TWI719092B - 樹脂組成物 - Google Patents
樹脂組成物 Download PDFInfo
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- TWI719092B TWI719092B TW105141427A TW105141427A TWI719092B TW I719092 B TWI719092 B TW I719092B TW 105141427 A TW105141427 A TW 105141427A TW 105141427 A TW105141427 A TW 105141427A TW I719092 B TWI719092 B TW I719092B
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- 239000011342 resin composition Substances 0.000 title claims abstract description 73
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 5
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 4
- -1 quinonediazide compound Chemical class 0.000 claims description 24
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明之課題係提供一種熱硬化性的樹脂組成物。
作為解決本發明課題之技術手段之樹脂組成物,其係含有(A)成分、(B)成分及溶劑之樹脂組成物,基於前述樹脂組成物中除去前述溶劑後的全部成分之含有量,前述(B)成分之含有量為0.1質量%至5.0質量%。(A)成分:具有下述式(1)所表示之構造單位及下述式(2)所表示之構造單位之自交聯性共聚物,(B)成分:下述式(3)所表示之化合物,
(式中,R0分別獨立表示為氫原子或甲基,X表示為-O-基或-NH-基,R1表示為單鍵或伸烷基,R2表示為烷基,a表示為1至5的整數,b表示為0至4的整數,R3表示為具有醚鍵及/或酯鍵之2價的有機基,R5表示為烷基,f表示為1至5的整數,g表示為0至4的整數,R6表示為單鍵或伸烷基,Y表示為單鍵或酯鍵,A表示為可包含至少1個雜原子之1價至4價的有機基或雜原子,h表示為1至4的整數)。
Description
本發明係關於一種樹脂組成物、及由該樹脂組成物所形成的硬化膜、保護膜、平坦化膜及微透鏡。本發明之樹脂組成物係不含有醌二疊氮化合物(quinone diazide compound)等的感光劑之組成物,本發明之樹脂組成物中所包含之自交聯性共聚物,不伴隨交聯劑而共聚物彼此可熱交聯來形成硬化膜。
液晶顯示器、CCD/CMOS影像感測器等的電子裝置,在其製造步驟中,進行被暴露在溶劑或酸或鹼溶液等的藥液之處理、或濺鍍、乾式蝕刻、回流焊錫等的被暴露在高溫之處理。藉由如此般的處理為了防止元件劣化或損傷,而進行在元件上形成對如此般的處理具有耐性的硬化膜來作為保護膜。對於如此般的保護膜要求著耐藥品性、高透明性、耐熱性、耐濕性等。進而,為了製造具備有高可靠性的前述電子裝置,對於前述硬化膜亦要求著長期的耐熱性及耐濕性。
在形成有如濾色器(color filter)般凹凸的表面上來形成前述硬化膜之情形時,就稍後接著的步驟中之製程裕度之確保、裝置特性的均勻性之確保等的觀點而言,是需要平坦化性為高的硬化膜。又,也進行由如此般的硬化膜來製作微透鏡。
作為CCD/CMOS影像感測器用微透鏡之製作方法之一,已知有回蝕刻法(專利文獻1及專利文獻2)。即,在濾色器上所形成的微透鏡用樹脂層上形成阻劑圖型(resist pattern),藉由熱處理使該阻劑圖型回焊來形成透鏡圖型。藉由將該阻劑圖型進行回焊所形成的透鏡圖型作為蝕刻遮罩(etching mask),對下層的微透鏡用樹脂層進行回蝕刻並將透鏡圖型形狀轉印至微透鏡用樹脂層來製作微透鏡。
例如專利文獻3至專利文獻5中揭示著一種微透鏡形成所使用之樹脂組成物。然而,皆為感光性(感放射線性)樹脂組成物,可以說是不適合藉由上述之回蝕刻法來形成微透鏡之材料。
專利文獻6中揭示著一種微透鏡形成所使用之非感光性樹脂組成物。但,由該非感光性樹脂組成物所形成的膜之耐濕性為不明確。
[專利文獻1]日本特開平1-10666號公報
[專利文獻2]日本特開平6-112459號公報
[專利文獻3]日本特開2006-251464號公報
[專利文獻4]日本特開2007-033518號公報
[專利文獻5]日本特開2007-171572號公報
[專利文獻6]國際公開WO2014/065100號
本發明係基於前述情事而完成之發明,本發明之目的係提供一種可形成具有優異的耐藥品性、耐熱性、耐濕性、透明性及平坦化性的硬化膜之樹脂組成物。又,本發明之其他目的係提供一種具有優異的耐藥品性、耐熱性、耐濕性及透明性的微透鏡。
本發明人為了解決前述課題而進行了深入研究,結果完成了本發明。即,本發明係一種樹脂組成物,其係含有下述(A)成分、下述(B)成分及溶劑之樹脂組成物,基於前述樹脂組成物中除去前述溶劑後的全部成分之含有量,前述(B)成分之含有量為0.1質量%至5.0質量%,(A)成分:具有下述式(1)所表示之構造單位及下述式(2)所表示之構造單位之自交聯性共聚物,(B)成分:下述式(3)所表示之化合物,
(式中,R0分別獨立表示為氫原子或甲基,X表示為-O-基或-NH-基,R1表示為單鍵或碳原子數1至6的直鏈狀或支鏈狀的伸烷基,R2表示為碳原子數1至6的直鏈狀或支鏈狀的烷基,a表示為1至5的整數,b表示為0至4的整數,且a與b為滿足1≦a+b≦5,若b表示為2、3或4時,R2可相互不同,R3表示為下述式(I)、式(II)或式(III)所表示之2價的有機基,若R3表示為下述式(I)所表示之2價的有機基時,該式(I)中之羰基係與上述式(2)所表示之構造單位的主鏈鍵結,R4表示為具有環氧基的有機基,R5表示為碳原子數1至6的直鏈狀或支鏈狀的烷基,f表示為1至5的整數,g表示為0至4的整數,且f與g為滿足1≦f+g≦5,若g表示為2、3或4時,R5可相互不同,R6表示為單鍵或碳原子數1至6的直鏈狀或支鏈狀的伸烷基,Y表示為單鍵或酯鍵,A表示為可包含至少1個雜原子之1價、2價、3價或4價的有機基或表示為雜原子,h表示為1至4的整
數)
(式中,c表示為0至3的整數,d表示為1至3的整數,e分別獨立表示為2至6的整數)。
前述式(3)所表示之化合物中,若A表示為包含至少1個雜原子之1價、2價、3價或4價的有機基或表示為雜原子之情形時,作為該雜原子可舉出例如氮原子、氧原子及硫原子。又,作為前述1價、2價、3價或4價的有機基,可舉出例如碳原子數1至20的直鏈狀或支鏈狀的烴基、芳香族烴基、雜環基。又,若Y表示為酯鍵之情形時,該酯鍵表示為-C(=O)O-。前述式(3)係例如下述式(3a)至式(3e)所表示。
(式中,A及h係與前述式(3)之定義為相同)。
前述式(2)所表示之構造單位係例如下述式(2-1)或式(2-2)所表示之構造單位。
(式中,R0分別獨立表示為氫原子或甲基,R3表示為前述式(I)、式(II)或式(III)所表示之2價的有機基)。
前述(A)成分之自交聯性共聚物係進而亦可具有下述式(4)所表示之構造單位。
(式中,R0分別獨立表示為氫原子或甲基,Y表示為苯基、聯苯基或萘基,該苯基、該聯苯基及該萘基係氫原子的一部分或全部可被碳原子數1至10的烷基、碳原子數1至10的烷氧基、氰基或鹵化基所取代)。
本發明之樹脂組成物係例如作為保護膜用樹脂組成物、平坦化膜用樹脂組成物及微透鏡用樹脂組成物為有用。又,本發明係一種硬化膜之製作方法,其係包含:將前述樹脂組成物塗布在基材上之步驟、以80℃至300℃的溫度烘烤0.3分鐘至60分鐘之步驟。進而,本發明係一種微透鏡之製作方法,其係包含:在藉由前述方法
所製作的硬化膜上形成阻劑圖型之步驟、藉由加熱處理使前述阻劑圖型回焊來形成透鏡圖型之步驟、將前述透鏡圖型作為遮罩對前述硬化膜進行回蝕刻並將該透鏡圖型的形狀轉印至該硬化膜之步驟。
由本發明之樹脂組成物所形成的硬化膜係具有優異的耐藥品性、耐熱性、耐濕性、透明性及平坦化性。據此,由本發明之樹脂組成物所形成的硬化膜,在其形成步驟、或配線等的周邊裝置之形成步驟中,當進行被暴露在溶劑或酸或鹼溶液等的藥液之處理、或濺鍍、乾式蝕刻、回流焊錫等的被暴露在高溫之處理之情形時,可顯著地減少元件劣化或損傷之可能性。進而,若使用由本發明之樹脂組成物所形成之硬化膜之情形時,可製造具有高可靠性的電子裝置。又,由本發明之樹脂組成物來形成保護膜、平坦化膜或微透鏡,並在其上塗布阻劑、或進行電極/配線形成步驟之情形時,亦可顯著地減少與阻劑之混合(mixing)、因藥液而致使保護膜、平坦化膜或微透鏡之變形及剝離之類的問題。因此,本發明之樹脂組成物係適合作為形成保護膜、平坦化膜及微透鏡之材料。
[圖1]圖1係表示利用光學顯微鏡來觀察在烘箱內以
150℃加熱1,000小時後的硬化膜表面之結果。
[圖2]圖2係表示利用光學顯微鏡來觀察在恆溫恆濕器內以85℃ 85%RH下靜置1,000小時後的硬化膜表面之結果。
本發明係含有自交聯性共聚物、前述式(3)所表示之化合物、與溶劑之樹脂組成物。以下說明各成分之詳細。本發明之樹脂組成物中除去溶劑後的全部成分(以下亦稱為固形分)係通常基於樹脂組成物的全部質量為1質量%至50質量%。
<(A)成分>
本發明之樹脂組成物中所包含之(A)成分係自交聯性共聚物、且具有前述式(1)所表示之構造單位及式(2)所表示之構造單位。
作為形成前述式(1)所表示之構造單位之化合物(單體)之具體例,可舉出2-羥基苯基(甲基)丙烯酸酯、3-羥基苯基(甲基)丙烯酸酯、4-羥基苯基(甲基)丙烯酸酯、4-羥基苄基(甲基)丙烯酸酯、4-羥基苯乙基(甲基)丙烯酸酯、3,5-二甲基-4-羥基苯基(甲基)丙烯酸酯、3,5-二甲基-4-羥基苄基(甲基)丙烯酸酯、3,5-二甲基-4-羥基苯乙基(甲基)丙烯酸酯、N-(2-羥基
苯基)(甲基)丙烯醯胺、N-(3-羥基苯基)(甲基)丙烯醯胺、N-(4-羥基苯基)(甲基)丙烯醯胺、N-(4-羥基苄基)(甲基)丙烯醯胺、N-(4-羥基苯乙基)(甲基)丙烯醯胺、N-(3,5-二甲基-4-羥基苯基)(甲基)丙烯醯胺、N-(3,5-二甲基-4-羥基苄基)(甲基)丙烯醯胺、及N-(3,5-二甲基-4-羥基苯乙基)(甲基)丙烯醯胺。尚,該等之化合物係可單獨使用、亦可組合2種以上來使用。尚,本說明書中,(甲基)丙烯酸酯係指甲基丙烯酸酯及丙烯酸酯,(甲基)丙烯醯胺係指甲基丙烯醯胺及丙烯醯胺。
作為形成前述式(2)所表示之構造單位之化合物(單體)之具體例,可舉出下述式(2-3)至式(2-18)所表示之單體。尚,該等之單體系可單獨使用、亦可組合2種以上來使用。
本發明之樹脂組成物中所包含之自交聯性共
聚物,除了前述式(1)所表示之構造單位及式(2)所表示之構造單位以外,進而可含有前述式(4)所表示之構造單位。藉由調節前述式(4)所表示之構造單位之含有量,從而能夠將硬化膜的光學特性或乾式蝕刻速率調節到更寬的範圍。
作為形成前述式(4)所表示之構造單位之化合物(單體)之具體例,可舉出苯乙烯、α-甲基苯乙烯、2-甲基苯乙烯、3-甲基苯乙烯、4-甲基苯乙烯、4-tert-丁基苯乙烯、4-甲氧基苯乙烯、4-氰基苯乙烯、4-氟苯乙烯、4-氯苯乙烯、4-溴苯乙烯、4-乙烯基聯苯基、1-乙烯基萘及2-乙烯基萘。該等之化合物係可單獨使用、亦可組合2種以上來使用。
具有前述式(1)所表示之構造單位及式(2)所表示之構造單位之自交聯性共聚物中,相對於前述式(1)所表示之構造單位及前述式(2)所表示之構造單位的和100mol%,前述式(1)所表示之構造單位的含有率為5mol%至95mol%,較佳為10mol%至90mol%,前述式(2)所表示之構造單位的含有率為5mol%至95mol%,較佳為10mol%至90mol%。
若前述自交聯性共聚物進而具有前述式(4)所表示之構造單位之情形時,相對於前述式(1)所表示之構造單位、前述式(2)所表示之構造單位及前述式(4)所表示之構造單位的和100mol%,前述式(1)所表示之構造單位的含有率為5mol%至90mol%,較佳為
10mol%至80mol%,前述式(2)所表示之構造單位的含有率為5mol%至90mol%,較佳為10mol%至80mol%,前述式(4)所表示之構造單位的含有率為5mol%至90mol%,較佳為10mol%至80mol%。
前述自交聯性共聚物的重量平均分子量通常為1,000至100,000,較佳為3,000至50,000。尚,重量平均分子量係藉由凝膠滲透層析法(GPC)使用聚苯乙烯作為標準試樣所得到的值。
又,本發明之樹脂組成物中之前述自交聯性共聚物之含有量,基於該樹脂組成物中之固形分之含有量通常為1質量%至99質量%,較佳為5質量%至95質量%。
本發明中,得到前述自交聯性共聚物之方法並無特別限定,但一般而言,藉由除了形成前述前述式(1)所表示之構造單位之化合物(單體)及形成前述式(2)所表示之構造單位之化合物(單體)、或該等之化合物(單體)以外,還將形成前述式(4)所表示之構造單位之化合物(單體),在聚合起始劑存在下的溶劑中,通常以50℃至120℃的溫度下使其進行聚合反應而可得到。以如此般之方式所得到之共聚物,通常為溶解在溶劑中之溶液狀態,也能夠在此狀態下不進行離析而使用於本發明之樹脂組成物。
又,將以如上述般之方式所得到之自交聯性共聚物的溶液投入至已進行攪拌的己烷、二乙基醚、甲
醇、水等的不良溶劑中並使該共聚物再沈澱,將所生成的沈澱物進行過濾.洗淨後,藉由在常壓或減壓下進行常溫乾燥或加熱乾燥,從而可將該共聚物作成粉體。藉由如此般的操作,可除去與前述自交聯性共聚物共存的聚合起始劑或未反應化合物。本發明中,前述自交聯性共聚物的粉體可直接使用、或可將該粉體再溶解至例如後述之溶劑中而以溶液的狀態來使用。
<(B)成分>
本發明之樹脂組成物中所包含之(B)成分為前述式(3)所表示之化合物,係被添加作為抗氧化劑。作為前述式(3)所表示之化合物之具體例,可舉出例如下述式(3-1)至式(3-10)所表示之化合物。尚,該等之化合物可單獨使用、亦可組合2種以上來使用。
又,本發明之樹脂組成物中之(B)成分之含有量,基於該樹脂組成物中之固形分之含有量為0.1質量%至5.0質量%,較佳為0.2質量%至5.0質量%。若前述(B)成分之含有量超過5.0質量%之情形時,使用包含該(B)成分之樹脂組成物並在基材上所形成之硬化膜,由於長期的耐熱性及耐濕性為低、且在硬化膜表面上會產生異物,因而該硬化膜的平滑性為惡化,故為不佳。
本發明之樹脂組成物之調製方法並無特別限定,可舉出將例如具有前述式(1)所表示之構造單位及式(2)所表示之構造單位之共聚物、或具有前述式(1)所表示之構造單位、式(2)所表示之構造單位及式(4)所表示之構造單位之共聚物、與前述式(3)所表示之化
合物溶解在溶劑中來製成均勻的溶液之方法。進而,可舉出在該調製方法的適當階段中,因應所需進而添加其他的添加劑來混合之方法。
作為上述溶劑,只要是可溶解前述自交聯性共聚物及前述式(3)所表示之化合物即可並無特別限定。作為如此般的溶劑,可舉出例如乙二醇單甲基醚、乙二醇單乙基醚、甲基溶纖劑乙酸酯、乙基溶纖劑乙酸酯、二乙二醇單甲基醚、二乙二醇單乙基醚、丙二醇、丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、丙二醇單乙基醚乙酸酯、丙二醇丙基醚乙酸酯、丙二醇單丁基醚、丙二醇單丁基醚乙酸酯、甲苯、二甲苯、甲基乙基酮、環戊酮、環己酮、2-羥基丙酸乙酯、2-羥基-2-甲基丙酸乙酯、乙氧基乙酸乙酯、羥基乙酸乙酯、2-羥基-3-甲基丁酸甲酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸甲酯、丙酮酸甲酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乳酸丁酯、2-庚酮及γ-丁內酯。該等之溶劑可單獨使用、亦可組合2種以上來使用。
在該等之溶劑中,就將本發明之樹脂組成物塗布在基材上所形成之硬化膜的平坦性提升之觀點而言,以丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚、丙二醇單丙基醚、2-庚酮、乳酸乙酯、乳酸丁酯、環戊酮及環己酮為較佳。
又,本發明之樹脂組成物,就提升塗布性之目的下,亦可含有界面活性劑。作為該界面活性劑,可舉
出例如聚氧乙烯月桂醚、聚氧乙烯硬脂醚、聚氧乙烯鯨蠟醚、聚氧乙烯油基醚等的聚氧乙烯烷基醚類、聚氧乙烯苯基辛基醚、聚氧亞乙基壬基苯基醚等的聚氧乙烯烷芳醚類、聚氧乙烯.聚氧化丙烯嵌段共聚物類、去水山梨醇單月桂酸酯、去水山梨醇單棕櫚酸酯、去水山梨醇單硬脂酸酯、去水山梨醇單油酸酯、去水山梨醇三油酸酯、去水山梨醇三硬脂酸酯等的去水山梨醇脂肪酸酯類、聚氧乙烯去水山梨醇單月桂酸酯、聚氧乙烯去水山梨醇單棕櫚酸酯、聚氧乙烯去水山梨醇單硬脂酸酯、聚氧乙烯去水山梨醇三油酸酯、聚氧乙烯去水山梨醇三硬脂酸酯等的聚氧乙烯去水山梨醇脂肪酸酯類等的非離子系界面活性劑、F-Top〔註冊商標〕EF301、同EF303、同EF352(以上為三菱Materials電子化成(股)製)、MEGAFACE〔註冊商標〕F-171、同F-173、同R-30、同R-40、同R-40-LM(以上、DIC(股)製)、Fluorad FC430、同FC431(以上為住友3M(股)製)、AashiGuard〔註冊商標〕AG710、Surflon〔註冊商標〕S-382、同SC101、同SC102、同SC103、同SC104、同SC105、同SC106(旭硝子(股)製)、FTX-206D、FTX-212D、FTX-218、FTX-220D、FTX-230D、FTX-240D、FTX-212P、FTX-220P、FTX-228P、FTX-240G等的Ftergent series((股)NEOS製)等的氟系界面活性劑、有機矽氧烷聚合物KP341(信越化學工業(股)製)。該等之界面活性劑可單獨使用、亦可組合2種以上來使用。
又,若使用前述界面活性劑之情形時,本發明之樹脂組成物中之界面活性劑之含有量,基於該樹脂組成物中之固形分之含有量為0.001質量%至3質量%,較佳為0.005質量%至1質量%,又較佳為0.01質量%至0.5質量%。
本發明之樹脂組成物,由於該樹脂組成物所包含之共聚物為自交聯型,故不一定需要添加交聯劑,但在不損及本發明之效果,因應所需可包含交聯劑。又,本發明之樹脂組成物,在不損及本發明之效果,因應所需可包含硬化助劑、紫外線吸收劑、增感劑、可塑劑、密著輔助劑等的添加劑。
<硬化膜、保護膜及平坦化膜之製作方法>
對於使用本發明之樹脂組成物之硬化膜、保護膜及平坦化膜之製作方法進行說明。藉由旋轉器、塗布機等的適當的塗布方法,在基材(例如在半導體基板、玻璃基板、石英基板、矽晶圓及該等的表面形成有各種金屬膜或濾色器等的基板)上塗布本發明之樹脂組成物後,使用加熱板、烘箱等的加熱手段進行烘烤來使其硬化,來製作硬化膜、保護膜、或平坦化膜。烘烤條件可從烘烤溫度80℃至300℃、烘烤時間0.3分鐘至60分鐘之條件中來做適當選擇。前述烘烤亦可分成2階段以上來處理。又,作為所製作之硬化膜、保護膜或平坦化膜的膜厚,例如0.001μm至100μm,較佳為0.01μm至10μm。
<微透鏡之製作方法>
對於使用本發明之樹脂組成物之微透鏡之製作例來進行說明。藉由旋轉器、塗布機等的適當的塗布方法,在基材(例如在半導體基板、玻璃基板、石英基板、矽晶圓及該等的表面形成有各種金屬膜或濾色器等的基板)上塗布本發明之樹脂組成物後,使用加熱板、烘箱等的加熱手段進行烘烤並使其硬化,來製作硬化膜。烘烤條件可從烘烤溫度80℃至300℃、烘烤時間0.3分鐘至60分鐘之條件中來做適當選擇。前述烘烤亦可分成2階段以上來處理。又,作為所製作之硬化膜的膜厚,例如0.1μm至100μm,較佳為0.5μm至10μm。
之後,在所製作的硬化膜之上塗布阻劑,通過指定的遮罩進行曝光,因應所需進行曝光後加熱(PEB),藉由鹼液顯影、淋洗顯影液並進行乾燥,從而形成指定的阻劑圖型。曝光時可使用例如g線、i線、KrF準分子雷射、ArF準分子雷射。
接著,藉由加熱處理使前述阻劑圖型回焊來形成透鏡圖型。將該透鏡圖型作為蝕刻遮罩對下層的硬化膜進行回蝕刻並將該透鏡圖型的形狀轉印至該硬化膜。可經過以上之過程來製作微透鏡。
以下基於實施例及比較例更詳細地說明本發
明,但本發明並不被限定於該等實施例中。
裝置:日本分光(股)製GPC系統
管柱:Shodex〔註冊商標〕KF-804L及803L
管柱烘箱:40℃
流量:1mL/分
溶離液:四氫呋喃
<合成例1>
使苯乙烯300g、4-羥基苯基甲基丙烯酸酯205g、前述式(2-7)所表示之單體246g、及2,2’-偶氮二異丁腈47.0g,溶解在丙二醇單甲基醚976g後,將該溶液以4小時滴入至將丙二醇單甲基醚222g保持在70℃的燒瓶中。滴入結束後,進而使其反應18小時從而可得到共聚物的溶液(固形分濃度40質量%)。所得到之共聚物的重量平均分子量Mw為21,000(聚苯乙烯換算)。
<實施例1>
使合成例1所得到之(A)成分之自交聯性共聚物的溶液(固形分濃度40質量%)50.0g、(B)成分之前述式(3-10)所表示之化合物0.6g及作為界面活性劑之MEGAFACE〔註冊商標〕R-30(DIC(股)製)0.01g,溶
解在丙二醇單甲基醚乙酸酯3.6g及丙二醇單甲基醚14.4g中後製成溶液。之後,使用孔徑0.10μm的聚乙烯製微濾器進行過濾來調製樹脂組成物。
<實施例2>
除了使用作為(B)成分之前述式(3-10)所表示之化合物1.0g、丙二醇單甲基醚乙酸酯4.3g及丙二醇單甲基醚14.7g以外,以與上述實施例1相同的條件來調製樹脂組成物。
<實施例3>
除了使用作為(B)成分之前述式(3-8)所表示之化合物0.1g、丙二醇單甲基醚乙酸酯2.8g及丙二醇單甲基醚14.1g以外,以與上述實施例1相同的條件來調製樹脂組成物。
<實施例4>
除了使用作為(B)成分之前述式(3-6)所表示之化合物0.6g以外,以與上述實施例1相同的條件來調製樹脂組成物。
<比較例1>
使合成例1所得到之(A)成分之自交聯性共聚物的溶液(固形分濃度40質量%)50.0g、及作為界面活性劑
之MEGAFACE〔註冊商標〕R-30(DIC(股)製)0.01g,溶解在丙二醇單甲基醚乙酸酯2.7g及丙二醇單甲基醚14.0g中後製成溶液。之後,使用孔徑0.10μm的聚乙烯製微濾器用進行過濾來調製樹脂組成物。
<比較例2>
除了使用作為(B)成分之前述式(3-10)所表示之化合物1.6g、丙二醇單甲基醚乙酸酯5.3g及丙二醇單甲基醚15.1g以外,以與上述實施例1相同的條件來調製樹脂組成物。
將實施例1至實施例4以及比較例1及比較例2所調製的樹脂組成物,使用旋轉塗布機分別塗布在矽晶圓上,並在加熱板上以100℃進行1分鐘、進而以150℃進行10分鐘烘烤,形成膜厚4μm的硬化膜。對於該等之硬化膜,在丙二醇單甲基醚、丙二醇單甲基醚乙酸酯、乳酸乙酯、乙酸丁酯、3-甲氧基丙酸甲酯、丙酮、甲基異丁酮、2-庚酮、2-丙醇、N-甲基吡咯啶酮及2.38質量%濃度的水氫氧化四甲基銨(TMAH)水溶液中,分別進行以23℃的溫度條件下、浸漬10分鐘之試驗。進行浸漬前及浸漬後的膜厚測定,並算出在浸漬前後的膜厚變化。將前述浸漬溶劑之中即使是1種,對於浸漬前的膜厚有10%以上的膜厚增減之情形時設為“×”,將對於全部的溶劑之膜厚增
減都未滿10%之情形時設為“○”來評估耐藥品性。將評估結果表示於表1。
將實施例1至實施例4以及比較例1及比較例2所調製的樹脂組成物,使用旋轉塗布機分別塗布在石英基板上及矽晶圓上,在加熱板上以100℃進行1分鐘、進而以150℃進行10分鐘烘烤,形成膜厚4μm的硬化膜。對於在石英基板上所形成的該等之硬化膜,使用紫外線可見分光光度計UV-2550((股)島津製作所製),在波長400nm~800nm的範圍內使波長每次變化2nm並測定透射率。將所測定的透射率的最低值作為最低透射率並表示於表1。又,對於在矽晶圓上所形成的該等之硬化膜,使用光學顯微鏡以倍率100倍來觀察該硬化膜的表面,並確認沒有異物。進而,將在石英基板上及矽晶圓上所形成的該等之硬化膜,在烘箱內以150℃加熱1,000小時。之後,對於在石英基板上所形成的該等之硬化膜,再次在波長400nm~800nm的範圍內使波長每次變化2nm並測定透射率,將所測定的透射率的最低值作為最低透射率並表示於表1。又,對於在矽晶圓上所形成的該等之硬化膜,使用光學顯微鏡以倍率100倍來觀察該硬化膜的表面。將相對於1,000小時加熱前的最低透射率有5%以上的透射率降低之情形時設為“×”,透射率降低未滿5%之情形時設為“○”,於1,000小時加熱後,在硬化膜的表面有異物產
生之情形時設為“×”,沒有異物產生之情形時設為“○”來評估耐熱性。將評估結果表示於表1。
將實施例1至實施例4以及比較例1及比較例2所調製的樹脂組成物,使用旋轉塗布機分別塗布在石英基板及矽晶圓上,在加熱板上以100℃進行1分鐘、進而以150℃進行10分鐘烘烤,形成膜厚4μm的硬化膜。對於在石英基板上所形成的該等之硬化膜,使用紫外線可見分光光度計UV-2550((股)島津製作所製),在波長400nm~800nm的範圍內使波長每次變化2nm並測定透射率。將所測定的透射率的最低值作為最低透射率並表示於表1。又,對於在矽晶圓上所形成的該等之硬化膜,使用光學顯微鏡以倍率100倍來觀察該硬化膜的表面,並確認沒有異物。進而,將在石英基板上及矽晶圓上所形成的該等之硬化膜,在恆溫恆濕器內以85℃ 85%RH下靜置1,000小時。之後,對於在石英基板上所形成的該等之硬化膜,再次在波長400nm~800nm的範圍內使波長每次變化2nm並測定最低透射率,將所測定的透射率的最低值作為最低透射率並表示於表1。又,對於在矽晶圓上所形成的該等之硬化膜,使用光學顯微鏡以倍率100倍來觀察該硬化膜的表面。將相對於靜置1,000小時前的最低透射率有5%以上的透射率降低之情形時設為“×”、透射率降低未滿5%之情形時設為“○”,於靜置1,000小時後,在硬化膜
的表面有異物產生之情形時設為“×”、沒有異物產生之情形時設為“○”來評估耐熱耐濕性。將評估結果表示於表1。
從表1之結果可得知,由本發明之樹脂組成物所形成的硬化膜係具有高耐藥品性、高透明性之同時,即使是在以150℃加熱1,000小時後,及以85℃ 85%RH下靜置1,000小時後,不會著色且不會產生異物,係具有高耐熱性及高耐熱耐濕性。另一方面可得知,關於由比較例1及比較例2所調製的樹脂組成物所形成的硬化膜,結果將分別是比較例1為不滿足耐熱性、比較例2為不滿足耐熱耐濕性,故作為保護膜、平坦化膜及微透鏡用是不適合的。
Claims (11)
- 一種不含有醌二疊氮化合物之樹脂組成物,其係含有下述(A)成分、下述(B)成分、溶劑及界面活性劑之樹脂組成物,且不含有前述(A)成分、前述(B)成分、前述溶劑及前述界面活性劑以外的成分;基於前述樹脂組成物中除去前述溶劑後的全部成分之含有量,前述(B)成分之含有量為0.1質量%至5.0質量%;(A)成分:具有下述式(1)所表示之構造單位及下述式(2)所表示之構造單位之自交聯性共聚物,(B)成分:下述式(3)所表示之化合物,
- 如請求項1或請求項2之樹脂組成物,其中,前述自交聯性共聚物的重量平均分子量為1,000至100,000。
- 如請求項1或請求項2之樹脂組成物,其中,前述雜原子為氮原子、氧原子或硫原子。
- 如請求項1或請求項2之樹脂組成物,其係保護膜用。
- 如請求項1或請求項2之樹脂組成物,其係平坦化膜用。
- 如請求項1或請求項2之樹脂組成物,其係微透鏡用。
- 一種硬化膜之製作方法,其係包含將請求項1至請求項5中任一項之樹脂組成物塗布在基材上,並以80℃至300℃的溫度烘烤0.3分鐘至60分鐘之步驟。
- 一種微透鏡之製作方法,其係包含:在藉由請求項9之方法所製作的硬化膜上形成阻劑圖型之步驟、藉由加熱處理使前述阻劑圖型回焊來形成透鏡圖型之步驟、將前述透鏡圖型作為遮罩對前述硬化膜進行回蝕刻並將該透 鏡圖型的形狀轉印至該硬化膜之步驟。
- 如請求項10之微透鏡之製作方法,其中,前述基材為形成有濾色器的基板。
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