TWI553927B - 閘極絕緣材料、閘極絕緣膜、及有機場效型電晶體 - Google Patents
閘極絕緣材料、閘極絕緣膜、及有機場效型電晶體 Download PDFInfo
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- TWI553927B TWI553927B TW098108358A TW98108358A TWI553927B TW I553927 B TWI553927 B TW I553927B TW 098108358 A TW098108358 A TW 098108358A TW 98108358 A TW98108358 A TW 98108358A TW I553927 B TWI553927 B TW I553927B
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- Prior art keywords
- gate insulating
- insulating material
- group
- insulating film
- fet
- Prior art date
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- 239000011810 insulating material Substances 0.000 title claims description 132
- 230000005669 field effect Effects 0.000 title description 5
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- 238000009835 boiling Methods 0.000 claims description 17
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- 239000001257 hydrogen Substances 0.000 claims description 6
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- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 0.000 description 1
- 125000003866 trichloromethyl group Chemical group ClC(Cl)(Cl)* 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Description
本發明關於閘極絕緣材料、閘極絕緣膜及有機場效型電晶體。
近年來,有提案使用成形性優異的有機半導體當作半導體層的有機場效型電晶體(以下稱為有機FET)。利用有機半導體當作印墨,藉由噴墨技術或網版技術等,而使直接在基板上形成電路圖案成為可能,因此代替以往使用無機半導體的場效型電晶體(以下稱為FET),旺盛地檢討使用有機半導體的有機FET。作為顯示FET性能的重要指標,可舉出移動度。移動度的提高,即意味增加開通(on)電流。此提高FET的開關特性,例如與液晶顯示裝置中實現高階調者有關聯。例如,於液晶顯示裝置的情況,要求移動度0.1cm2/V.sec以上。又,另一重要指標係磁滯。磁滯表示對於電壓經歷而言電流值的變動幅度,為了FET的安定驅動,必須減小磁滯值。
作為FET的重要構件,有閘極絕緣膜。通常,半導體層係成膜在由閘極絕緣膜所成的閘極絕緣層上,但是由於在半導體層中的閘極絕緣層界面附近形成電流通道(channel),閘極絕緣膜(尤其表面)的性質係大幅影響FET特性。一般地,作為閘極絕緣膜,有氧化矽等的無機膜,為了形成無機膜,需要CVD等的高價真空裝置,而高成本。又,於無機膜的形成中需要高溫程序,在塑膠等的撓性基板上有製作困難的問題。另一方面,有機聚合物等的有機材料,由於可溶於有機溶劑中,以噴墨印刷等的塗布法係可低成本地形成薄膜,而且可以低溫程序在撓性基板上製作,故進行集中精力的研究。
作為可溶於有機溶劑中的塗布型閘極絕緣材料之例,已知有聚乙烯基苯酚與交聯劑的組合(例如參照非專利文獻1)。然而,由於胺基、酚基等的極性基大量殘留,有FET特性尤其磁滯大的課題。又,若具有如此的極性基,則以光阻等進行圖案加工時,在光阻的塗布、顯像、剝離步驟中,藥液會滲入絕緣膜而引起膨潤,有使絕緣膜劣化的可能性。作為其它閘極絕緣膜之例,有聚矽氧烷(例如參照專利文獻1~3),但是由於聚矽氧烷的撥水性高,於在聚矽氧烷膜上塗布光阻或有機半導體的程序中,發生塗布液的彈開,有難以形成均勻的膜之問題。另一方面,有揭示以導入有環氧基的聚矽氧烷來改善光阻的塗膜性之方法(例如參照專利文獻4),但是關於使用該聚矽氧烷的FET並沒有報告例。
專利文獻1:特開2004-304121號公報(申請專利範圍)
專利文獻2:特開2005-120371號公報(申請專利範圍)
專利文獻3:特開2007-258663號公報(申請專利範圍)
專利文獻4:特開2007-119744號公報(申請專利範圍)
非專利文獻1:“APPLIED PHYSICS LETTERS,vol.82,p.4175-4177(2003年)
本發明之目的為供耐藥品性及光阻、有機半導體塗液的塗布性優異,而且使低磁滯成為可能的閘極絕緣材料、閘極絕緣膜及用其的FET。
本發明係一種閘極絕緣材料,其特徵為含有至少以通式(1)所示的矽烷化合物及通式(2)所示的含環氧基的矽烷化合物當作共聚合成分的聚矽氧烷,R1 mSi(OR2)4-m (1)
此處,R1表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R1以複數存在時,各R1可相同或不同;R2表示烷基或環烷基,於R2以複數存在時,各R2可相同或不同;m表示1~3的整數;R3 nR4 lSi(OR5)4-n-l (2)
此處,R3表示在鏈的一部分具有1個以上的環氧基之烷基或環烷基,於R3以複數存在時,各R3可相同或不同;R4表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R4以複數存在時,各R4可相同或不同;R5表示烷基或環烷基,於R5以複數存在時,各R5可相同或不同;l表示0~2的整數,n表示1或2;但是,l+n≦3。
又,本發明係一種閘極絕緣膜,其係藉由在100℃~300℃的範圍熱處理由塗布前述閘極絕緣材料所形成的塗膜而得。再者,本發明係一種有機場效型電晶體,其具有閘極、閘極絕緣層、半導體層、源極、汲極,其中該閘極絕緣層含有前述閘極絕緣膜。
依照本發明,可提供耐藥品性及光阻、有機半導體塗液的塗布性優異,而且使低磁滯成為可能的閘極絕緣材料、閘極絕緣膜及用其的有機場效型電晶體。
茲詳細說明本發明之以至少以通式(1)所示的矽烷化合物及通式(2)所示的含環氧基的矽烷化合物當作共聚合成分的聚矽氧烷。
首先,說明通式(1)所示的矽烷化合物。R1 msi(OR2)4-m (1)
此處,R1表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R1以複數存在時,各R1可相同或不同;R2表示烷基或環烷基,於R2以複數存在時,各R2可相同或不同;m表示1~3的整數。
烷基例如表示甲基、乙基、正丙基、異丙基、正丁基、第二丁基、第三丁基等的飽和脂肪族烴基,其可具有或不具有取代基。具有取代基時所追加的取代基係沒有特別的限制,例如可舉出烷氧基、芳基、雜芳基等,此等可更具有取代基。又,烷基的碳數係沒有特別的限定,從取得容易性或成本之點來看,較佳為1以上20以下,更佳為1以上8以下。
環烷基例如表示環丙基、環己基、原冰片基、金剛烷基等的飽和脂環式烴基,其可具有或不具有取代基。具有取代基時,取代基係沒有特別的限制,例如可舉出烷基、烷氧基、芳基、雜芳基等、此等取代基可更具有取代基。此等取代基的說明亦與以下的記載共通。環烷基的碳數係沒有特別的限定,較佳為3以上20以下的範圍。
雜環基例如表示吡喃環、哌啶環、醯胺環等之從環內具有碳以外的原子之脂肪族環所導出的基,此等可具有或不具有取代基。雜環基的碳數係沒有特別的限定,更佳為2以上20以下的範圍。
芳基例如表示苯基、萘基、聯苯基、蒽基、菲基、三聯苯基、芘基等的芳香族烴基,其可具有或不具有取代基。芳基的碳數係沒有特別的限定,較佳為6~40的範圍。
雜芳基例如表示呋喃基、噻吩基、苯并呋噻基、二苯并呋噻基、吡啶基、喹啉基等之在環內具有一個或複數個碳以外的原子之芳香族基,其可具有或不具有取代基。雜芳基的碳數係沒有特別的限定,較佳為2~30的範圍。
烯基例如表示乙烯基、烯丙基、丁二烯基等之含雙鍵的不飽和脂肪族烴基,其可具有或不具有取代基。烯基的碳數係沒有特別的限定,較佳為2以上20以下的範圍。
又,作為上述取代基所舉出的烷氧基,例如表示甲氧基、乙氧基、丙氧基等之醚鍵的一方經脂肪族烴基所取代的官能基,該脂肪族烴基可具有或不具有取代基。烷氧基的碳數係沒有特別的限定,較佳為1以上20以下的範圍。
藉由本發明所用的聚矽氧烷中導入通式(1)所示的矽烷化合物,可形成在可見光區域保持高的透明性,同時提高絕緣性、耐藥品性,而且磁滯原因的絕緣膜內之陷阱少的閘極絕緣膜。
又,通式(1)中的m個R1的至少1個若為芳基或雜芳基,由於可提高閘極絕緣膜的柔軟性,防止龜裂發生,故較宜。
作為本發明所用的通式(1)所示的矽烷化合物,具體地可舉出乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、丙基三甲氧基矽烷、丙基三乙氧基矽烷、己基三甲氧基矽烷、十八基三甲氧基矽烷、十八基三乙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、對甲苯基三甲氧基矽烷、苄基三甲氧基矽烷、α-萘基三甲氧基矽烷、β-萘基三甲氧基矽烷、3-胺丙基三乙氧基矽烷、N-(2-胺乙基)-3-胺丙基三甲氧基矽烷、3-氯丙基三甲氧基矽烷、二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、二苯基二甲氧基矽烷、二苯基二乙氧基矽烷、甲基苯基二甲氧基矽烷、甲基乙烯基二甲氧基矽烷、甲基乙烯基二乙氧基矽烷、3-胺丙基甲基二甲氧基矽烷、N-(2-胺乙基)-3-胺丙基甲基二甲氧基矽烷、3-氯丙基甲基二甲氧基矽烷、3-氯丙基甲基二乙氧基矽烷、環己基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基二甲氧基矽烷、十八基甲基二甲氧基矽烷、三甲氧基矽烷、三氟乙基三甲氧基矽烷、三氟乙基三乙氧基矽烷、三氟乙基三異丙氧基矽烷、三氟丙基三甲氧基矽烷、三氟丙基三乙氧基矽烷、三氟丙基三異丙氧基矽烷、十七氟癸基三甲氧基矽烷、十七氟癸基三乙氧基矽烷、十七氟癸基三異丙氧基矽烷、十三氟辛基三乙氧基矽烷、十三氟辛基三甲氧基矽烷、十三氟辛基三異丙氧基矽烷、三氟乙基甲基二甲氧基矽烷、三氟乙基甲基二乙氧基矽烷、三氟乙基甲基二異丙氧基矽烷、三氟丙基甲基二甲氧基矽烷、三氟丙基甲基二乙氧基矽烷、三氟丙基甲基二異丙氧基矽烷、十七氟癸基甲基二甲氧基矽烷、十七氟癸基甲基二乙氧基矽烷、十七氟癸基甲基二異丙氧基矽烷、十三氟辛基甲基二甲氧基矽烷、十三氟辛基甲基二乙氧基矽烷、十三氟辛基甲基二異丙氧基矽烷、三氟乙基乙基二甲氧基矽烷、三氟乙基乙基二乙氧基矽烷、三氟乙基乙基二異丙氧基矽烷、三氟丙基乙基二甲氧基矽烷、三氟丙基乙基二乙氧基矽烷、三氟丙基乙基二異丙氧基矽烷、十七氟癸基乙基二甲氧基矽烷、十七氟癸基乙基二乙氧基矽烷、十七氟癸基乙基二異丙氧基矽烷、十三氟辛基乙基二乙氧基矽烷、十三氟辛基乙基二甲氧基矽烷、十三氟辛基乙基二異丙氧基矽烷、對三氟苯基三乙氧基矽烷等。
於上述矽烷化合物之中,為了提高交聯密度,提高耐藥品性與絕緣特性,較宜使用m=1的乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、丙基三甲氧基矽烷、丙基三乙氧基矽烷、己基三甲氧基矽烷、十八基三甲氧基矽烷、十八基三乙氧基矽烷、苯基三甲氧基矽烷、對甲苯基三甲氧基矽烷、苄基三甲氧基矽烷、α-萘基三甲氧基矽烷、β-萘基三甲氧基矽烷、三氟乙基三甲氧基矽烷、三甲氧基矽烷、對三氟苯基三乙氧基矽烷。又,從量產性的觀點來看,特佳為使用R2係甲基的乙烯基三甲氧基矽烷、甲基三甲氧基矽烷、乙基三甲氧基矽烷、丙基三甲氧基矽烷、己基三甲氧基矽烷、十八基三甲氧基矽烷、十八基三甲氧基矽烷、苯基三甲氧基矽烷、對甲苯基三甲氧基矽烷、苄基三甲氧基矽烷、α-萘基三甲氧基矽烷、β-萘基三甲氧基矽烷、三氟乙基三甲氧基矽烷、三甲氧基矽烷。
又,可舉出組合2種以上的通式(1)所示的矽烷化合物當作較佳例。其中,特佳為組合具有烷基的矽烷化合物與具有芳基或雜芳基的矽烷化合物,因為可使高的絕緣性與用於防止龜裂的柔軟性並存。
接著,說明通式(2)所示之含環氧基的矽烷化合物。R3 nR4 lSi(OR5)4-n-l (2)
此處,R3表示在鏈的一部分具有1個以上的環氧基之烷基或環烷基,於R3以複數存在時,各R3可相同或不同;R4表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R4以複數存在時,各R4可相同或不同;R5表示烷基或環烷基,於R5以複數存在時,各R5可相同或不同;l表示0~2的整數,n表示1或2;但是,l+n≦3。
R3之在鏈的一部分具有環氧基的烷基或環烷基,表示在鏈的一部分具有相鄰的2個碳原子與1個氧原子鍵結而形成的3員環醚構造之烷基或環烷基。
R3~R5的其它說明係與上述R1及R2的說明同樣。
由於本發明所用的聚矽氧烷具有通式(2)所示的含環氧基的矽烷化合物,故在閘極絕緣膜上光阻或有機半導體塗液的塗布性可變良好,且可得到磁滯小的優異FET。
作為本發明所用之通式(2)所示的含環氧基的矽烷化合物,具體地可舉出γ-環氧丙氧基丙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、γ-環氧丙氧基丙基三乙氧基矽烷、β-(3,4-環氧基環己基)乙基三乙氧基矽烷、γ-環氧丙氧基丙基三異丙氧基矽烷、β-(3,4-環氧基環己基)乙基三異丙氧基矽烷、γ-環氧丙氧基丙基甲基二甲氧基矽烷、β-(3,4-環氧基環己基)乙基甲基二甲氧基矽烷、γ-環氧丙氧基丙基甲基二乙氧基矽烷、β-(3,4-環氧基環己基)乙基甲基二乙氧基矽烷、γ-環氧丙氧基丙基甲基二異丙氧基矽烷、β-(3,4-環氧基環己基)乙基甲基二異丙氧基矽烷、γ-環氧丙氧基丙基乙基二甲氧基矽烷、β-(3,4-環氧基環己基)乙基乙基二甲氧基矽烷、γ-環氧丙氧基丙基乙基二乙氧基矽烷、β-(3,4-環氧基環己基)乙基乙基二乙氧基矽烷、γ-環氧丙氧基丙基乙基二異丙氧基矽烷、β-(3,4-環氧基環己基)乙基乙基二異丙氧基矽烷、β-(3,4-環氧基環己基)丙基三甲氧基矽烷、γ-環氧丙氧基乙基三甲氧基矽烷等。
於此等之中,為了提高交聯密度,提高耐藥品性與絕緣特性,較宜使用n=1、l=0的γ-環氧丙氧基丙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、γ-環氧丙氧基丙基三乙氧基矽烷、β-(3,4-環氧基環己基)乙基三乙氧基矽烷、γ-環氧丙氧基丙基三異丙氧基矽烷、β-(3,4-環氧基環己基)乙基三異丙氧基矽烷、β-(3,4-環氧基環己基)丙基三甲氧基矽烷、γ-環氧丙氧基乙基三甲氧基矽烷。又,從量產性的觀點來看,特佳為使用R5係甲基的γ-環氧丙氧基丙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷、β-(3,4-環氧基環己基)丙基三甲氧基矽烷、γ-環氧丙氧基乙基三甲氧基矽烷。
本發明所用的聚矽氧烷,除了含有通式(1)或(2)所示的矽烷化合物,亦可含有其它矽烷化合物當作共聚合成分。作為其它矽烷化合物,可舉出四甲氧基矽烷、四乙氧基矽烷等。
又,於聚矽氧烷之中,從通式(2)所示的含環氧基的矽烷化合物而來的構成單位之含量,相對於聚矽氧烷的共聚合成分之矽烷化合物的全部構成單位而言,較佳為0.1莫耳%~40莫耳%。若為0.1莫耳%以上,則可得到抑制有機半導體塗液的彈開之良好塗布性,更佳為1莫耳%以上。另一方面,若為40莫耳%以下,可得到磁滯小的優異FET特性,更佳為35莫耳%以下。
本發明所用的聚矽氧烷,例如可藉由以下的方法來獲得。於溶劑中溶解全部矽烷化合物,於其中費1~180分鐘添加酸觸媒及水後,於室溫~80℃使水解反應1~180分鐘。水解反應時的溫度更佳為室溫~55℃。在50℃以上、溶劑的沸點以下將此反應液加熱1~100小時,進行縮合反應,可得到含環氧基的聚矽氧烷。於此情況下,為了對通式(2)所示的含環氧基的矽烷化合物的環氧基附加水而形成二醇,除了與全部矽烷化合物中的烷氧基成當量的水,亦必須添加與環氧基成當量以上的水。
又,水解的各種條件,係考慮反應規模、反應容器的大小、形狀等,例如藉由設定酸濃度、反應溫度、反應時間等,可得到適合於目的用途的物性。
作為矽烷化合物之水解反應所利用的酸觸媒,可舉出甲酸、草酸、鹽酸、硫酸、乙酸、三氟乙酸、磷酸、多磷酸、多元羧酸或其酐、離子交換樹脂等的酸觸媒。酸觸媒的含量,相對於聚矽氧烷的共聚合成分之全部矽烷化合物100重量份而言,較佳為0.05重量份以上,更佳為0.1重量份以上。又,較佳為10重量份以下,更佳為5重量份以下。酸觸媒的含量若為0.05重量份以上,則水解反應可充分進行,而若為10重量份以下,可抑制劇烈的反應。
作為水解反應所用的溶劑,較佳為有機溶劑,可舉出乙醇、丙醇、丁醇、3-甲基-3-甲氧基-1-丁醇等的醇類、乙二醇、丙二醇等的二醇類、乙二醇單甲基醚、丙二醇單甲基醚、丙二醇單丁基醚、二乙基醚等的醚類、甲基異丁基酮、二異丁基酮等的酮類、二甲基甲醯胺、二甲基乙醯胺等的醯胺類、醋酸乙酯、乙基溶纖劑醋酸酯、3-甲基-3-甲氧基-1-丁醇醋酸酯等的醋酸酯類、甲苯、二甲苯、己烷、環己烷等的芳香族或脂肪族烴,以及γ-丁內酯、N-甲基-2-吡咯啶酮、二甲亞碸等。溶劑的量,相對於聚矽氧烷的共聚合成分之全部矽烷化合物100重量份而言,較佳為50重量份~500重量份的範圍。若為50重量份以上,可抑制劇烈的反應,而若為500重量份以下,則水解反應可充分進行。
又,作為水解所用的水,較佳為離子交換水。水量係可任意選擇,除了與矽烷化合物中的烷氧基成當量莫耳的水,亦可添加與環氧基成當量莫耳以上的水,為了提高聚矽氧烷的聚合度,亦可進行再加熱或鹼觸媒的添加。
本發明所用之含有含環氧基的矽烷化合物當作共聚合成分的聚矽氧烷,由於絕緣性、耐藥品性高,且磁滯原因的絕緣膜內之陷阱少,故適用作為閘極絕緣材料。聚矽氧烷含有含環氧基的矽烷化合物者,係可藉由單獨或複數地組合元素分析、核磁共振分析、紅外分光分析等的各種有機分析手法來判定。
本發明的閘極絕緣材料亦可含有1種或2種以上的聚矽氧烷。又,可混合使用1種以上的聚矽氧烷與1種以上的前述矽烷化合物。
本發明的閘極絕緣材料較佳為更含有1大氣壓的沸點為110~200℃的溶劑。作為如此的溶劑,具體地可舉出乙二醇單甲基醚、乙二醇單乙基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單正丁基醚、丙二醇單第三丁基醚、乙二醇二甲基醚、乙二醇二乙基醚、乙二醇二丁基醚、二乙二醇乙基甲基醚等的醚類、乙二醇單乙基醚醋酸酯、丙二醇單甲基醚醋酸酯、丙基醋酸酯、丁基醋酸酯、異丁基醋酸酯、3-甲氧基丁基醋酸酯、3-甲基-3-甲氧基丁基醋酸酯、乳酸甲酯、乳酸乙酯、乳酸丁酯等的醋酸酯類、乙醯基丙酮、甲基丙基酮、甲基丁基酮、甲基異丁基酮、環戊酮、2-庚酮等的酮類、丁基醇、異丁基醇、戊醇、4-甲基-2-戊醇、3-甲基-2-丁醇、3-甲基-3-甲氧基丁醇、二丙酮醇等的醇類、甲苯、二甲苯等的芳香族烴類。若沸點為110℃以上,則在閘極絕緣材料塗布時,可抑制溶劑的揮發,塗布性良好,而若為200℃以下,則可得到膜中所殘留的溶劑少,耐藥品性或絕緣性優異的閘極絕緣膜。更佳的沸點為130℃~190℃。此等溶劑可單獨或以2種以上來使用。
此等溶劑的較佳含量,相對於100重量份的聚矽氧烷而言係100重量份~1500重量份。若為100重量份以上,則在閘極絕緣材料塗布時,可抑制溶劑的揮發而塗布性良好,而若為1500重量份以下,則可得到膜中所殘留的溶劑少,藥品性或絕緣性優異的閘極絕緣膜。
於使用2種以上的溶劑時,亦可以含有1種以上的大氣壓下沸點低於110℃的低沸點溶劑或大氣壓下沸點超過200℃的高沸點溶劑。
本發明的閘極絕緣材料更佳為含有粒子。從閘極絕緣膜的平坦性之觀點來看,粒子的粒徑較佳為100nm以下,更佳為50nm以下。又,從與聚矽氧烷的相溶性之觀點來看,較佳為溶膠狀態。更佳地,為了減小FET的閘值電壓(Vt),比介電常數為3以上的粒子係較宜。作為粒子的具體例,可舉出矽石粒子、二氧化鈦粒子、鈦酸鋇粒子、氧化鋯粒子、硫酸鋇粒子等。
本發明的閘極絕緣材料更佳為含有硬化劑。作為硬化劑,較佳為金屬烷氧化物化合物或金屬螯合化合物,亦可併用此等。
作為金屬烷氧化物化合物的較佳具體例,可舉出二乙氧化鎂、三異丙氧化鋁、氧化鋯四(正丁氧化物)、氧化鋯四(第三丁氧化物)、四異丙氧化鉿、四異丙氧化鈦等。
金屬螯合物係可藉由使金屬烷氧化物與螯合化劑反應而容易獲得。作為螯合化劑之例,可使用乙醯基丙酮、苯甲醯基丙酮、二苯甲醯基甲烷等的β-二酮、乙醯基醋酸乙酯、苯甲醯基醋酸乙酯等的β-酮酸酯等。
作為金屬螯合化合物的較佳具體例,可舉出乙基乙醯基醋酸酯鋁二異丙氧化物、鋁三(乙基乙醯基醋酸酯)、烷基乙醯基醋酸酯二異丙氧化鋁、鋁單乙醯基醋酸酯雙(乙基乙醯基醋酸酯)、鋁三(乙醯基丙酮化物)等的鋁螯合化合物、乙基乙醯基醋酸酯鎂單異丙氧化物、鎂雙(乙基乙醯基醋酸酯)、烷基乙醯基醋酸酯鎂單異丙氧化物、鎂雙(乙醯基丙酮化物)等的鎂螯合化合物、氧化鋯四(乙基乙醯基醋酸酯)、氧化鋯四(乙醯基丙酮化物)等的氧化鋯螯合化合物、鈦四(乙基乙醯基醋酸酯)、鈦四(乙醯基丙酮化物)等的鈦螯合化合物。於此等硬化劑之中,較佳為四異丙氧化鈦、鋁三(乙醯基丙酮化物)、鋁三(乙基乙醯基醋酸酯)、鎂雙(乙醯基丙酮化物)、鎂雙(乙基乙醯基醋酸酯)、氧化鋯四(乙基乙醯基醋酸酯)、氧化鋯四(乙醯基丙酮化物)、鈦四(乙基乙醯基醋酸酯)、鈦四(乙醯基丙酮化物),若考慮保存安定性、取得容易性,特佳為四異丙氧化鈦、鋁三(乙醯基丙酮化物)、鋁三(乙基乙醯基醋酸酯)、氧化鋯四(乙基乙醯基醋酸酯)、氧化鋯四(乙醯基丙酮化物)、鈦四(乙基乙醯基醋酸酯)、鈦四(乙醯基丙酮化物)
相對於100重量份的聚矽氧烷而言,硬化劑的含量較佳為0.1重量份~10重量份,更佳為1重量份~6重量份。含量若為0.1重量份以上,則硬化充分進行,可得到具有良好的耐藥品性或絕緣性的閘極絕緣膜。另一方面,若為10重量份以下,則閘極絕緣材料的保存安定性良好。
本發明的閘極絕緣材料亦可更含有藉由光而產生酸的化合物,於此情況下,具有負型的感光性。作為藉由光而產生酸的化合物(光酸產生劑),可舉出鎓鹽化合物、含鹵素的化合物、重氮酮化合物、重氮甲烷化合物、碸化合物、磺酸酯化合物、磺醯亞胺化合物等當作例子。
作為鎓鹽化合物的具體例,可舉出重氮鎓鹽、銨鹽、碘鎓鹽、鋶鹽、鏻鹽、氧鎓鹽等。作為較佳的鎓鹽,可舉出二苯基碘鎓三氟甲磺酸鹽、二苯基碘鎓芘磺酸鹽、二苯基碘鎓十二基苯磺酸鹽、三苯基鋶三氟甲磺酸鹽(商品名「TPS-105」綠化學(股)製)、4-第三丁基苯基二苯基鋶三氟甲磺酸鹽(商品名「WPAG-339」和光純藥工業(股)製)、4-甲氧基苯基二苯基鋶三氟甲磺酸鹽(商品名「WPAG-370」和光純藥工業(股)製)、三苯基鋶九氟甲磺酸鹽(商品名「TPS-109」綠化學(股)製)、三苯基鋶六氟銻酸鹽、三苯基鋶萘磺酸鹽、(羥苯基)苄基甲基鋶甲苯磺酸鹽等。
作為含鹵素的化合物之具體例,可舉出含鹵烷基的烴化合物、含鹵烷基的雜環狀化合物等。較佳為較佳之含鹵素的化合物,可舉出1,1-雙(4-氯苯基)-2,2,2-三氯乙烷、2-苯基-4,6-雙(三氯甲基)-S-三、2-萘基-4,6-雙(三氯甲基)-S-三等。
作為重氮酮化合物的具體例,可舉出1,3-二酮基-2-重氮化合物、重氮苯醌化合物、重氮萘醌化合物等。較佳的重氮酮化合物例如可為1,2-萘醌二疊氮基-4-磺酸與2,2,3,4,4’-四羥基二苯甲酮的酯、1,2-萘醌二疊氮基-4-磺酸與1,1,1-三(4-羥苯基)乙烷的酯等。
作為重氮甲烷化合物的具體例,可舉出雙(三氟甲基磺醯基)重氮甲烷、雙(環己基磺醯基)重氮甲烷、雙(苯基磺醯基)重氮甲烷、雙(對甲苯基磺醯基)重氮甲烷、雙(2,4-二甲苯基磺醯基)重氮甲烷、雙(對氯苯基磺醯基)重氮甲烷、甲基磺醯基對甲苯磺醯基重氮甲烷、環己基磺醯基(1,1-二甲基乙基磺醯基)重氮甲烷、雙(1,1-二甲基乙基磺醯基)重氮甲烷、苯基磺醯基(苯甲醯基)重氮甲烷等。
作為碸化合物的具體例,可舉出β-酮基碸化合物、β-磺醯基碸化合物等。作為較佳的化合物,可舉出4-三苯甲醯甲基碸、基苯甲醯甲基碸、雙(苯基磺醯基)甲烷等。
作為磺酸酯化合物之例,可舉出磺酸烷基酯、磺酸鹵烷基酯、磺酸芳基酯、磺酸亞胺基酯等。作為具體例,可舉出苯偶姻甲苯磺酸酯、焦棓酚三甲磺酸酯、硝基苄基-9,10-二乙氧基蒽-2-磺酸酯等。
作為磺醯亞胺化合物的具體例,可舉出N-(三氟甲基磺醯氧基)琥珀醯亞胺、N-(三氟甲基磺醯氧基)酞醯亞胺、N-(三氟甲基磺醯氧基)二苯基馬來醯亞胺、N-(三氟甲基磺醯氧基)雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(三氟甲基磺醯氧基)-7-氧雜雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(三氟甲基磺醯氧基)雙環[2.2.1]庚烷-5,6-氧基-2,3-二羧醯亞胺、N-(三氟甲基磺醯氧基)萘基二羧醯亞胺、N-(樟腦磺醯氧基)琥珀醯亞胺、N-(樟腦磺醯氧基)酞醯亞胺、N-(樟腦磺醯氧基)二苯基馬來醯亞胺、N-(樟腦磺醯氧基)雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(樟腦磺醯氧基)-7-氧雜雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(樟腦磺醯氧基)雙環[2.2.1]庚烷-5,6-氧基-2,3-二羧醯亞胺、N-(樟腦磺醯氧基)萘基二羧醯亞胺、N-(4-甲基苯基磺醯氧基)琥珀醯亞胺、N-(4-甲基苯基磺醯氧基)酞醯亞胺、N-(4-甲基苯基磺醯氧基)二苯基馬來醯亞胺、N-(4-甲基苯基磺醯氧基)雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(4-甲基苯基磺醯氧基)-7-氧雜雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(4-甲基苯基磺醯氧基)雙環[2.2.1]庚烷-5,6-氧基-2,3-二羧醯亞胺、N-(4-甲基苯基磺醯氧基)萘基二羧醯亞胺、N-(2-三氟甲基苯基磺醯氧基)琥珀醯亞胺、N-(2-三氟甲基苯基磺醯氧基)酞醯亞胺、N-(2-三氟甲基苯基磺醯氧基)二苯基馬來醯亞胺、N-(2-三氟甲基苯基磺醯氧基)雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(2-三氟甲基苯基磺醯氧基)-7-氧雜雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(2-三氟甲基苯基磺醯氧基)雙環[2.2.1]庚烷-5,6-氧基-2,3-二羧醯亞胺、N-(2-三氟甲基苯基磺醯氧基)萘基二羧醯亞胺、N-(4-氟苯基磺醯氧基)琥珀醯亞胺、N-(2-氟苯基磺醯氧基)酞醯亞胺、N-(4-氟苯基磺醯氧基)二苯基馬來醯亞胺、N-(4-氟苯基磺醯氧基)雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(4-氟苯基磺醯氧基)-7-氧雜雙環[2.2.1]庚-5-烯-2,3-二羧醯亞胺、N-(4-氟苯基磺醯氧基)雙環[2.2.1]庚烷-5,6-氧基-2,3-二羧醯亞胺、N-(4-氟苯基磺醯氧基)萘基二羧醯亞胺等。
於上述以外,亦可舉出5-原冰片烯-2,3-二羧基亞胺基三氟甲磺酸鹽(商品名「NDI-105」綠化學(股)製)、5-原冰片烯-2,3-二羧基亞胺基甲苯磺酸酯(商品名「NDI-101」綠化學(股)製)、4-甲基苯基磺醯氧基亞胺基-α-(4-甲氧基苯基)乙腈(商品名「PAI-101」綠化學(股)製)、三氟甲基磺醯氧基亞胺基-α-(4-甲氧基苯基)乙腈(商品名「PAI-105」綠化學(股)製)、9-樟腦磺醯氧基亞胺基α-4-甲氧基苯基乙腈(商品名「PAI-106」綠化學(股)製)、1,8-萘二甲醯亞胺基丁烷磺酸酯(商品名「NAI-1004」綠化學(股)製)、1,8-萘二甲醯亞胺基甲苯磺酸酯(商品名「NAI-101」綠化學(股)製)、1,8-萘二甲醯亞胺基三氟甲磺酸鹽(商品名「NAI-105」綠化學(股)製)、1,8-萘二甲醯亞胺基九氟丁烷磺酸酯(商品名「NAI-109」綠化學(股)製)等。於此等之中,特佳為TPS-105、WPAG-339、WPAG-370、TPS-109、二苯基碘鎓芘磺酸鹽、NDI-105、PAI-101、NAI-105。
可以使用單獨或2種以上的光酸產生劑。相對於100重量份的聚矽氧烷而言,光酸產生劑的含量較佳為1~10重量份,更佳為1~7重量份。光酸產生劑的含量若為1重量份以上,則可容易地進行圖案形成,而若為10重量份以下,則與顯像液親和性良好,顯像性變良好。
再者,光酸產生劑較佳為與作為增感劑的9,10-二取代蒽系化合物組合使用。該增感劑由於不會因光褪色反應而發生著色,故即使殘留在閘極絕緣膜中,也可維持高的透明性,同時達成高感度化。
作為9,10-二取代蒽系化合物,可舉出9,10-二苯基蒽、9,10-雙(4-甲氧基苯基)蒽、9,10-雙(三苯基矽烷基)蒽、9,10-二甲氧基蒽、9,10-二乙氧基蒽、9,10-二丙氧基蒽、9,10-二丁氧基蒽、9,10-二戊氧基蒽、2-第三丁基-9,10-二丁氧基蒽、9,10-雙(三甲基矽烷基乙炔基)蒽等。於此等之中,特佳的化合物為9,10-二甲氧基蒽、9,10-二乙氧基蒽、9,10-二丙氧基蒽、9,10-二丁氧基蒽。
亦可使用單獨或2種以上的此等增感劑。相對於100重量份的聚矽氧烷而言,增感劑的含量較佳為0.05~5重量份,更佳為0.1~3重量份。增感劑的含量若為0.05重量份以上,則可容易地進行圖案的形成,若為5重量份以下,則與顯像液親和性良好,顯像性變良好。
又,作為增感劑,不限定於上述9,10-二取代蒽系化合物,可使用眾所周知的材料。
於本發明的閘極絕緣材料中,通式(1)及(2)所示的矽烷化合物或其它矽烷化合物的水解物即矽烷醇係存在。矽烷醇係藉由酸或鹼的作用進行縮合而成為矽氧烷,但閘極絕緣材料若在保管中進行縮合則黏度上升,成為塗膜的膜厚變化之要因。用作為閘極絕緣膜時,由於膜厚變化係因為在閘極電壓印加時即以離子狀態蓄積的絕緣膜中之電荷容量變化,故成為FET特性變動的要因。因此,將閘極絕緣材料的pH控制在矽烷醇的縮合速度慢的條件之2~7,較佳在3~6,以抑制黏度的上升。pH係可藉由使閘極絕緣材料與同重量的水接觸攪拌,測定該水溶液相的pH而調查。作為pH控制方法,較宜使用將閘極絕緣材料水洗的方法、以離子交換樹脂去除過剩的酸或鹼之方法等。
又,本發明的閘極絕緣材料視需要可含有黏度調整劑、界面活性劑、安定化劑等。
作為界面活性劑,例如可舉出氟系界面活性劑、聚矽氧系界面活性劑、聚環氧烷系界面活性劑、丙烯酸系界面活性劑等。
作為氟系界面活性劑的具體例,可舉出1,1,2,2-四氟辛基(1,1,2,2-四氟丙基)醚、1,1,2,2-四氟辛基己基醚、八乙二醇二(1,1,2,2-四氟丁基)醚、六乙二醇(1,1,2,2,3,3-六氟戊基)醚、八丙二醇二(1,1,2,2-四氟丁基)醚、六丙二醇二(1,1,2,2,3,3-六氟戊基)醚、全氟十二基磺酸鈉、1,1,2,2,8,8,9,9,10,10-十氟十二烷、1,1,2,2,3,3-六氟癸烷、N-[3-(全氟辛烷磺醯胺)丙基]-N,N’-二甲基-N-羧基亞甲基銨甜菜鹼、全氟烷基磺醯胺丙基三甲基銨鹽、全氟烷基-N-乙基磺醯基甘胺酸鹽、磷酸雙(N-全氟辛基磺醯基-N-乙基胺乙基)、單全氟烷基乙基磷酸酯等。又,作為市售品,可舉出Megafac F142D、同F172、同F173、同F183(以上、大日本油墨化學工業(股)製)、Eftop EF301、同303、同352(新秋田化成(股)製)、Fluorad FC-430、同FC-431(住友3M(股)製))、Asahiguard AG710、Surflon S-382、同SC-101、同SC-102、同SC-103、同SC-104、同SC-105、同SC-106(旭硝子(股)製)、BM-1000、BM-1100(裕商(股)製)、NBX-15、FTX-218(NEOS(股)製)等。
作為聚矽氧系界面活性劑,可舉出SH28PA、SH7PA、SH21PA、SH30PA、ST94PA(皆為東麗.道康寧.聚矽氧(股)製)、BYK-333(BYK化學.日本(股)製)等。作為其它界面活性劑之例,可舉出聚氧化乙烯月桂基醚、聚氧化乙烯硬脂基醚、聚氧化乙烯壬基苯基醚、聚氧化乙烯二硬脂酸酯等。
相對於100重量份的聚矽氧烷而言,界面活性劑的含量較佳為0.0001~1重量份。亦可同時使用2種以上的界面活性劑。
接著,詳細說明本發明的閘極絕緣膜。本發明的閘極絕緣膜係可藉由塗布本發明的閘極絕緣材料,將所形成的塗膜在100~300℃的範圍進行熱處理而得。
作為上述閘極絕緣材料的塗布方法,可舉出旋塗法、刮塗法、縫模塗布法、網版印刷法、桿塗法、鑄模法、印刷轉印法、浸漬吊起法、噴墨法等眾所周知的方法。藉由前述塗布方法將閘極絕緣材料塗布在玻璃基板或塑膠基板上及使乾燥,對所得之塗膜進行熱處理,可形成閘極絕緣膜。又,於含有光酸產生劑的閘極絕緣材料之情況,對塗膜進行曝光、顯像後,藉由熱處理,可形成閘極絕緣膜。乾燥溫度較佳為50~150℃。
閘極絕緣膜的膜厚較佳為0.01~5μm,更佳為0.05~1μm。熱處理的溫度較佳為在100~300℃的範圍。從在塑膠基板上形成閘極絕緣膜的觀點來看,更佳為120~200℃。
此處,說明使用含有光酸產生劑的閘極絕緣材料之塗膜的圖案形成。從塗膜的上方通過具有所欲圖案的光罩照射(曝光)化學線。作為曝光所用的化學線,有紫外線、可見光線、電子線、X射線等,但於本發明中較佳為利用水銀燈的i線(365nm)、h線(405nm)、g線(436nm)。接著,將經曝光的塗膜顯像。作為顯像液,較佳為四甲銨、二乙醇胺、二乙基胺基乙醇、氫氧化鈉、氫氧化鉀、碳酸鈉、碳酸鉀、三乙胺、二乙胺、甲胺、二甲胺、醋酸二甲基胺乙酯、二甲基胺基乙醇、甲基丙烯酸二甲胺基乙酯、環己胺、乙二胺、六亞甲基二胺等之顯示鹼性的化合物之水溶液,可含有1種或2種以上。又,於此等鹼水溶液中,亦可以混合使用N-甲基-2-吡咯啶酮、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、二甲亞碸、γ-丁內酯、二甲基丙烯醯胺等的極性溶劑、甲醇、乙醇、異丙醇等的醇類、乳酸乙酯、丙二醇單甲基醚醋酸酯等的酯類、環戊酮、環己酮、異丁基酮、甲基異丁基酮等的酮類等。顯像後通常以水進行沖洗處理,亦可將乙醇、異丙醇等的醇類、乳酸乙酯、丙二醇單甲基醚醋酸酯等的酯類等加到水中而進行沖洗處理。
又,本發明的閘極絕緣膜之比介電常數較佳為3~50。比介電常數愈大則愈可減小FET的閘值電壓。
而且,本發明的閘極絕緣膜較佳為鹼金屬或鹼土類金屬、鹵素離子的濃度少。具體地,重金屬、鹵素離子較佳皆為閘極絕緣材料的100ppm以下,更佳皆為1ppm以下,特佳皆為0.1ppm以下。
接著,說明使用本發明的閘極絕緣膜之FET。本發明的FET係具有閘極、閘極絕緣層、半導體層、源極及汲極的有機場效型電晶體,前述閘極絕緣層含有本發明的閘極絕緣膜。
第1圖及第2圖係顯示本發明的FET之例的模型剖面圖。於第1圖中,在具有以含有本發明的閘極絕緣膜之閘極絕緣層3所覆蓋的閘極2之基板1上,形成源極5及汲極6後,再於其上形成半導體層4。於第2圖中,在具有以含有本發明的閘極絕緣膜之閘極絕緣層3所覆蓋的閘極2之基板1上,形成含有本發明的有機電晶體材料之半導體層4後,再於其上形成源極5及汲極6。
作為基板1所用的材料,例如可舉出矽晶圓、玻璃、氧化鋁燒結體等的無機材料、聚醯亞胺、聚酯、聚碳酸酯、聚碸、聚醚碸、聚乙烯、聚苯硫醚、聚對二甲苯等的有機材料。
作為閘極2、源極5及汲極6所用的材料,例如可舉出、氧化錫、氧化銦、氧化錫銦(ITO)等的導電性金屬氧化物,或鉑、金、銀、銅、鐵、錫、鋅、鋁、銦、鉻、鋰、鈉、鉀、銫、鈣、鎂、鈀、鉬、非晶形矽或多晶矽等的金屬或此等的合金、碘化銅、硫化銅等的無機導電性物質、聚噻吩、聚吡咯、聚苯胺、聚伸乙二氧基噻吩與聚苯乙烯磺酸的錯合物等,以碘等的摻雜等而提高導電率的導電性聚合物等,惟不受此等所限定。此等電極材料可單獨使用,也可層合或混合複數的材料來使用。
於本發明的FET中,閘極絕緣層3含有本發明的閘極絕緣膜。閘極絕緣層3係可由單層或複數層所構成。於複數層的情況中,可層合本發明的複數閘極絕緣膜,也可層合本發明的閘極絕緣膜與眾所周知的閘極絕緣膜。作為已知的閘極絕緣膜,並沒有特別的限定,可使用氧化矽、氧化鋁等的無機材料、聚醯亞胺、聚乙烯醇、聚氯乙烯、聚對苯二甲酸乙二酯、聚偏二氟乙烯、聚矽氧烷、聚乙烯基苯酚(PVP)等的有機高分子材料,或無機材料粉末與有機高分子材料的混合物。
閘極絕緣層3的膜厚較佳為0.01μm以上5μm以下。藉由成為此範圍的膜厚,可容易形成均勻的薄膜,而且可抑制閘極電壓所無法控制的源極.汲極間電流,可更提高FET的開關比。膜厚係可藉由原子間力顯微鏡或橢圓偏振測量法等來測定。
半導體層4所用的有機半導體,只要是顯示半導體性的材料,可不受分子量拘束而使用,較佳可使用載子移動度高的材料。又,更佳為可溶於有機溶劑中者,藉由在玻璃基板或塑膠基板上塗布溶液,可簡便地形成半導體層。有機半導體的種類係沒有特別的限定,可舉出聚-3-己基噻吩、聚苯并噻吩等的聚噻吩類、聚(2,5-雙(2-噻吩基)-3,6-雙十五基噻吩并[3,2-b]噻吩)、聚(4,8-二己基-2,6-雙(3-己基噻吩-2-基)苯并[1,2-b:4,5-b’]二噻吩)、聚(4-辛基-2-(3-辛基噻吩-2-基)噻唑)、聚(5,5’-雙(4-辛基噻唑-2-基)-2,2’-聯二噻吩)等在主鏈中含有噻吩單元的化合物、聚吡咯類、聚(對伸苯基伸乙烯基)等的聚(對伸苯基伸乙烯基)類、聚苯胺類、聚乙炔類、聚二乙炔類、聚咔唑類、聚呋喃、聚苯并呋喃等的聚呋喃類、吡啶、喹啉、菲繞啉、唑、二唑等之以含氮芳香環當作構成單位的聚雜芳基類、蒽、芘、丁省、戊省、己省、紅螢烯等的縮合多環芳香族化合物、呋喃、噻吩、苯并噻吩、二苯并呋喃、吡啶、喹啉、菲繞啉、唑、二唑等的含氮芳香族化合物、4,4’-雙(N-(3-甲基苯基)-N-苯基胺基)聯苯所代表的芳香族胺衍生物、雙(N-烯丙基咔唑)或雙(N-烷基咔唑)等的雙咔唑衍生物、吡唑啉衍生物、茋系化合物、腙系化合物、銅酞花青等的金屬酞花青類、銅卟啉等的金屬卟啉類、二苯乙烯基苯衍生物、胺基苯乙烯基衍生物、芳香族乙炔衍生物、萘-1,4,5,8-四羧酸二醯亞胺、苝-3,4,9,10-四羧酸二醯亞胺等的縮合環四羧酸二醯亞胺類、部花青、啡、若丹明等的有機色素等當作例子。亦可以含有2種以上的此等。其中,較佳為具有噻吩骨架的有機半導體。
又,作為半導體層4的另一較佳形態,可舉出使用有機半導體與碳奈米管(CNT)的複合物之方法。添加CNT者係較宜用作為提高有機半導體的移動度之手段。
有機半導體與CNT的複合物中所含有的CNT之重量分率,為了得到半導體特性,相對於有機半導體而言,較佳為0.01~3重量%。若比0.01重量%還小,則添加的效果小,而比3重量%大的重量分率係不適合作為半導體層用,因為複合物的導電率過剩地增加。更佳為2重量%以下。藉由成為2重量%以下,可容易得到高移動度與高開關比的並存。
於FET中使用有機半導體與CNT的複合物時,較佳為CNT的長度小且比源極與汲極間的距離(通道長)還短。若比其還長,則成為使電極間短路的原因。因此,較佳為使用長度至少比源極與汲極間的距離(通道長)還短的CNT,或是經過將CNT縮成比通道長還短的步驟。一般市售的CNT係有長度分布,含有比通道長還長的CNT。因此,最好為施加有將CNT縮成比通道長還短的步驟,可確實防止電極間的短路。CNT的平均長度係取決於電極間距離,較佳使用5μm以下,更佳為使用1μm以下。
又,CNT的直徑係沒有特別的限定,係1nm以上100nm以下,更佳為50nm以下。
於本發明中,較佳為使用表面的至少一部分附著有共軛系聚合物的CNT。藉此,可使CNT更均勻分散在基質(有機半導體)中,可實現高的移動度以及高的開關比。CNT的表面之至少一部分附著有共軛系聚合物的狀態,係意味CNT的表面之一部分或全部經共軛系聚合物所被覆的狀態。茲推測共軛系聚合物可被覆CNT係因為從各自的共軛系構造而來的π電子雲重疊而產生相互作用。CNT是否被共軛系聚合物所被覆,可以從經被覆的CNT之反射色與未經被覆的CNT之色接近共軛系聚合物的色來判斷。定量地藉由X射線光電子分光(XPS)等的元素分析,可鑑定附著物的存在及附著物對CNT的重量比。
使CNT附著共軛系聚合物的方法,可舉出(I)於熔融的共軛系聚合物中添加CNT及混合的方法,(II)使共軛系聚合物溶解於溶劑中,於其中添加CNT及混合的方法,(III)預先藉由超音波等將CNT預備分散,對其添加共軛系聚合物及混合的方法,(IV)於溶劑中加入共軛系聚合物與CNT,對此混合系照射超音波及混合的方法等。於本發明中,可使用任一種方法,也可組合任一種方法。
上述被覆CNT的共軛聚合物,例如是聚噻吩系聚合物、聚吡咯系聚合物、聚苯胺系聚合物、聚乙炔系聚合物、聚對伸苯基系聚合物、聚對伸苯基伸乙烯基系聚合物等,並沒有特別的限定。上述聚合物較宜使用單一的單體單元所排列者,也可使用不同的單體單元經嵌段共聚合者、無規共聚合者。又,亦可使用接枝聚合者。於上述聚合物中,本發明特佳為使用對CNT的附著容易,容易形成CNT複合體的聚噻吩系聚合物。
半導體層4的形成步驟亦可使用電阻加熱蒸鍍、電子線束、濺鍍、CVD等乾式的方法,但從製造成本或適合大面積的觀點來看,以及在含有本發明的閘極絕緣膜之閘極絕緣層3中,為了發揮抑制塗液的彈開之優點,較宜使用塗布法。具體地,可較佳地使用旋塗法、刮塗法、縫模塗布法、網版印刷法、桿塗法、鑄模法、印刷轉印法、浸漬吊起法、噴墨法等,可按照塗膜厚度控制或配向控制等所要得到的塗膜特性來選擇塗布方法。又,為了減低對塑膠基板的影響,溶液塗布後的加熱處理較佳為220℃以下。所形成的FET係可藉由改變閘極電壓來控制源極與汲極之間所流動的電流。FET的移動度係可使用下述的(a)式來算出。
μ=(δId/δVg)L.D/(W.εr.ε.Vsd) (a)
但是,Id(A)係源極.汲極間的電流,Vsd(V)係源極.汲極間的電壓,Vg(V)係閘極電壓,D(m)係絕緣層的厚度,L(m)係通道長,W(m)係通道寬,εr係閘極絕緣層的比介電常數,ε係真空的介電常數(8.85×10-12F/m)。
又,可由某一員的閘極電壓之Id(開通電流)值與某一負的閘極電壓之Id(關閉電流)值的比來求得開關比。
磁滯係可由從正到負施加Vg時的Id=10-8A之閘極電壓Vg1與從負到正施加Vg時的Id=10-8A之閘極電壓Vg2的差之絕對值|Vg1-Vg2|來求得。
本發明的閘極絕緣材料及閘極絕緣膜係可有利地用於薄膜的場效型電晶體、光電動勢元件、開關元件等各種裝置的製造。
以下舉出實施例來說明本發明,惟本發明不受此等實施例所限定。再者,以下(1)~(8)說明實施例中的各評價法。
於6吋矽晶圖上及6吋玻璃基板上,以乾燥後的膜厚成為0.5μm的方式,使用旋塗機來塗布閘極絕緣材料,接著使用熱板(大日本屏幕製造(股)製SCW-636),在120℃乾燥3分鐘,而得到塗膜。
關於在閘極絕緣材料之中不具有感光性的材料,藉由以下方法來製作閘極絕緣膜。將上述(1)所製作的6吋矽晶圓上及6吋玻璃基板上之塗膜,在指定的溫度、時間進行加熱處理而得到閘極絕緣膜。
關於在閘極絕緣材料之中具有感光性的材料,藉由以下方法來製作閘極絕緣膜。將以上述(1)記載之方法所製作的在6吋矽晶圓上及6吋玻璃基板上所形成的塗膜,固定在i線步進曝光機(GCA製DSW-8000),以800mJ/cm2的曝光量將塗膜全面曝光。曝光後,藉由90℃的熱板進行1分鐘的PEB,以2.38重量%的TMAH水溶液(三菱瓦斯化學(股)製,ELM-D)來顯像60秒,接著以純水沖洗。藉由在指定的溫度、時間對此膜進行加熱處理,而得到閘極絕緣膜。
使用Lambdace STM-602(大日本屏幕製造(股)製),在1.55的折射率進行膜厚的測定。
將以上述(2)記載的方法所製作的6吋矽晶圓上之閘極絕緣膜,在溫度經控制25℃的二甲亞碸/乙醇混合溶液(重量比70/30)中浸漬30分鐘。算出此時之浸漬前後的殘膜率。於此值為95~105%,可說是耐藥品性良好。殘膜率係依照下式來算出。
殘膜率(%)=浸漬後的膜厚÷浸漬前的膜厚×100。
使用接觸角計(協和界面科學(股)製,CA-D型),在室溫下於針尖形成直徑1.5mm的水滴,使此接觸以上述(2)記載的方法所製作的6吋矽晶圓上之閘極絕緣膜,形成液滴。測定此時所產生的液滴與面的角度,當作接觸角。此接觸角為90°以下時,可說是表面潤濕性良好。
對由上述(2)-2記載的方法所製作的6吋矽晶圓上之塗膜,使用光學顯微鏡的Lambdace STM-602,評價感度及解像度。再者,以100μm的線與間隙圖案形成1對1的寬之曝光量(以下稱為最合適曝光量)當作感度,將最合適曝光量之顯像後所得到的最小圖案尺寸當作解像度。
對於1克閘極絕緣材料,添加1克水。將pH試驗紙浸入其中,由其色變化來測定pH。
於以上述(2)方法所製作的6吋矽晶圓上之閘極絕緣膜上,藉由真空蒸鍍形成鋁電極,使用LCR計(橫河.Hewlett Packard(股)製),由下述(b)式來算出比介電常數K。
K=C.d/(ε.S) (b)
但是,C(F)係靜電容量,d(m)係絕緣膜厚,ε係真空的介電常數(8.85×10-12F/m)、S(m2)係上部電極(鋁電極)面積。
將0.10克共軛系聚合物的聚-3-己基噻吩(Aldrich公司製,區域規則性,數量平均分子量(Mn):13000,以下稱為P3HT)加到裝有5毫升氯仿的燒瓶中,在超音波洗淨機(井內盛榮堂(股)製US-2,輸出120W)中藉由超音波攪拌而得到P3HT的氯仿溶液。接著,在滴管中取得此溶液,以每次0.5毫升滴下到20毫升甲醇與10毫升0.1當量鹽酸的混合溶液之中,進行再沈澱。藉由0.1μm之孔徑的薄膜過濾器(PTFE公司製:四氟乙烯)來過濾分離採集固體的P3HT,以甲醇充分沖洗後,藉由真空乾燥來去除溶劑。進行再一次的溶解及再沈澱,而得到90毫克再沈澱物P3HT。
接著,將1.5毫克CNT(CNI公司製,單層CNT,純度95%,以下稱為單層CNT)及1.5毫克上述P3HT加到30毫升的氯仿中,邊冰冷邊使用超音波均化器(東京理化器械(股)製VCX-500)以250W輸出進行30分鐘的超音波攪拌。在已進行30分鐘超音波射的時間點暫時停止照射,追加1.5毫克P3HT,再照射1分鐘的超音波,而得到CNT複合體分散液A(相對於溶劑而言CNT濃度0.05g/l)。
於上述CNT複合體分散液A中,為了調查P3HT是否附著在CNT,使用薄膜過濾器來過濾5毫升的分散液A,在過濾器上捕集CNT。趁溶劑還沒有乾時,迅速將所捕集的CNT轉印到矽晶圓上,得到經乾燥的CNT。使用X射線光電子分光法(XPS),對此CNT進行元素分析,結果測出P3HT中所含有的硫元素。因此,可確認CNT複合體分散液A中的CNT附著P3HT。
接著,於上述分散液A中添加氯仿以稀釋到0.02g/l,使用薄膜過濾器(孔徑10μm,直徑25mm,MILLIPORE公司製Omnipore Membrane)來進行過濾,去除長度10μm以上的CNT。以所得到的濾液當作CNT複合體分散液B。於0.18毫升CNT複合體分散液B、0.12毫升氯仿的混合溶液中,添加0.90毫克當作有機半導體的下述OSC-1([1]),使用超音波洗淨機(井內盛榮堂(股)製US-2,輸出120W)照射30分鐘的超音波,以製作有機半導體溶液X。此時,調整濃度以使得OSC-1相對於氯仿而言的濃度為3g/l,CNT相對於OSC-1而言的濃度為0.4重量%。
使61.3克(0.45莫耳)甲基三甲氧基矽烷(以下稱為MTMSi)、12.3克(0.05莫耳)β-(3,4-環氧基環己基)乙基三甲氧基矽烷(以下稱為β-EpETMSi)、及99.2克(0.5莫耳)苯基三甲氧基矽烷(以下稱為PhTMSi)溶解在203.4克丙二醇單丁基醚(沸點170℃,以下稱為PGMB)中,於其中邊攪拌邊添加54.9克水、0.864克磷酸。於105℃的浴溫加熱所得到的溶液2小時,使內溫上升到90℃為止,餾出主要由副生成的甲醇所構成的成分。接著在130℃的浴溫加熱2小時,使內溫上升到118℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度26.0重量%的聚矽氧烷A。
量取50.0克所得之聚矽氧烷A,混合16.6克PGMB,在室溫攪拌2小時,而得到閘極絕緣材料A。接著,在6吋矽晶圓上及6吋玻璃基板上,以乾燥後的膜厚成為0.5μm的方式,使用旋塗機來塗布閘極絕緣材料A,接著使用熱板(大日本屏幕製造(股)製SCW-636),在120℃乾燥3分鐘,而得到塗膜。將所得到的塗膜在200℃熱處理60分鐘以製作閘極絕緣膜,對耐藥品性、表面潤濕性進行評價。測定此閘極絕緣材料A的pH,結果為3。
製作第1圖的FET。於玻璃製的基板1(膜厚0.7mm)上,藉由電阻加熱法,通過光罩,真空蒸鍍5nm鉻及50nm金,而形成閘極2。接著,將上述(2)製作的閘極絕緣材料A旋塗(2000rpm×30秒)在形成有上述閘極的玻璃基板上,將所得到的塗膜在氮氣流下於200℃加熱處理1小時,形成膜厚為600nm的閘極絕緣層3。接著,藉由電阻加熱法,通過光罩,以膜厚成為50nm的方式,真空蒸鍍金,而形成源極5及汲極6。
此等兩電極的寬(通道寬W)為0.5cm,兩電極的間隔(通道長L)為20μm。於形成有電極的基板上,滴下0.1毫升的上述(1)所製作的有機半導體溶液X,藉由旋塗(800rpm×0.3秒)來形成厚度25nm的半導體層4。於電極安裝引線後,將所得到的FET在真空烘箱中於100℃進行1小時的熱處理,徐徐冷卻到50℃以下後,開放大氣,使FET移動到測定箱,在真空中靜置。
接著,測定上述FET之閘極電壓(Vg)改變時的源極.汲極間電流(Id)-源極.汲極間電壓(Vsd)特性。測定係使用Hewlett Packard公司製皮可安培計/電壓源4140B,在真空下測定。由Vg=+50~-50V改變時Vsd=-5V的Id值之變化來求得線形區域的移動度,結果為0.2cm2/V.sec。又,由此時Id的最大值與最小值之比來求得開關比,結果為5×105。再者,由在Id=10-8往返的閘極電壓差之絕對值|Vg1-Vg2|來求得磁滯,結果為10V。
使95.3克(0.7莫耳)MTMSi、24.6克(0.1莫耳)β-EpETMSi、39.7克(0.2莫耳)PhTMSi溶解在183克PGMB中,於其中邊攪拌邊添加55.8克水、0.80克磷酸。於105℃的浴溫加熱所得到的溶液2小時,使內溫上升到90℃為止,餾出主要由副生成的甲醇所構成的成分。接著在130℃的浴溫加熱2小時,使內溫上升到118℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度28.0重量%的聚矽氧烷B。量取50.0克所得之聚矽氧烷B,當作氧化鋯系硬化劑,添加0.40克氧化鋯四(乙醯基丙酮化物)(以下稱為ZrAcAc),再混合21.7克PGMB,於室溫攪拌2小時,而得到閘極絕緣材料B。測定此閘極絕緣材料B的pH,結果為3。接著,除了使用閘極絕緣材料B當作閘極絕緣材料,塗膜的加熱處理為在180℃進行60分鐘以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
使40.9克(0.3莫耳)MTMSi、73.8克(0.3莫耳)β-EpETMSi、79.3克(0.4莫耳)PhTMSi溶解在231克丙二醇單丙基醚(沸點150℃,以下稱為PGMP)中,於其中邊攪拌邊添加59.4克水、0.59克磷酸。於105℃的浴溫加熱所得到的溶液2小時,使內溫上升到90℃為止,餾出主要由副生成的甲醇所構成的成分。接著在140℃的浴溫加熱2小時,使內溫上升到118℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度24.3重量%的聚矽氧烷C。量取50.0克所得之聚矽氧烷C,當作鎂系硬化劑,添加0.60克鎂雙(乙醯基醋酸酯)(商品名Nasemu Magnesium,日本化學產業(股)公司製,以下稱為MgAcAc),再混合12.3克二乙二醇乙基甲基醚(沸點176℃,以下稱為DGEM),於室溫攪拌2小時,而得到閘極絕緣材料C。測定此閘極絕緣材料C的pH,結果為4。接著,除了使用閘極絕緣材料C當作閘極絕緣材料,塗膜的加熱處理為在230℃進行5分鐘以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
使66.7克(0.49莫耳)MTMSi、2.36克(0.01莫耳)γ-環氧丙氧基丙基三甲氧基矽烷(以下稱為γ-GPTMSi)、99.2克(0.5莫耳)PhTMSi溶解在471.1克丙二醇單甲基醚(沸點121℃,以下稱為PGMM)中,於其中邊攪拌邊添加54.2克水、0.85克磷酸。於105℃的浴溫加熱所得到的溶液2小時,使內溫上升到90℃為止,餾出主要由副生成的甲醇所構成的成分。接著在115℃的浴溫加熱4小時,使內溫上升到118℃為止,餾出主要由水與PGMM所構成的成分後,冷卻到室溫為止,得到固體成分濃度40.0重量%的聚矽氧烷D。量取50.0克所得之聚矽氧烷D,添加1.00克四異丙氧基化鈦(以下稱為TiTP),再混合52.5克丙二醇單第三丁基醚(沸點143℃,以下稱為PGMtB),於室溫攪拌2小時,而得到閘極絕緣材料D。測定此閘極絕緣材料D的pH,結果為3。接著,除了使用閘極絕緣材料D當作閘極絕緣材料以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
量取50.0克實施例1得所之固體成分濃度26.0重量%的聚矽氧烷A,混合16.5克PGMB,添加0.10克光酸產生劑PAI-101(綠化學(股)製)及0.03克增感劑的9,10-二丁氧基蒽(東京化成工業(股)製,以下稱為DBA),於室溫攪拌2小時,而得到閘極絕緣材料A1。測定此閘極絕緣材料A1的pH,結果為3。使用所得到的閘極絕緣材料A1,對感光特性進行評價。接著,除了使用閘極絕緣材料A1當作閘極絕緣材料,塗膜的加熱處理為在170℃進行60分鐘以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
除了添加200克(0.66莫耳)矽溶膠(PL-2L,扶桑化學製,矽石粒子濃度20重量%)以外,與實施例1同樣地進行聚矽氧烷合成,得到固體成分濃度35重量%的聚矽氧烷A2。量取50.0克所得到的聚矽氧烷A2,添加1.00克TiTP,再混合40.0克PGMtB,於室溫攪拌2小時,而得到閘極絕緣材料A2。測定此閘極絕緣材料A2的pH,結果為3。接著,除了使用閘極絕緣材料A2當作閘極絕緣材料,塗膜的加熱處理為在180℃進行60分鐘以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
量取50.0克實施例1所得之固體成分濃度26.0重量%的聚矽氧烷A,混合16.5克PGMB,添加0.15克光酸產生劑PAl-101及0.15克當作具有腈基的化合物之戊二腈(東京化成工業(股)製,以下稱為GN),於室溫攪拌2小時,而得到閘極絕緣材料A3。測定此閘極絕緣材料A3的pH,結果為3。接著,除了使用閘極絕緣料A3當作閘極絕緣材料,塗膜的加熱處理為在200℃進行60分鐘以外,與實施例5同樣地製作閘極絕緣膜及FET,進行評價。
除了溶劑為異丙基醇(沸點82.4℃,以下稱為IPA),聚縮合加熱條件為在內溫80℃進行3小時以外,與實施例1同樣地合成聚矽氧烷,得到固體成分19.5%的聚矽氧烷F。量取50.0克所得之聚矽氧烷F,當作鋁系硬化劑,添加0.60克鋁三(乙基乙醯基醋酸酯)(商品名ALCH-TR,川研精密化學(股)公司製,以下稱為AlTEA),於室溫攪拌2小時,而得到閘極絕緣材料F。測定此閘極絕緣材料F的pH,結果為3。使用所得到的閘極絕緣材料F,藉由旋塗機來形成塗膜,結果由為溶劑的沸點低,看到一部分的膜不均。接著,除了使用閘極絕緣材料F當作閘極絕緣材料,塗膜的加熱處理為在180℃進行60分鐘以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
除了56.9克(0.3莫耳)3-甲基丙烯醯氧基丙基三甲氧基矽烷甲基三甲氧基矽烷(以下稱為McTMSi)、24.6克(0.10莫耳)β-EpETMSi及139克(0.6莫耳)PhTMSi以外,與實施例1同樣地合成聚矽氧烷,得到固體成分26.0%的聚矽氧烷G。量取50.0克所得之聚矽氧烷G,添加16.6克PGMB、0.60克AlTEA,於室溫攪拌2小時,而得到閘極絕緣材料G。測定此閘極絕緣材料G的pH,結果為3。接著,除了使用閘極絕緣材料G當作閘極絕緣材料以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
除了使用34.1克(0.25莫耳)MTMSi、99.2克(0.5莫耳)PhTMSi及30.1克(0.25莫耳)二甲基二甲氧基矽烷(以下稱為DMDMSi)以外,與實施例1同樣地合成聚矽氧烷,得到固體成分濃度26.5重量%的聚矽氧烷H。
量取50.0克所得之聚矽氧烷H,混合16.0克PGMB,添加0.60克AlTEA,於室溫攪拌2小時,而得到閘極絕緣材料H。
接著,除了使用閘極絕緣材料H當作閘極絕緣材料以外,與實施例1同樣地製作閘極絕緣膜,對耐藥品性、表面潤濕性進行評價。又,將有機半導體複合物X旋塗在前述閘極絕緣膜上,但發生彈開,無法形成膜。
將聚乙烯基苯酚(Aldrich公司製,重量平均分子量(Mw):20000,以下稱為PVP)、聚蜜胺-co-甲醛(Aldrich公司製,數量平均分子量(Mn):432,以下稱為PMF)及丙二醇單甲基醚醋酸酯(沸點:146℃,Aldrich公司製,以下稱為PGMEA)以PVP:PMF:PGMEA=10:5:100的重量比混合,而成為閘極絕緣材料I。
接著,除了使用閘極絕緣材料I當作閘極絕緣材料以外,與實施例1同樣地製作閘極絕緣膜及FET,進行評價。
使20.4克(0.15莫耳)MTMSi、39.7克(0.2莫耳)PhTMSi、37.0克(0.15莫耳)β-EpETMSi溶解在88.5克PGMEA中,於其中邊攪拌邊添加29.7克水與0.39克磷酸的混合溶液。於70℃的浴溫加熱所得到的溶液1小時,餾出主要由副生成的甲醇所構成的成分。接著,於115℃的浴溫加熱3小時,使內溫上升到110℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度48.20重量%的聚矽氧烷J。
量取10.0克所得到的聚矽氧烷J,添加15.0克PGMEA、0.25克ZrAcAc,於室溫攪拌2小時,而得到閘極絕緣材料J。
接著,除了使用閘極絕緣材料J當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
使18.4克(0.135莫耳)MTMSi、29.8克(0.15莫耳)PhTMSi、3.70克(0.015莫耳)β-EpETMSi溶解在46.7克PGMEA中,於其中邊攪拌邊添加16.5克水與0.21克磷酸的混合溶液。於70℃的浴溫加熱所得到的溶液1小時,餾出主要由副生成的甲醇所構成的成分。接著,於115℃的浴溫加熱3小時,使內溫上升到110℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度48.8重量%的聚矽氧烷K。
量取10.0克所得之聚矽氧烷K,添加15.0克PGMEA、0.25克ZrAcAc,於室溫攪拌2小時,而得到閘極絕緣材料K。
接著,除了使用閘極絕緣材料K當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
使6.81克(0.050莫耳)MTMSi、19.8克(0.10莫耳)PhTMSi、2.64克(0.010莫耳)β-EpETMSi、5.96克(0.0080莫耳)聚四乙氧基矽烷(商品名Silicate 40,多摩化學工業(股)製,以下稱為PTES)溶解在32.16克PGMEA中,於其中邊攪拌邊添加10.6克水與0.14克磷酸的混合溶液。於70℃的浴溫加熱所得到的溶液1小時,餾出主要由副生成的乙醇與甲醇所構成的成分。接著,於115℃的浴溫加熱3小時,使內溫上升到110℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度43.9重量%的聚矽氧烷L。
量取10.0克所得之聚矽氧烷L,添加13.0克PGMEA、0.25克ZrAcAc,於室溫攪拌2小時,而得到閘極絕緣材料L。
接著,除了使用閘極絕緣材料L當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
使54.5克(0.4莫耳)MTMSi、24.6克(0.1莫耳)β-EpETMSi、99.2克(05莫耳)PhTMSi溶解在160.0克PGMEA,於其中邊攪拌邊添加55.9克水、0.71克磷酸。於105℃的浴溫加熱所得到的溶液2小時,使內溫上升到90℃為止,餾出主要由副生成的甲醇所構成的成分。接著,於130℃的浴溫加熱2小時,使內溫上升到118℃為止,餾出主要由水所構成的成分後,冷卻到室溫為止,得到固體成分濃度45.4重量%的聚矽氧烷M。量取10.0克所得之聚矽氧烷M,添加14.0克PGMEA、0.25克ZrAcAc,於室溫攪拌2小時,而得到閘極絕緣材料M。
接著,除了使用閘極絕緣材料M當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替β-EpETMSi,使用β-(3,4-環氧基環己基)乙基甲基二甲氧基矽烷(以下稱為β-EpEMDMSi)以外,與實施例13同樣地合成聚矽氧烷N,製作閘極絕緣材料N。
接著,除了使用閘極絕緣材料N當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替β-EpETMSi,使用β-(3,4-環氧基環己基)丙基三甲氧基矽烷(以下稱為β-EpPTMSi)以外,與實施例13同樣地合成聚矽氧烷O,製作閘極絕緣材料O。
接著,除了使用閘極絕緣材料O當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替β-EpETMSi,使用γ-環氧丙氧基丙基甲基二甲氧基矽烷(以下稱為γ-GPMDMSi)以外,與實施例13同樣地合成聚矽氧烷P,製作閘極絕緣材料P。
接著,除了使用閘極絕緣材料P當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替β-EpETMSi,使用γ-環氧丙氧基乙基三甲氧基矽烷(以下稱為γ-GETMSi)以外,與實施例13同樣地合成聚矽氧烷Q,製作閘極絕緣材料Q。
接著,除了使用閘極絕緣材料Q當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替MTMSi,使用乙基三甲氧基矽烷(以下稱為ETMSi)以外,與實施例13同樣地合成聚矽氧烷R,製作閘極絕緣材料R。
接著,除了使用閘極絕緣材料R當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替MTMSi,使用苄基三甲氧基矽烷(以下稱為BTMSi)以外,與實施例13同樣地合成聚矽氧烷S,製作閘極絕緣材料S。
接著,除了使用閘極絕緣材料S當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替PhTMSi,使用對甲苯基三甲氧基矽烷(以下稱為ToTMSi)以外,與實施例13同樣地合成聚矽氧烷T,製作閘極絕緣材料T。
接著,除了使用閘極絕緣材料T當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替PhTMSi,使用β-萘基三甲氧基矽烷(以下稱為NaTMSi)以外,與實施例13同樣地合成聚矽氧烷U,製作閘極絕緣材料U。
接著,除了使用閘極絕緣材料U當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
量取10.0克實施例13所得之聚矽氧烷M,添加15.0克PGMEA、0.25克ZrAcAc、0.25克3-胺丙基三乙氧基矽烷(以下稱為APTESi),於室溫攪拌2小時,而得到閘極絕緣材料V。
接著,除了使用閘極絕緣材料V當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了代替APTESi,使用十八基三乙氧基矽烷(以下稱為OTESi)以外,與實施例22同樣地製作閘極絕緣材料W。
接著,除了使用閘極絕緣材料W當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了使用對三氟苯基三乙氧基矽烷(以下稱為TFPhTESi)代替APTESi以外,與實施例22同樣地製作閘極絕緣材料X。
接著,除了使用閘極絕緣材料X當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了絕緣層的加熱處理為在大氣中200℃、1小時以外,與實施例13同樣地製作FET,進行評價。
量取5.0克實施例10所得之聚矽氧烷J及5.0克實施例12所得之聚矽氧烷L,添加15.0克PGMEA、0.25克ZrAcAc,於室溫攪拌2小時,而得到閘極絕緣材料Y。
接著,除了使用閘極絕緣材料Y當作閘極絕緣材料以外,與實施例1同樣地製作FET,進行評價。
除了使用下述OSC-2([2])當作有機半導體以外,與實施例13同樣地製作FET,進行評價。
除了使用P3HT當作有機半導體以外,與實施例13同樣地製作FET,進行評價。
除了不用CNT以外,與實施例15同樣地製作FET,進行評價。
以下顯示實施例1~29所用的矽烷化合物之構造。
表1中顯示實施例1~9及比較例1~2的閘極絕緣材料組成,表3中顯示實施例10~29的閘極絕緣材料組成。又,表2中顯示實施例1~9及比較例1~2的FET評價結果,表4中顯示實施例10~29的FET評價結果。
本發明的閘極絕緣材料及閘極絕緣膜係為可用於智慧卡、安全標籤、平面顯示器用的電晶體陣列等所可利用的有機場效型電晶體或其它有機電晶體。
1...基板
2...閘極
3...閘極絕緣層
4...半導體層
5...源極
6...汲極
第1圖係顯示本發明一態樣的FET之模型剖面圖。
第2圖係顯示本發明另一態樣的FET之模型剖面圖。
Claims (9)
- 一種閘極絕緣材料,其特徵為含有至少以通式(1)所示的矽烷化合物及通式(2)所示的含環氧基的矽烷化合物當作共聚合成分的聚矽氧烷,該聚矽氧烷中的從通式(2)所示的含環氧基的矽烷化合物而來的構成單位之含量為0.1~40莫耳%,R1 mSi(OR2)4-m (1)此處,R1表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R1以複數存在時,各R1可相同或不同;R2表示烷基或環烷基,於R2以複數存在時,各R2可相同或不同;m表示1~3的整數;R3 nR4 1Si(OR5)4-n-1 (2)此處,R3表示在鏈的一部分具有1個以上的環氧基之烷基或環烷基,於R3以複數存在時,各R3可相同或不同;R4表示氫、烷基、環烷基、雜環基、芳基、雜芳基或烯基,於R4以複數存在時,各R4可相同或不同;R5表示烷基或環烷基,於R5以複數存在時,各R5可相同或不同;1表示0~2的整數,n表示1或2;但是,1+n≦3。
- 如申請專利範圍第1項之閘極絕緣材料,其中該通式(1)中的m個R1的至少1個為芳基或雜芳基。
- 如申請專利範圍第1或2項之閘極絕緣材料,其中更含有在1氣壓的沸點為110~200℃的溶劑。
- 如申請專利範圍第1或2項之閘極絕緣材料,其中更含有粒子。
- 如申請專利範圍第1或2項之閘極絕緣材料,其中更含有當作硬化劑的金屬烷氧化物化合物及/或金屬螯合化合物。
- 如申請專利範圍第1或2項之閘極絕緣材料,其中更含藉由光而產生酸的化合物。
- 如申請專利範圍第1或2項之閘極絕緣材料,其pH為2~7。
- 一種閘極絕緣膜,其係藉由在100℃~300℃的範圍熱處理由塗布如申請專利範圍第1至7項中任一項之閘極絕緣材料所形成的塗膜而得。
- 一種有機場效型電晶體,其具有含如申請專利範圍第8項之閘極絕緣膜的閘極絕緣層、閘極、半導體層、源極及汲極。
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US20110068417A1 (en) | 2011-03-24 |
EP2259289A4 (en) | 2013-09-04 |
CN102089870A (zh) | 2011-06-08 |
WO2009116373A1 (ja) | 2009-09-24 |
JP5407860B2 (ja) | 2014-02-05 |
KR20100126407A (ko) | 2010-12-01 |
CN102089870B (zh) | 2013-08-28 |
TW201001772A (en) | 2010-01-01 |
JPWO2009116373A1 (ja) | 2011-07-21 |
EP2259289A1 (en) | 2010-12-08 |
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