰基-1,2,4-噻二唑-3-基硫烷基)琥珀酸、2-(5-巰基-1,3,4-噻二唑-2-基硫烷基)琥珀酸、(5-巰基-1,2,4-噻二唑-3-基硫)乙酸、(5-巰基-1,3,4-噻二唑-2-基硫)乙酸、3-(5-巰基-1,2,4-噻二唑-3-基硫)丙酸、2-(5-巰基-1,3,4-噻二唑-2-基硫)丙酸、3-(5-巰基-1,2,4-噻二唑-3-基硫)琥珀酸、2-(5-巰基-1,3,4-噻二唑-2-基硫)琥珀酸、4-(3-巰基-1,2,4-噻二唑-5-基)硫丁烷磺酸、4-(2-巰基-1,3,4-噻二唑-5-基)硫丁烷磺酸等含氮原子及硫原子的五員雜環化合物;
吡啶-2,3-二羧酸、吡啶-2,4-二羧酸、吡啶-2,5-二羧酸、吡啶-2,6-二羧酸、吡啶-3,4-二羧酸、吡啶-3,5-二羧酸、嗒井(pyridazine)-3,4-二羧酸、嗒井-3,5-二羧酸、嗒井-3,6-二羧酸、嗒井-4,5-二羧酸、嘧啶-2,4-二羧酸、嘧啶-2,5-二羧酸、
嘧啶-4,5-二羧酸、嘧啶-4,6-二羧酸、吡嗪(pyrazine)-2,3-二羧酸、吡嗪-2,5-二羧酸、吡啶-2,6-二羧酸、三嗪-2,4-二羧酸、2-二乙基胺基-4,6-二巰基-s-三嗪、2-二丙基胺基-4,6-二巰基-s-三嗪、2-二丁基胺基-4,6-二巰基-s-三嗪、2-苯胺基-4,6-二巰基-s-三嗪、2,4,6-三巰基-s-三嗪等含氮原子之六員雜環化合物。
熱潛性酸性基只要是藉由光或加熱而產生酸性的官能基的基即可,作為其具體例,可舉出鋶鹽基、苯并噻唑鹽基、銨鹽基、鏻鹽基、錪鹽基、封端羧酸(blocked carboxylic acid)基。這些之中,較佳為鋶鹽基,例如可使用六氟化磷系或六氟化銻系的鋶鹽基。作為具有此種鋶鹽基的化合物,例如可使用Sanaid SI系列(100L,110L,150、180L,三新化學工業公司製)等。
作為鹼性基,只要是具有鹼性的官能基即可,作為其具體例,可舉出胺基、含氮雜環。作為含胺基的化合物,可舉出六亞甲基二胺等的脂肪族聚胺類;4,4'-二胺基二苯基醚、二胺基二苯基碸等的芳香族聚胺類。作為含氮雜環化合物,例如2-甲基咪唑(品名;2MZ)、4-甲基-2-乙基咪唑(品名;2E4MZ)、2-苯基咪唑(品名;2PZ)、4-甲基-2-乙基咪唑(品名;2P4MZ)、1-苄基-2甲基咪唑(品名;1B2MZ)、2-乙基咪唑(品名;2EZ)、2-異丙基咪唑(品名;2IZ)、1-氰基乙基-2-甲基咪唑(品名;2MZ-CN)、1-氰基乙基-2-乙基-4-甲基咪唑(品名;2E4MZ-CN)、1-氰基乙基-2-十一烷基咪唑(品名;C11Z-CN)等。
作為具有熱潛性鹼性基的化合物,只要是藉由光或加熱而
產生鹼性的官能基的化合物即可。作為其具體例,可舉出WPBG-018、WPBG-027、WPBG-082、WPBG-140(以上為和光純藥工業公司製)等。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的硬化觸媒(F)的含量,較佳為0.01~50重量份,更佳為0.1~20重量份,更佳為1~10重量份。藉由使硬化觸媒(F)的含量於上述範圍,能夠有效的降低樹脂組合物硬化時之硬化所需的熱能,藉此能夠降低製造成本。
於本發明所使用樹脂組合物中,也可更含有溶劑。作為溶劑並沒有特別的限制,作為樹脂組合物的溶劑之公知溶劑,例如可舉出:丙酮、甲乙酮、環戊酮、2-己酮、3-己酮、2-庚酮、3-庚酮、4-庚酮、2-辛酮、3-辛酮、4-辛酮等直鏈酮類;正丙醇、異丙醇、正丁醇、環己醇等醇類;乙二醇二甲醚、乙二醇二乙醚、二噁烷等醚類;乙二醇單甲醚、乙二醇單乙醚等醇醚類;甲酸丙酯、甲酸丁酯、乙酸丙酯、乙酸丁酯、丙酸甲酯、丙酸乙酯、丁酸甲酯、丁酸乙酯、乳酸甲酯、乳酸乙酯等酯類;賽路蘇(cellosolve)乙酸酯、甲基賽路蘇乙酸酯、乙基賽路蘇乙酸酯、丙基賽路蘇乙酸酯、丁基賽路蘇乙酸酯等賽路蘇酯類;丙二醇、丙二醇單甲醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、丙二醇單丁醚等丙二醇類;二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇二甲醚、二乙二醇二乙醚、二乙二醇甲乙醚等二乙二醇類;γ-丁內酯、γ-戊內酯、γ-己內酯、γ-辛內酯等飽和γ-內酯類;三氯乙烯等鹵化烴類;甲苯、二甲苯等芳香
族烴類;二甲基乙醯胺、二甲基甲醯胺、N-甲基乙醯胺等極性溶劑等。這些溶劑可單獨使用也可組合2種以上使用。相對於含羥基-氰基烷基的樹脂(A)100重量份,溶劑的含量較佳為10~10000重量份,更佳為50~5000重量份,再更佳為100~1000重量份的範圍。而且,樹脂組合物中含有溶劑時,溶劑通常於閘極絕緣膜形成後除去。
而且,本發明的樹脂組合物,在不妨礙本發明效果的範圍,可視所望含有抗氧化劑、界面活性劑、耦合劑或其衍生物、增感劑、光安定劑、消泡劑、顏料、染料、填料等其他的調配劑等。這些之中,例如耦合劑或其衍生物、增感劑、光安定劑,可使用日本專利公開公報特開2011-75609號公報所記載者。
作為抗氧化劑,沒有特別的限制,可使用通常的聚合物使用的苯酚系抗氧化劑、磷系抗氧化劑、硫系抗氧化劑、胺系抗氧化劑、內酯系抗氧化劑等。藉由含有抗氧化劑,能夠提昇所得的閘極絕緣膜的耐光性、耐熱性。
作為苯酚系抗氧化劑,例如可使用:2-第三丁基-6-(3-第三丁基-2-羥基-5-甲基苄基)-4-甲基苯基丙烯酸酯、2,4-二第三戊基-6-[1-(3,5-二第三戊基-2-羥基苯基)乙基]苯基丙烯酸酯等日本專利公開公報特開昭63-179953號公報或特開平1-168643號公報中記載的丙烯酸酯系化合物;2,6-二第三丁基-4-甲基苯酚、2,6-二第三丁基-4-乙基苯酚、十八基-3-(3,5-二第三丁基-4-羥基苯基)丙酸酯、2,2'-亞甲基-雙(4-甲基-6-第三丁基苯酚)、4,4'-亞丁基-雙(6-第三丁基間甲酚)、4,4'-
硫代雙(3-甲基-6-第三丁基苯酚)、雙(3-環己基-2-羥基-5-甲基苯基)甲烷、3,9-雙〔2-[3-(3-第三丁基-4-羥基-5-甲基苯基)丙醯基氧基]-1,1-二甲基乙基〕-2,4,8,10-肆氧螺[5,5]十一烷、1,1,3-參(2-甲基-4-羥基-5-第三丁基苯基)丁烷、季戊四醇-肆[3-(3,5-二第三丁基-4-羥基苯基)丙酸酯]、三乙二醇雙[3-(3-第三丁基-4-羥基-5-甲基苯基)丙酸酯]、生育酚等烷基取代苯酚系化合物;6-(4-羥基-3,5-二第三丁基苯胺基)-2,4-雙-辛基硫-1,3,5-三嗪(triazine)、6-(4-羥基-3,5-二甲基苯胺基)-2,4-雙-辛基硫-1,3,5-三嗪、6-(4-羥基-3-甲基-5-第三丁基苯胺基)-2,4-雙-辛基硫-1,3,5-三嗪、2-辛基硫-4,6-雙-(3,5-二第三丁基-4-氧基苯胺基)-1,3,5-三嗪等含三嗪基苯酚化合物等。
作為磷系抗氧化劑,只要是一般樹脂工業通常使用者即可,並沒有特別的限制,例如可使用:三苯基亞磷酸酯、二苯基異癸基亞磷酸酯、苯基二異癸基亞磷酸酯、參(壬基苯基)亞磷酸酯、參(二壬基苯基)亞磷酸酯、參(2,4-二第三丁基苯基)亞磷酸酯、參(2-第三丁基-4-甲基苯基)亞磷酸酯、參(環己基苯基)亞磷酸酯、2,2'-亞甲基雙(4,6-二第三丁基)辛基亞磷酸酯、9,10-二氫-9-氧雜-10-膦菲-10-氧化物、10-(3,5-二第三丁基-4-羥基苄基)-9,10-二氫-9-氧雜-10-膦菲-10-氧化物、10-癸氧基-9,10-二氫-9-氧雜-10-膦菲等的單亞磷酸酯系化合物;4,4'-亞丁基-雙(3-甲基-6-第三丁基-二-三癸基亞磷酸酯)、4,4'-異亞丙基-雙[苯基二烷基(C12~C15)亞磷酸酯]、4,4'-異亞丙基-雙[二苯基單烷基(C12~C15)亞磷酸酯]、1,1,3-
參(2-甲基-4-二-三癸基亞磷酸酯-5-第三丁基苯基)丁烷、肆(2,4-二第三丁基苯基)-4,4'-聯苯基二亞磷酸酯、環新戊烷四基雙(十八基亞磷酸酯)、環新戊烷四基雙(異癸基亞磷酸酯)、環新戊烷四基雙(壬基苯基亞磷酸酯)、環新戊烷四基雙(2,4-二第三丁基苯基亞磷酸酯)、環新戊烷四基雙(2,4-二甲基苯基亞磷酸酯)、環新戊烷四基雙(2,6-二第三丁基苯基亞磷酸酯)等的二亞磷酸酯系化合物。這些之中,較佳為單亞磷酸酯系化合物,特佳為參(壬基苯基)亞磷酸酯、參(二壬基苯基)亞磷酸酯、參(2,4-二第三丁基苯基)亞磷酸酯等。
作為硫系抗氧化劑,例如可使用:3,3'-硫二丙酸二月桂酯、3,3'-硫二丙酸二肉豆蔻酯、3,3'-硫二丙酸二硬脂酯、3,3'-硫二丙酸月桂基硬脂酯、季戊四醇肆-(β-月桂基硫丙酸酯)、3,9-雙(2-十二基硫乙基)-2,4,8,10-肆氧螺[5,5]十一烷等。
這些抗氧化劑,可個別單獨使用或組合2種以上使用。
相對於含羥基-氰基烷基的樹脂(A)100重量份,本發明的樹脂組合物中的抗氧化劑的含量較佳為0.1~10重量份,更佳為1~5重量份。如使抗氧化劑的含量於上述範圍內,可以得到閘極絕緣膜的耐光性以及耐熱性良好的閘極絕緣膜。
界面活性劑是為了條紋(塗佈條痕)等的防止之目的而使用。作為界面活性劑,例如可舉出矽酮系界面活性劑、氟系界面活性劑、聚氧伸烷基系界面活性劑、甲基丙烯酸共聚物系界面活性劑、丙烯酸共聚物系界面活性劑。
作為矽酮系界面活性劑,例如可舉出:「SH28PA」、「SH29PA、SH30PA、ST80PA、ST83PA、ST86PA、SF8416、SH203、SH230、SF8419、SF8422、FS1265、SH510、SH550、SH710、SH8400、SF8410、SH8700、SF8427」(以上為Toray Dow Corning公司製),商品名「KP-321、KP-323、KP-324、KP-340、KP-341」(以上為信越化學工業股份有限公司製),商品名「TSF400、TSF401、TSF410、TSF4440、TSF4445、TSF4450、TSF4446、TSF4452、TSF4460(以上為Momentive Performance Materials Japan合同會社製),商品名「BYK300、BYK301、BYK302、BYK306、BYK307、BYK310、BYK315、BYK320、BYK322、BYK323、BYK331、BYK333、BYK370、BYK375、BYK377、BYK378」(以上為BYK Japan公司製)等。
作為氟系界面活性劑,例如可舉出:Fluorient「FC-430、FC-431」(以上為住友3M股份有限公司製),Surflon「S-141、S-145、S-381、S-393」(以上為旭硝子股份有限公司製),Eftop(註冊商標)「EF301、EF303、EF351、EF352」(以上為JEMCO股份有限公司製),MEGAFACE(註冊商標)「F171、F172、F173、R-30」(以上為DIC股份有限公司製)。
作為聚氧伸烷基系界面活性劑,例如可舉出:聚氧伸乙基月桂醚、聚氧伸乙基硬脂醚、聚氧伸乙基油醚、聚氧伸乙基辛基苯醚、聚氧伸乙基壬基苯醚等聚氧伸乙基烷醚類;聚乙二醇二月桂酸酯、聚乙二醇二硬脂酸酯聚氧伸乙基二烷基酯類等。
這些界面活性劑,可個別單獨使用或組合2種以上使用。
相對於含羥基-氰基烷基的樹脂(A)100重量份,
本發明的樹脂組合物中的界面活性劑的含量較佳為0.01~0.5重量份,更佳為0.02~0.2重量份。如使界面活性劑的含量於上述範圍內,能夠提高條紋(塗佈條痕)的防止效果。
本發明所使用的樹脂組合物的製備方法不特別限定,可將構成樹脂組合物的各成分以公知的方法混合即可。
混合的方法不特別限定,較佳為將構成樹脂組合物的各成分溶解或分散於溶劑而獲得的溶液或分散液混合。藉此,樹脂組合物能以溶液或分散液的形態獲得。
將構成樹脂組合物的各成分溶解或分散於溶劑的方法,可依照常法實施。具體而言,可利用使用攪拌子與磁性攪拌器的攪拌、高速均質機、分散器、行星攪拌機、雙軸攪拌機、球磨機、三輥等進行。而且,將各成分溶解或分散於溶劑後,可例如使用孔徑為0.1μm左右的過濾器等過濾。
其次,對本發明的閘極絕緣膜進行說明。本發明的閘極絕緣膜由上述本發明的樹脂組合物所構成,通常用於薄膜電晶體。
於下述中,以本發明的閘極絕緣膜適用於底閘極型的薄膜電晶體的情形為例進行說明。此處,第1圖所示為作為本發明的閘極絕緣膜所適用的薄膜電晶體的一例之底閘極型的薄膜電晶體1的剖面圖。作為本發明的閘極絕緣膜所適用的薄膜電晶體,只要是具有如第1圖所示結構的薄膜電晶體則沒有任何限制。
如第1圖所示,作為本發明的閘極絕緣膜所適用
的薄膜電晶體的一例之底閘極型的薄膜電晶體1,在基板2上具有閘極電極3、上述本發明的樹脂組合物所構成的閘極絕緣膜4、半導體層5、源極電極6以及汲極電極7、保護層8。尚且,於第1圖中雖然顯示單一的薄膜電晶體1,但是亦可為在基板2上形成複數的薄膜電晶體1的此種構成(例如主動陣列基板等)。
作為基板2並沒有特別的限定,例如可舉出聚碳酸酯、聚醯亞胺、聚對苯二甲酸乙二酯、脂環式烯烴聚合物等具有柔軟性的塑膠所構成的可撓性基板,石英、鈉玻璃、無機鹼玻璃等的玻璃基板,矽晶圓等的矽基板等。
閘極電極3由導電性材料所形成。作為導電性材料,例如可舉出鉑、金、銀、鎳、鉻、銅、鐵、錫、銻鉛、鉭、銦、鈀、碲、錸、銥、鋁、釕、鍺、鉬、鎢、氧化錫.銻、氧化銦.錫(ITO)、氟摻雜氧化鋅、鋅、碳、石墨、玻璃碳、銀膠以及碳膠、鋰、鈹、鎂、鉀、鈣、鈧、鈦、錳、鋯、鎵、鈮、鈉、鈉-鉀合金、鎂/銅混合物、鎂/銀混合物、鎂/鋁混合物、鎂/銦混合物、鋁/氧化鋁混合物、鋰/鋁混合物、鋁/鈦混合物、鉬/鈦混合物等。而且,藉由摻雜等而提昇導電率的公知的導電性高分子,例如可舉出導電性聚苯胺、導電性聚吡咯、導電性聚噻吩(聚乙烯二氧基噻吩與聚苯乙烯磺酸的錯合物)等。
閘極絕緣膜4由上述本發明的樹脂組合物所構成,在以規定圖案形成有閘極電極3的基板2上塗佈上述本發明的樹脂組合物,因應需要去除溶劑後藉由硬化而形成。
半導體層5為非晶質矽半導體、有機半導體或非
晶質氧化物半導體所構成的層,這些之中,由更為提高本發明的作用效果的觀點,特佳為由非晶質氧化物半導體所構成的層。半導體層5為由有機半導體所構成的層之情形,例如可使用稠五苯(pentacene)或聚噻吩衍生物、聚伸苯基伸乙烯基衍生物、聚伸噻吩基伸乙烯基衍生物、聚烯丙基胺衍生物、聚乙炔衍生物、並苯(acene)衍生物、寡噻吩等所代表的有機半導體材料。而且,半導體層5為由非晶質氧化物半導體所構成的層之情形,可為包含In、Ga以及Zn中的至少1種元素的非晶質氧化物半導體所構成的濺鍍膜。作為非晶質氧化物半導體,只要是包含In、Ga以及Zn中的至少1種元素者即可,例如可舉出氧化鋅(ZnO)、銦鋅氧化物(IZO)、鋅錫氧化物(ZTO)、鋁鋅氧化物(AZO)、鎵鋅氧化物(GZO)、銦鎵鋅氧化物(IGZO)等。
源極電極6以及汲極電極7由導電性材料所形成。作為導電性材料,可以使用與上述閘極電極3相同的材料。
保護層8是被覆並保護包含基板2、閘極電極3、閘極絕緣膜4、半導體層5、源極電極6以及汲極電極7的各構成要素的露出表面之層。作為構成保護層8的材料例如可舉出:SiO2、SiONx、SiNx以及Al2O3等的無機膜,以及丙烯酸(acryl)、聚醯亞胺、環烯烴、環氧、酚醛清漆等的各種樹脂所構成的有機膜。尚且,此保護層8可為單層,亦可為多層。尚且,本實施型態的薄膜電晶體1構成為具備保護層8,但是亦可以不具備保護層8。
其次,對使用非晶質氧化物半導體作為半導體層5
之情形的第1圖所示的薄膜電晶體1的製造方法進行說明。第2圖所示為薄膜電晶體1的製造步驟的圖。
首先,在基板2上,將用以形成閘極電極3的導電性材料所構成的層,藉由濺鍍法等形成在基板2上。其次,藉由微影法形成抗蝕劑圖案(未圖示),以抗蝕劑圖案作為罩幕,對於導電性材料所構成的層,以濕蝕刻法進行蝕刻,其次,藉由剝離抗蝕劑圖案,如第2(A)圖所示,在基板2上形成閘極電極3。
其次,如第2(B)圖所示,於形成有閘極電極3的基板2上塗佈本發明的樹脂組合物,因應需要去除溶劑之後,藉由硬化形成閘極絕緣膜4。作為樹脂組合物的塗佈方法,例如噴塗法、旋塗法、輥塗法、模塗法、刮刀法、旋轉塗佈法、棒塗法、網板印刷法等的各種方法。而且,硬化溫度(交聯溫度)通常為100~300℃,更佳為100~250℃,再更佳為100~230℃,硬化時間通常為0.5~300分鐘,較佳為1~150分鐘,更佳為1~60分鐘。閘極絕緣膜4的厚度並沒有特別的限定,較佳為100~2000nm,更佳為100~1000nm,再更佳為100~500nm。
其次,如第2(C)圖所示,在形成有閘極電極3以及閘極絕緣膜4的基板2之閘極絕緣膜4上形成半導體層5。具體而言,首先在閘極絕緣膜4上使用濺鍍法,將包含In、Ga以及Zn中的至少1種元素的非晶質氧化物半導體所構成的層(以下稱為「非晶質氧化物半導體層」),形成於閘極絕緣膜4的表面整體。非晶質氧化物半導體例如在半導體層5以銦鎵鋅氧化物(IGZO)形成的情形,使用將氧化銦(In2O3)、氧化
鎵(Ga2O3)、以及氧化鋅(ZnO)個別以等莫耳混合並燒結的靶材,藉由直流(Direct Current)濺鍍法成膜。尚且,濺鍍可在腔室內導入流量100~300sccm的氬(Ar)氣與流量5~20sccm的氧(O2)氣以進行。而且,此時的基板溫度為150~400℃。尚且,形成非晶質氧化物半導體層之後,亦可以於200~500℃的大氣氣體環境中進行1~2小時程度的回火。其次,於所形成的非晶質半導體層的表面形成規定的抗蝕劑圖案,並以抗蝕劑圖案為罩幕,以乾蝕刻法對非晶質氧化物半導體層進行蝕刻,其後藉由剝離抗蝕劑圖案,如第2(C)圖所示,在閘極絕緣膜4上形成半導體層5。
其次,如第2(D)圖所示,在閘極絕緣膜4以及半導體層5上形成源極電極6以及汲極電極7。具體而言,首先,使用濺鍍法,在基板2、閘極絕緣膜4以及半導體層5的上面之全面,形成用於形成源極電極6以及汲極電極7之不同導電性材料所構成的層。其次,於所形成的導電性材料所構成的層上,利用微影法形成與源極電極6以及汲極電極7的形狀對應的抗蝕劑圖案。然後,以所形成的抗蝕劑圖案為罩幕,藉由乾蝕刻法蝕刻導電性材料所構成的層,其後藉由剝離抗蝕劑圖案,如第2(D)圖所示,形成源極電極6以及汲極電極7。
其次,以覆蓋閘極絕緣膜4、半導體層5、源極電極6以及汲極電極7的上面(露出面)的全體之方式形成保護層(鈍化膜)8,以製造如第1圖所示的底閘極型(通道蝕刻型)的薄膜電晶體1。保護層8使用前述的材料等,例如可以藉由電漿化學氣相沈積(CVD)法等而形成。依照上述,製造
第1圖所示的底閘極型的薄膜電晶體1。
於本發明中,於此種的底閘極型的薄膜電晶體1等的電子部件等所使用的閘極絕緣膜,其為上述的本發明的樹脂組合物所形成者。該樹脂組合物含有含羥基-氰基烷基的樹脂(A)、環氧化合物(B)、硬化劑(C)以及交聯劑(D),而且可提供介電常數高、耐藥品性以及密著性優良,而且膜形成後進行高溫處理時的密著性降低被適當防止的樹脂膜。因此,如依本發明,藉由使第1圖所示的薄膜電晶體1的閘極絕緣膜4由本發明的樹脂組合物而形成,在閘極絕緣膜4上形成半導體層5或源極電極6、汲極電極7時,即使暴露於顯影液或蝕刻液的情形,藉由其優良的耐藥品性,能夠有效的防止劣化所致的膜厚變動。再加上,根據本發明,於形成半導體層5或源極電極6、汲極電極7時,即使進行較高溫的燒結的情形,使用本發明的樹脂組合物所構成閘極絕緣膜4,由於為膜形成後進行高溫處理時的密著性降低被適當防止的樹脂膜,亦能夠有效的防止此種的燒結所致的密著性降低。特別是,使用本發明的樹脂組合物所得的閘極絕緣膜4,由於如此能夠有效防止劣化所致的膜厚變動或膜形成後進行高溫處理時的密著性降低,並達成高介電常數,因此如此所得的薄膜電晶體1等的電子部件的高性能化成為可能。
尚且,於上述中,是以第1圖所示的底閘極型的薄膜電晶體1為例進行說明,但本發明的閘極絕緣膜並不限定於此種的底閘極型的薄膜電晶體1,以第3圖所示的頂閘極型的薄膜電晶體1a起始,能夠適用於各種電子部件的閘極絕緣
膜。此處,第3圖所示為具備本發明的樹脂組合物所構成的閘極絕緣膜之頂閘極型的薄膜電晶體1a的剖面圖,與上述薄膜電晶體1為相同構成的部件附上相同的編號,並省略其說明。尚且,第3圖所示的頂閘極型的薄膜電晶體1a,於基板2上具有源極電極6、汲極電極7、半導體層5、上述本發明的樹脂組合物所構成的閘極絕緣膜4以及閘極電極3。
或者是,本發明的樹脂組合物所構成的閘極絕緣膜,可較佳的適用於如第4圖所示的蝕刻終止層型的薄膜電晶體1b的閘極絕緣膜。此處,第4圖所示為具備本發明的樹脂組合物所構成的閘極絕緣膜之蝕刻終止層型的薄膜電晶體1b的剖面圖,與上述薄膜電晶體1為相同構成的部件附上相同的編號,並省略其說明。第4圖所示的薄膜電晶體1b,除了以覆蓋通道部10的方式而形成的蝕刻終止層9之外,具有與上述第1圖所示的薄膜電晶體1相同的構成。如第4圖所示,於此薄膜電晶體1b中,構成為:以覆蓋半導體層5的端部附近以及蝕刻終止層9的端部附近的方式,個別設置源極電極6以及汲極電極7。尚且,於第4圖中所示為未形成保護膜8的態樣,但亦可以如同第1圖所示的薄膜電晶體1,在源極電極6、汲極電極7以及蝕刻終止層9上形成保護層8。
以下舉出實施例以及比較例,以對本發明進行更為具體的說明。除非另有註明,各例中的份以及%為重量基準。
尚且,各特性的定義以及評價方法如下所述。
使用各實施例以及各比較例中所製作的樹脂組合物,將樹脂組合物旋轉塗佈於矽晶圓上之後,使用熱板以110℃預烤2分鐘,以形成樹脂膜。其次,藉由於氮氣中以180℃加熱1小時,以得到形成有500nm厚的樹脂膜的矽晶圓所構成的樹脂膜試料。然後,使用所得的樹脂膜試料,以JIS C6481為基準,以10kHz(室溫)測定樹脂膜的介電常數。
使用各實施例以及各比較例中所製作的樹脂組合物,將樹脂組合物旋轉塗佈於玻璃基板上之後,使用熱板以110℃預烤2分鐘,以形成樹脂膜。其次,藉由於氮氣中以180℃加熱1小時,以得到形成有2μm厚樹脂膜的附樹脂膜的基板。
密著性試驗,藉由以下說明的表面-界面切削法(SAICAS法)以進行。亦即是,將上述所得的附樹脂膜的基板之樹脂膜的部份以刀具切割為1mm寬度,對於已切割的附樹脂膜的基板,於作為密著性測定裝置的DAIPLA WINTES公司的SAICAS DN-20型,使用作為切割刀的1.0mm寬、斜角(rake angle)20。、底角10。的單結晶鑽石製的切割刀,以水平速度0.2μm/秒、垂直速度0.02μm/秒切割試料,且切割刀切割至樹脂膜與玻璃基板表面的界面時,使垂直速度為0μm/秒而使切割刀與基板平行的移動以測定平行力FH[N]。然後,由所得的平行力FH[N]與切割刀的寬度w[m],依照式「P[N/m]=FH[N]/w[m]」而計算剝離強度P,並將所得的剝離強度P作為樹脂膜的密著性的值,以下述基準進行評價。
A:剝離強度P為100N/m以上
B:剝離強度P為80N/m以上、未滿100N/m
C:剝離強度P未滿80N/m
與上述「成膜後的密著性」的評價相同的得到形成有2μm厚度樹脂膜的附樹脂膜的基板,進而,藉由對依此所得之附樹脂膜的基板以220℃加熱1小時,得到附追加燒結樹脂膜的基板。然後,除了使用附追加燒結樹脂膜的基板以外,與上述「成膜後的密著性」的評價相同的求取剝離強度P,以相同的基準評價追加燒結後的密著性。
與上述「成膜後的密著性」的評價相同的得到樹脂膜試料,將所得的樹脂膜試料於丙酮中以25℃浸泡15分鐘,並測定浸泡前後的樹脂膜的厚度變化率,藉此進行耐藥品性的評價。尚且,浸泡前後的樹脂膜的厚度變化率,依照「浸泡前後的樹脂膜的厚度變化率(%)=(|浸泡後的樹脂膜的厚度-浸泡前的樹脂膜的厚度|/浸泡前的樹脂膜的厚度)×100」而計算。而且,耐藥品性依下述進行評價。
A:浸泡前後的樹脂膜的厚度變化率未滿10%
B:浸泡前後的樹脂膜的厚度變化率為10%以上、未滿20%
C:浸泡前後的樹脂膜的厚度變化率為20%以上
將作為含羥基-氰基烷基的樹脂(A)之氰基烷基化普魯蘭多醣(Pullulan)(商品名「Cyanoresin CR-S」,信越化學工業公司製,羥基:氰基乙基=10:90(莫耳比))100份、作為環氧
化合物(B)之肆(環氧丙基氧基苯基)乙烷(商品名「jER1031S」,三菱化學公司製)20份、作為硬化劑(C)之苯酚-芳烷基型樹脂(商品名「KAYAHARD GPH-65」,日本化藥公司製,羥基值:175mgKOH/g)10份、作為交聯劑(D)之上述式(9)所示的化合物(商品名「Nikalac MX270」,三和化學公司製)5份、作為苯酚化合物(E)之酚醛清漆型酚樹脂(商品名「PAPA-PN4」,旭有機材工業公司製,羥基值:104mgKOH/g)10份,作為硬化觸媒(F)之PF6 -系鋶鹽(商品名「Sanaid SI-110L」,三新化學工業公司製)份、3-環氧丙基丙基三甲氧基矽烷(商品名「Z6040」,Toray Dow Corning股份有限公司製,矽烷耦合劑)1份、以及作為溶劑之γ-丁內酯60份、丙二醇單甲醚乙酸酯40份混合並溶解後,以孔徑0.2μm的聚四氟乙烯製過濾器過濾,以製備樹脂組合物。
然後,使用上述所得的樹脂組合物,依照上述的方法進行介電常數、成膜後的密著性、追加燒結後的密著性以及耐藥品性的各試驗、評價。結果表示於表1。
於製備樹脂組合物時,除了將表1所示的各化合物使用表1所示的調配量以外,與實施例1相同的製備樹脂組合物,並相同的進行試驗、評價。結果表示於表1。
於製備樹脂組合物時,除了將表1所示的各化合物使用表1所示的調配量以外,與實施例1相同的製備樹脂組合物,並相同的進行試驗、評價。結果表示於表1。
尚且,表1中的各化合物如下所述。
.「氰基乙基化聚乙烯醇」為氰基乙基化聚乙烯醇(商品名「Cyanoresin CR-V」,信越化學工業公司製,羥基:氰基乙基=15:85(莫耳比),含羥基-氰基烷基的樹脂(A))
.「聚乙烯基苯酚」為聚乙烯基苯酚(商品名「Maruka Linker-MS4P」,丸善石油化學公司製,含有羥基但不含氰基烷基的樹脂)
.「環氧化合物(Epiclon HP4700)」為具有萘骨架的環氧化合物(商品名「Epiclon HP4700」,DIC公司製,環氧化合物(B))
.「環氧化合物(NC-6000)」為2-[4-(2,3-環氧基丙氧基)苯基]-2-[4-[1,1-雙[4-([2,3-環氧基丙氧基]苯基)]乙基]苯基]丙烷(商品名「NC-6000」,日本化藥公司製,環氧化合物(B))
.「環氧化合物(jERYX8800)」為蒽二氫化物型環氧樹脂(商品名「jERYX8800」,三菱化學公司製,環氧化合物(B))
.「硬化劑(MEH-7800)」為苯酚-芳烷基型樹脂(商品名「MEH-7800」,明和化成公司製,硬化劑(C),羥基值:175mgKOH/g)
.「硬化劑(MEH-7851)」為苯酚-聯苯基型樹脂(商品名「MEH-7851」,明和化成公司製,硬化劑(C),羥基值:220mgKOH/g)
.「式(7)所示的交聯劑(Nikalac MX280)」為上述式(7)所示的化合物(商品名「Nikalac MX280」,三和化學公司製,交聯劑(D))
.「三聚氰胺系交聯劑(Cylink 2000)」為三聚氰胺系交聯劑(商品名「Cylink 2000」,Cytec Industries公司製,三聚氰胺系交聯劑)
.「三聚氰胺系交聯劑(Cymel 350)」為三聚氰胺系交聯劑(商品名「Cymel 350」,Cytec Industries公司製,三聚氰胺系交聯劑
如表1所示,含有含羥基-氰基烷基的樹脂(A)、環氧樹脂(B)、硬化劑(C)以及具有上述一般式(1)所表示的結構的交聯劑(D)的本發明之樹脂組合物所構成的樹脂膜,任一的介電常數高、耐藥品性、成膜後的密著性以及追加燒結後的密著性優良,而適用於各種電子部件的閘極絕緣膜用途,特別是適用於底閘極型的薄膜電晶體的閘極絕緣膜用途(實施例1~11)。
另一方面,於使用三聚氰胺系交聯劑取代具有上述一般式(1)所表示的結構的交聯劑(D)的情形,所得的樹脂膜具有在追加燒結後密著性變差的結果(比較例1、2)。
而且,於未調配硬化劑(C)的情形,所得的樹脂膜亦具有在追加燒結後密著性變差的結果(比較例3)。
進而,於使用聚乙烯苯酚(含有羥基但不含氰基烷基的樹脂)取代含羥基-氰基烷基的樹脂(A)的情形,所得的樹脂膜具有介電常數變低、且在追加燒結後密著性變差的結果(比較例4)。
1‧‧‧薄膜電晶體
2‧‧‧基板
3‧‧‧閘極電極
4‧‧‧閘極絕緣膜
5‧‧‧半導體層
6‧‧‧源極電極
7‧‧‧汲極電極
8‧‧‧保護層
Claims (10)
- 一種樹脂組合物,包括:含有羥基以及氰基烷基的樹脂(A);分子內具有2個以上環氧基的環氧化合物(B);分子內具有2個以上羥基、且羥基值為150~300mgKOH/g的硬化劑(C);以及具有下述一般式(1)所表示結構的交聯劑(D)
- 如申請專利範圍第1項所述之樹脂組合物,其中前述樹脂(A)是將具有複數羥基的含羥基的有機化合物所含的羥基的一部份氰基烷基化而得者。
- 如申請專利範圍第2項所述之樹脂組合物,其中前述含羥基的有機化合物為普魯蘭多醣(Pullulan)或聚乙烯醇。
- 如申請專利範圍第1項所述之樹脂組合物,其中前述環氧化合物(B)為分子內具有2個以上環氧基之含芳香族烴結構的環氧化合物。
- 如申請專利範圍第1項所述之樹脂組合物,其中前述硬化劑(C)具有酚性羥基作為前述羥基。
- 如申請專利範圍第1項所述之樹脂組合物,其中進一步含 有分子內具有酚性的羥基、且羥基值未滿150mgKOH/g的酚類化合物(E)。
- 如申請專利範圍第1項所述之樹脂組合物,其中進一步含有硬化觸媒(F)。
- 如申請專利範圍第1項所述之樹脂組合物,其中前述樹脂(A)所含有的羥基與氰基烷基的比率,以「羥基:氰基烷基」的莫耳比為50:50~2:98。
- 如申請專利範圍第1項所述之樹脂組合物,其中前述交聯劑(D)為下述式(2)~(4)所表示的至少一種化合物,
- 一種閘極絕緣膜,使用如申請專利範圍第1項至第9項任一項所述之樹脂組合物而獲得。
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