TWI691506B - 矽烷化劑藥液的調製方法及表面處理方法 - Google Patents
矽烷化劑藥液的調製方法及表面處理方法 Download PDFInfo
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- TWI691506B TWI691506B TW105106517A TW105106517A TWI691506B TW I691506 B TWI691506 B TW I691506B TW 105106517 A TW105106517 A TW 105106517A TW 105106517 A TW105106517 A TW 105106517A TW I691506 B TWI691506 B TW I691506B
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- silanizing agent
- chemical solution
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- 238000004381 surface treatment Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 9
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 49
- 239000002184 metal Substances 0.000 claims abstract description 48
- 239000003960 organic solvent Substances 0.000 claims abstract description 48
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- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 3
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- VKPSKYDESGTTFR-UHFFFAOYSA-N 2,2,4,6,6-pentamethylheptane Chemical compound CC(C)(C)CC(C)CC(C)(C)C VKPSKYDESGTTFR-UHFFFAOYSA-N 0.000 description 2
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- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
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- 125000004344 phenylpropyl group Chemical group 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- 238000004321 preservation Methods 0.000 description 1
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- 229960000380 propiolactone Drugs 0.000 description 1
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- 238000002444 silanisation Methods 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- BCNZYOJHNLTNEZ-UHFFFAOYSA-N tert-butyldimethylsilyl chloride Chemical compound CC(C)(C)[Si](C)(C)Cl BCNZYOJHNLTNEZ-UHFFFAOYSA-N 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
- BRNULMACUQOKMR-UHFFFAOYSA-N thiomorpholine Chemical compound C1CSCCN1 BRNULMACUQOKMR-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
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- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
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- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- QVSRWXFOZLIWJS-UHFFFAOYSA-N trimethylsilyl propanoate Chemical compound CCC(=O)O[Si](C)(C)C QVSRWXFOZLIWJS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
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Abstract
本發明為提供調製減低金屬雜質濃度的矽烷化劑藥液之方法、及使用藉由如此調製方法所得之矽烷化劑藥液的表面處理方法。
本發明係關於含有使用預先使其與有機溶劑接觸的離子交換樹脂膜,減低處理前矽烷化劑藥液中之金屬雜質的步驟之矽烷化劑藥液的調製方法。於基板表面上,使藉由上述矽烷化劑藥液之調製方法所得之矽烷化劑藥液進行暴露,使上述基板表面進行疏水化的表面處理方法。
Description
本發明係關於矽烷化劑藥液之調製方法及表面處理方法。
近年來,半導體裝置的高集積化、微細化傾向之提高,圖型的微細化.高縱橫比化正進展著。然而另一方面,產生所謂的圖型倒落之問題。該圖型倒落為於基板上並列多數圖型而形成時,使鄰接圖型彼此以互相傾斜方式接近,視情況而使圖型自基部進行折損之現象。若產生如此圖型倒落時,因無法獲得所望製品,會引起製品的產率或信賴性降低之情況。
此所謂的「圖型」為,含有在半導體之製造步驟的光刻步驟(曝光.現像步驟)於基板上所形成的「抗蝕圖型」與在光刻步驟後之基板的蝕刻步驟所形成的「無機圖型」之雙方。有關本發明之基板表面的改質方法為這些圖型之中,於「無機圖型」的處理更有效果。
已知該圖型倒落係在對於藉由圖型形成後的純水等進行沖洗(Rinse)處理中,乾燥沖洗液時,會藉
由該沖洗液之表面張力而產生。換言之,於乾燥過程中除去沖洗液時,於圖型間依據沖洗液的表面張力之應力會起作用而產生圖型倒落。
因此,僅可將圖型表面經疏水化後,提高沖洗液之接觸角時,在沖洗後之乾燥過程中可減低於圖型間之作用力,進而可防止圖型倒落。又,圖型之縱橫比越大其於圖型間的作用力亦越大,故藉由疏水化之圖型倒落的抑制效果亦有變大的傾向。
其中,將矽烷化劑藥液經暴露後,使基板表面進行撥水化或疏水化的表面處理(例如專利文獻1)。
[專利文獻1]日本特開2010-114414號公報
矽烷化劑藥液與使用於洗淨晶圓的洗淨液同樣地,期待有增大裝置接合漏電流的顧慮之金屬雜質較少且乾淨者。然而,因亦存在藉由加熱容易變質的矽烷化劑藥液或具有水解性的矽烷化劑藥液,故有時無法使該藥液進行蒸餾純化。
本發明為有鑑於上述課題所成者,以提供調製金屬雜質濃度經減低的矽烷化劑藥液之方法、及使用藉
由如此調製方法所得之矽烷化劑藥液的表面處理方法為目的。
本發明之第一態樣為含有使用預先將使其與有機溶劑接觸的離子交換樹脂膜而減低處理前矽烷化劑藥液中之金屬雜質的步驟之矽烷化劑藥液的調製方法。
本發明之第二態樣為在基板表面上暴露藉由本發明之第一態樣的矽烷化劑藥液之調製方法所得的矽烷化劑藥液,使該基板表面進行疏水化的表面處理方法。
依據本發明,可提供調製減低金屬雜質濃度之矽烷化劑藥液的方法、及使用藉由如此調製方法所得的矽烷化劑藥液之表面處理方法。
[實施發明的形態]
≪矽烷化劑藥液之調製方法≫
本實施態樣之矽烷化劑藥液的調製方法為含有使用預先將使其與有機溶劑接觸的離子交換樹脂膜而減低處理前矽烷化劑藥液中之金屬雜質的步驟(以下有時稱為「金屬雜質減低步驟」)。金屬雜質減低步驟具體為含有於使處
理前矽烷化劑藥液透過預先與有機溶劑接觸的離子交換樹脂膜,更具體為含有(1)預先將離子交換樹脂膜接觸有機溶劑的步驟及(2)使處理前矽烷化劑藥液透過離子交換樹脂膜之步驟。
對於本說明書所謂「處理前矽烷化劑藥液」表示透過預先與有機溶劑接觸的離子交換樹脂膜之前的藥液。處理前矽烷化劑藥液為含有矽烷化劑及金屬雜質之液體,例如可為進一步含有有機溶劑的液體,但通常為無須含有有機溶劑之液體,例如亦可為除雜質以外僅含有矽烷化劑之液體,亦可為僅含有矽烷化劑及金屬雜質之液體。
[離子交換樹脂膜]
作為本實施態樣中所使用的離子交換樹脂膜,雖無特別限定,可使用將適當離子交換基固定於樹脂膜,含有離子交換樹脂之濾器,例如可舉出於高密度聚乙烯膜上將磺酸基等陽離子交換基經化學修飾的強酸性陽離子交換樹脂等離子交換樹脂膜等以外,亦可舉出於多孔質之高密度聚乙烯媒介物的細孔表面以化學性地導入強酸性陽離子交換樹脂,除粒子膜與離子交換樹脂膜成為一體結構的除粒子膜付離子交換樹脂膜等,以離子交換基經化學性修飾的聚伸烷基膜為佳。作為聚伸烷基,例如可舉出聚乙烯、聚丙烯等,以聚丙烯為佳。作為離子交換基,以陽離子交換基為佳。作為在本實施態樣所使用的離子交換樹脂膜,可使用作為金屬離子除去用濾器的市售品。
對於本實施態樣的矽烷化劑藥液之調製方法,離子交換樹脂膜為預先與有機溶劑接觸。離子交換樹脂膜係為乾燥狀態之市售品,又雖有與水溶液之親和性優良的親水性之素材,但依據本實施態樣,即使在使用如此離子交換樹脂膜之情況下,藉由預先與有機溶劑接觸,可有效果地減低處理前矽烷化劑藥液中之金屬雜質,該減低效果與未將離子交換樹脂膜預先與有機溶劑接觸的情況相比,有者顯著優異性。
[有機溶劑]
對於本實施態樣,作為預先與離子交換樹脂膜接觸的有機溶劑,以不具有與矽烷化劑進行反應的官能基之有機溶劑為佳。有機溶劑可單獨使用1種,亦可混合2種以上使用。
對於本實施態樣中,作為預先與離子交換樹脂膜接觸的較佳有機溶劑,具體可舉出二甲基亞碸等亞碸類;二甲基碸、二乙基碸、雙(2-羥基乙基)碸、四伸甲基碸等碸類;N,N-二甲基甲醯胺、N-甲基甲醯胺、N,N-二甲基乙醯胺、N-甲基乙醯胺、N,N-二乙基乙醯胺等醯胺類、N-甲基-2-吡咯啶酮、N-乙基-2-吡咯啶酮、N-丙基-2-吡咯啶酮、N-羥基甲基-2-吡咯啶酮、N-羥基乙基-2-吡咯啶酮等內醯胺類;1,3-二甲基-2-咪唑啉酮、1,3-二乙基-2-咪唑啉酮、1,3-二異丙基-2-咪唑啉酮等咪唑啉酮類;二甲基甘醇、二甲基二甘醇、二甲基三甘醇、甲基乙基二甘
醇、二乙基甘醇等二烷基甘醇醚類;乙二醇單甲基醚、乙二醇單乙基醚、乙二醇單-n-丙基醚、乙二醇單-n-丁基醚、二乙二醇單甲基醚、二乙二醇單乙基醚、二乙二醇單-n-丙基醚、二乙二醇單-n-丁基醚、三乙二醇單甲基醚、三乙二醇單乙基醚、丙二醇單甲基醚、丙二醇單乙基醚、丙二醇單-n-丙基醚、丙二醇單-n-丁基醚、二丙二醇單甲基醚、二丙二醇單乙基醚、二丙二醇單-n-丙基醚、二丙二醇單-n-丁基醚、三丙二醇單甲基醚、三丙二醇單乙基醚等(聚)烷二醇單烷基醚類;乙二醇單甲基醚乙酸酯、乙二醇單乙基醚乙酸酯、二乙二醇單甲基醚乙酸酯、二乙二醇單乙基醚乙酸酯、丙二醇單甲基醚乙酸酯、丙二醇單乙基醚乙酸酯等(聚)烷二醇單烷基醚乙酸酯類;二甲基醚、二乙基醚、甲基乙基醚、二丙基醚、二異丙基醚、二丁基醚、二異戊基醚、二乙二醇二甲基醚、二乙二醇甲基乙基醚、二乙二醇二乙基醚、四氫呋喃等其他醚類;甲基乙基酮、環己酮、2-庚酮、3-庚酮等酮類;2-羥基丙酸甲酯、2-羥基丙酸乙酯等乳酸烷基酯類;2-羥基-2-甲基丙酸乙酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸甲酯、3-乙氧基丙酸乙酯、乙氧基乙酸乙酯、羥基乙酸乙酯、2-羥基-3-甲基丁烷酸甲酯、3-甲基-3-甲氧基丁基乙酸酯、3-甲基-3-甲氧基丁基丙酸酯、乙酸乙酯、乙酸-n-丙酯、乙酸-i-丙酯、乙酸-n-丁酯、乙酸-i-丁酯、蟻酸-n-戊酯、乙酸-i-戊酯、丙酸-n-丁酯、丁酸乙酯、丁酸-n-丙酯、丁酸-i-丙酯、丁酸-n-丁酯、丙酮酸甲酯、丙酮酸
乙酯、丙酮酸-n-丙酯、乙醯乙酸甲酯、乙醯乙酸乙酯、2-氧代丁烷酸乙酯等其他酯類;β-丙內酯、γ-丁內酯、δ-戊內酯等內酯類;n-己烷、n-庚烷、n-辛烷、n-壬烷、甲基辛烷、n-癸烷、n-十一烷、n-十二烷、2,2,4,6,6-五甲基庚烷、2,2,4,4,6,8,8-七甲基壬烷、環己烷、甲基環己烷等直鏈狀、支鏈狀或環狀烴類;苯、甲苯、萘、1,3,5-三甲基苯等芳香族烴類;p-薄荷烷、二苯基薄荷烷、檸檬烯、松油烯、莰烷、降冰片烷、Pinang等萜烯類等。這些溶劑可單獨或混合2種以上使用。其中亦以丙二醇單甲基醚乙酸酯(PEMEA);直鏈狀、分支鏈狀或環狀之烴類;p-薄荷烷、二苯基薄荷烷、檸檬烯、松油烯、莰烷、降冰片烷、Pinang等萜烯類為佳。
[預先將離子交換樹脂膜與有機溶劑接觸之步驟]
對於本實施態樣中之金屬雜質減低步驟,具體為使處理前矽烷化劑藥液透過之前,預先將離子交換樹脂膜與有機溶劑接觸。
作為將離子交換樹脂膜與有機溶劑接觸的方法,並無特別限定,例如可舉出使有機溶劑透過離子交換樹脂膜之方法、於有機溶劑含浸離子交換樹脂膜的方法等,一邊於有機溶劑含浸離子交換樹脂膜,一邊將該有機溶劑徐徐少量地透過離子交換樹脂膜的方法為佳,具體為藉由於設置離子交換樹脂膜的過濾裝置中使有機溶劑液體通過而進行,此時藉由將離子交換樹脂膜含浸於有機溶劑程度的量
之有機溶劑投入於離子交換樹脂膜上,一邊於有機溶劑含浸離子交換樹脂膜一邊可將該有機溶劑徐徐少量地透過離子交換樹脂膜。
離子交換樹脂膜與有機溶劑之接觸,例如可進行1分鐘以上,較佳為10分鐘以上,更佳為20分鐘以上,作為接觸時間之上限值並無特別限定,但由製造效率之觀點來看,例如以2小時以下,較佳為1小時以下,更佳為40分鐘以下。
本實施態樣之矽烷化劑藥液的調製方法為藉由預先將離子交換樹脂膜與有機溶劑接觸,可提高離子交換樹脂膜之濕潤性,故在後步驟可容易地使欲透過的處理前矽烷化劑藥液到達存在於離子交換樹脂膜內部的孔,可顯著地減低於處理前矽烷化劑藥液所含有的金屬雜質之濃度以外,離子交換樹脂膜中即使含有水分,亦可除去該水分。
因矽烷化劑一般容易與水分進行反應而聚合,故預先減低反應步驟中之水分為佳。因此,於將離子交換樹脂膜與有機溶劑進行接觸之前進行氮氣淨化,於進行氮氣淨化的手套箱等封閉環境下將離子交換樹脂膜與有機溶劑接觸者為佳。
[於使處理前矽烷化劑藥液透過離子交換樹脂膜之步驟]
對於本實施態樣,如上述預先將離子交換樹脂膜與有
機溶劑接觸後,使處理前矽烷化劑藥液透過該離子交換樹脂膜。作為該透過方法並無特別限定,例如可於設置該離子交換樹脂膜的過濾裝置上通過處理前矽烷化劑藥液而進行,由製造效率之觀點來看,亦可將預先將離子交換樹脂膜與有機溶劑接觸的步驟如上述使用過濾裝置而進行後,接著可使用相同過濾裝置而進行。
作為預先將離子交換樹脂膜與有機溶劑接觸後,使處理前矽烷化劑藥液透過該離子交換樹脂膜之條件,並無特別限定,作為流速,例如10~400ml/分鐘,較佳為100~300ml/分鐘,更佳為150~250ml/分鐘之條件下進行。
[處理前矽烷化劑藥液]
對於本實施態樣所使用的處理前矽烷化劑藥液,如上述至少含有矽烷化劑及金屬雜質之液體。對於本說明書中之「處理前矽烷化劑藥液」為欲與在本實施態樣中之金屬雜質減低步驟中,透過上述離子交換樹脂膜後之從離子交換樹脂膜流出的處理後之矽烷化劑藥液(本說明書中,有時稱為「經處理之矽烷化劑藥液」。)做區別而使用的用語。當然對於處理前矽烷化劑藥液與經處理之矽烷化劑藥液所含有的矽烷化劑可為相同。
[矽烷化劑]
矽烷化劑的種類僅為可使基板表面性質疏水化者即
可,並無特別限定,可使用適宜地選自自過去使用於種種材料的撥水化或疏水化的矽烷化劑。本說明書中所謂「疏水化」為含有撥水化之概念。以下對於可使用在本實施態樣之矽烷化劑做說明。
使用於基板表面之疏水化的矽烷化劑,僅可對於基板表面得到所望疏水化效果者即可並無特別限定,可使用適宜地選自自過去作為種種材料的疏水化劑使用之矽烷化劑。
含於矽烷化劑藥液之矽烷化劑,例如可為下述一般式(1)所示矽化合物。
(R1)aSi(H)bX1 4-a-b (1)
(式中,R1各彼此獨立表示含有一部分或全部的氫原子可由氟原子所取代之碳數1~18的1價烴基的1價有機基,X1各彼此獨立表示與矽原子鍵結的原子為氮的1價官能基,a為1~3的整數,b為0~2的整數,a與b之合計為1~3)
作為較佳矽烷化劑,可舉出以下一般式(3)~(10)所示矽烷化劑或環狀矽氮烷化合物。以下以一般式(3)~(10)所示矽烷化劑與環狀矽氮烷化合物之順序作說明。
(一般式(3)所示矽烷化劑)
一般式(3)中,R1、R2及R3各獨立表示氫原子、鹵素原子或有機基。R1、R2及R3的碳數之合計為1以上。R4表示氫原子或飽和或不飽和的鏈狀烴基。R5表示氫原子、飽和或不飽和的鏈狀烴基、飽和或不飽和的非芳香族環狀烴基或非芳香族雜環基。R4及R5彼此鍵結可形成具有氮原子的非芳香族雜環。
R1、R2及R3若為鹵素原子時,以氯原子、溴原子、碘原子及氟原子為佳。
R1、R2及R3為有機基時,有機基除碳原子以外可含有雜原子。有機基可含有的雜原子種類若不阻礙本發明之目的的範圍下並無特別限定。作為可含於有機基之雜原子,以N、O、及S為佳。R1、R2及R3為有機基時,含於有機基的碳原子數與雜原子的數之合計若為R1、R2及R3的碳數合計為1以上時並無特別限定。R1、R2及R3為有機基時,含於有機基的碳原子數與雜原子數的合計以1~10為佳,以1~8為較佳,以1~3為特佳。R1、R2及R3若為有機基時,作為有機基,以飽和或不飽和的鏈狀烴基、芳烷基、及芳香族烴基為佳。作為飽和或不飽和的鏈狀烴基的較佳例子,可舉出甲基、乙基、乙烯基、n-丙基、異丙基、烯丙基、1-丙烯基、異丙烯基、n-丁基、sec-丁基、tert-丁基、3-丁烯基、n-戊基、異戊
基、sec-戊基、tert-戊基、n-己基、n-庚基、n-辛基、n-壬基、及n-癸基等。這些鏈狀烴基之中,以甲基、乙基、乙烯基、n-丙基、及烯丙基為較佳,以甲基、乙基、及乙烯基為特佳。作為芳烷基的較佳例子,可舉出苯甲基、苯基乙基、苯基丙基、α-萘甲基、及β-萘甲基。作為芳香族烴基的較佳例子,可舉出苯基、α-萘基、及β-萘基。
R4為飽和或不飽和的鏈狀烴基時,飽和或不飽和的鏈狀烴基的碳數以不妨礙本發明之目的的範圍下,並無特別限定。R4為飽和或不飽和的鏈狀烴基時,飽和或不飽和的鏈狀烴基的碳數以1~10為佳,以1~8為較佳,以1~3為特佳。R4為飽和或不飽和的鏈狀烴基時的較佳例子,與對於R1、R2及R3之較佳基所舉出的飽和或不飽和的鏈狀烴基相同。
R5為飽和或不飽和的鏈狀烴基時,飽和或不飽和的鏈狀烴基與R4相同。R5為飽和或不飽和的環狀烴基時,飽和或不飽和的環狀烴基之碳數以不妨礙本發明之目的的範圍下並無特別限定。R5為飽和或不飽和的非芳香族環狀烴基時,飽和或不飽和的非芳香族環狀烴基的碳數以3~10為佳,以3~6為較佳,以5或6為特佳。作為R5為飽和或環狀烴基時的較佳例子,可舉出環丙基、環丁基、環戊基、環己基、環戊基、及環辛基。R5為非芳香族雜環基時,於非芳香族雜環基所含的雜原子以不妨礙本發明之目的的範圍下並無特別限定。R5為非芳香族雜環基時,作為含於非芳香族雜環基的較佳雜原子,可舉出N、
O、及S。R5為非芳香族雜環基時,含於非芳香族雜環基的碳原子數與雜原子數之合計以不妨礙本發明之目的的範圍下並無特別限定。R5為非芳香族雜環基時,含於非芳香族雜環基的碳原子數與雜原子數的合計以3~10為佳,以3~6為較佳,以5或6為特佳。作為R5為非芳香族雜環基時的較佳例子,可舉出吡咯烷-1-基、哌啶-1-基、哌嗪-1-基、嗎啉-1-基、及硫代嗎啉-1-基。
R4及R5彼此鍵結所形成的非芳香族雜環基中所含的原子數以不妨礙本發明之目的的範圍下並無特別限定。R4及R5彼此鍵結所形成的非芳香族雜環基以3員環至10員環為佳,以5員環或6員環為較佳。R4及R5彼此鍵結所形成的非芳香族雜環基中所含的碳原子以外之雜原子種類,以不妨礙本發明之目的的範圍下並無特別限定。作為R4及R5彼此鍵結所形成的非芳香族雜環基中所含的較佳雜原子,可舉出N、O、及S。作為R4及R5彼此鍵結所形成的非芳香族雜環的較佳例子,可舉出吡咯烷、哌啶、哌嗪、嗎啉、及硫代嗎啉。
作為一般式(3)所示矽烷化劑的具體例子,可舉出N,N-二甲基胺基三甲基矽烷、N,N-二甲基胺基二甲基矽烷、N,N-二甲基胺基單甲基矽烷、N,N-二乙基胺基三甲基矽烷、t-丁基胺基三甲基矽烷、烯丙基胺基三甲基矽烷、三甲基矽基乙醯胺、N,N-二甲基胺基二甲基乙烯基矽烷、N,N-二甲基胺基二甲基丙基矽烷、N,N-二甲基胺基二甲基辛基矽烷、N,N-二甲基胺基二甲基苯基乙基矽烷、
N,N-二甲基胺基二甲基苯基矽烷、N,N-二甲基胺基二甲基-t-丁基矽烷、N,N-二甲基胺基三乙基矽烷、及三甲基矽烷胺等。
(一般式(4)所示矽烷化劑)
一般式(4)中,R1、R2及R3與上述一般式(3)相同。R6表示氫原子、甲基、三甲基矽基或二甲基矽基。R7、R8及R9各獨立表示氫原子或有機基。R7、R8及R9的碳數合計為1以上。
R7、R8、及R9為有機基時,有機基與R1、R2及R3為有機基時的有機基相同。
作為一般式(4)所示矽烷化劑的具體例子,可舉出六甲基二矽氮烷、N-甲基六甲基二矽氮烷、1,1,3,3-四甲基二矽氮烷、1,3-二甲基二矽氮烷、1,3-二-n-辛基-1,1,3,3-四甲基二矽氮烷、1,3-二乙烯基-1,1,3,3,-四甲基二矽氮烷、參(二甲基矽基)胺、參(三甲基矽基)胺、1-乙基-1,1,3,3,3-五甲基二矽氮烷、1-乙烯基-1,1,3,3,3-五甲基二矽氮烷、1-丙基-1,1,3,3,3-五甲基二矽氮烷、1-苯基乙基-1,1,3,3,3-五甲基二矽氮烷、1-tert-丁基-1,1,3,3,3-五甲基二矽氮烷、1-苯基-1,1,3,3,3-五甲基二矽氮烷、及1,1,1-三甲基-3,3,3-三乙基二矽氮烷等。
(一般式(5)所示矽烷化劑)
一般式(5)中,R1、R2及R3與上述一般式(3)相同。Y表示O、CHR11、CHOR11、CR11R11或NR12。R10及R11各獨立表示氫原子、飽和或不飽和的鏈狀烴基、飽和或不飽和的非芳香族環狀烴基、三烷基矽基、三烷基矽氧基、烷氧基、苯基、苯基乙基或乙醯基。R12表示氫原子、烷基或三烷基矽基。
R10及R11為飽和或不飽和的鏈狀烴基或飽和或不飽和的非芳香族環狀烴基時,飽和或不飽和的鏈狀烴基與飽和或不飽和的非芳香族環狀烴基與一般式(3)中之R5為飽和或不飽和的鏈狀烴基,或飽和或不飽和的非芳香族環狀烴基時相同。
R10及R11為三烷基矽基、三烷基矽氧基或烷氧基時,這些基所含的烷基的碳數以不阻礙本發明之目的的範圍下並無特別限定。這些基所含的烷基之碳數以1~10為佳,以1~8為較佳,以1~3為特佳。作為這些基所含的烷基之較佳例子,可舉出甲基、乙基、n-丙基、異丙基、n-丁基、sec-丁基、tert-丁基、n-戊基、異戊基、sec-戊基、tert-戊基、n-己基、n-庚基、n-辛基、n-壬基、及n-癸基等。這些烷基之中以甲基、乙基、及n-丙基為
較佳,以甲基及乙基為特佳。
R12為烷基或三烷基矽基時,含於烷基或三烷基矽基的烷基之碳數以不阻礙本發明之目的的範圍下並無特別限定。含於烷基或三烷基矽基的烷基之碳數以1~10為佳,以1~8為較佳,以1~3為特佳。作為含於烷基或三烷基矽基的烷基之較佳例子,可舉出甲基、乙基、n-丙基、異丙基、n-丁基、sec-丁基、tert-丁基、n-戊基、異戊基、sec-戊基、tert-戊基、n-己基、n-庚基、n-辛基、n-壬基、及n-癸基等。這些烷基之中以甲基、乙基、及n-丙基為較佳,以甲基及乙基為特佳。
作為一般式(5)所示矽烷化劑的具體例子,可舉出三甲基矽基乙酸酯、二甲基矽基乙酸酯、單甲基矽基乙酸酯、三甲基矽基丙酸酯、三甲基矽基丁酸酯、及三甲基矽基-2-丁酸酯等。
(一般式(6)所示矽烷化劑)
一般式(6)中,R1、R2及R3與上述一般式(3)相同。R6與上述一般式(4)相同。R13表示氫原子、飽和或不飽和的鏈狀烴基、三氟甲基或三烷基矽基胺基。
R13為飽和或不飽和的鏈狀烴基時,飽和或不
飽和的鏈狀烴基與一般式(3)中之R4為飽和或不飽和的鏈狀烴基時相同。
R13為三烷基矽基胺基時,含於三烷基矽基胺基之烷基與一般式(5)中之R10及R11為三烷基矽基、三烷基矽氧基或烷氧基時,含於這些基的烷基相同。
作為一般式(6)所示矽烷化劑的具體例子,可舉出N,N’-雙(三甲基矽基)尿素、N-三甲基矽基乙醯胺、N-甲基-N-三甲基矽基三氟乙醯胺、及N,N-雙(三甲基矽基)三氟乙醯胺等。
(一般式(7)所示矽烷化劑)
一般式(7)中,R14表示三烷基矽基。R15及R16各獨立表示氫原子或有機基。
R14為三烷基矽基時,含於三烷基矽基的烷基與一般式(5)中之R10及R11為三烷基矽基、三烷基矽氧基或烷氧基時,含於這些基的烷基相同。
R15及R16為有機基時,有機基與一般式(3)中之R1、R2及R3為有機基時的有機基相同。
作為一般式(7)所示矽烷化劑的具體例子,可舉出2-三甲基矽氧基戊烷-2-烯-4-酮等。
(一般式(8)所示矽烷化劑)
一般式(8)中,R1、R2及R3與上述一般式(3)相同。R17表示飽和或不飽和的鏈狀烴基、飽和或不飽和的非芳香族環狀烴基或非芳香族雜環基。R18表示-SiR1R2R3。P為0或1。
P為0時,作為R17的飽和或不飽和的鏈狀烴基、飽和或不飽和之非芳香族環狀烴基或非芳香族雜環基與一般式(3)中之R5相同。P為1時,作為R17的有機基為自一般式(3)中之R1、R2及R3為有機基時的有機基除去1個氫原子之2價基。
作為一般式(8)所示矽烷化劑的具體例子,可舉出1,2-雙(二甲基氯矽基)乙烷、及t-丁基二甲基氯矽烷等。
(一般式(9)所示矽烷化劑)
R19 qSi[N(CH3)2]4-q...(9)
一般式(9)中,R19各獨立為氫原子的一部分或全部可由氟原子所取代之碳數1~18的鏈狀烴基。q為1或2。
一般式(9)中,R19的碳數以2~18為佳,以8~18為較佳。
作為R19未由氟原子所取代之鏈狀飽和烴基時的例子,可舉出甲基、乙基、n-丙基、異丙基、丁基、sec-丁基、tert-丁基、異丁基、戊基、異戊基、tert-戊基、己基、2-己基、3-己基、庚基、2-庚基、3-庚基、異庚基、tert-庚基、n-辛基、異辛基、tert-辛基、2-乙基己基、壬基、異壬基、癸基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、及十八烷基等。
作為R19未由氟原子所取代的鏈狀不飽和烴基時的例子,可舉出乙烯基、1-丙烯基、烯丙基、異丙烯基、1-丁烯基、2-丁烯基、3-丁烯基、1,3-丁二烯基、1-乙基乙烯基、1-甲基-1-丙烯基、1-甲基-2-丙烯基、4-戊烯基、1,3-戊二烯基、2,4-戊二烯基、3-甲基-1-丁烯基、5-己烯基、2,4-伸己二烯基、6-庚烯基、7-辛烯基、8-壬烯基、9-癸烯基、10-十一烯基、11-十二烯基、12-十三烯基、13-十四烯基、14-十五烯基、15-十六烯基、16-十七烯基、17-十八烯基、乙炔基、炔丙基、1-丙炔基、1-丁炔基、2-丁炔基、3-丁炔基、1-戊炔基、2-戊炔基、3-戊炔基、4-戊炔基、1-己炔基、2-己炔基、3-己炔基、4-己炔基、5-己炔基、6-庚炔基、7-辛炔基、8-壬炔基、9-癸炔基、10-十一炔基、11-十二炔基、12-十三炔基、13-十四炔基、14-十五炔基、15-十六炔基、16-十七炔基、及17-十八炔基等。
R19為由氟原子所取代之鏈狀烴基時,氟原子之取代數、及取代位置並無特別限定。鏈狀烴基中之氟原
子的取代數以鏈狀烴基所具有的氫原子數之50%以上為佳,以70%以上為較佳,以80%以上為特佳。
作為R19,由可容易得到優良疏水化之效果的觀點來看,氫原子的一部分或全部可由氟原子所取代,以碳數1~18的直鏈烴基為佳。又,作為R19由矽烷化劑之保存安定性的觀點來看,氫原子的一部分或全部可由氟原子所取代,以碳數1~18的直鏈飽和烴基(碳數1~18的烷基)為較佳。
一般式(9)中,q為1或2,以1為佳。
(一般式(10)所示矽烷化劑)
R20 r[N(CH3)2]3-rSi-R22-SiR21 s[N(CH3)2]3-s...(1
0)
一般式(10)中,R20及R21各獨立為氫原子或碳數1~4的直鏈或分支鏈烷基。R22為碳數1~16的直鏈或分支鏈伸烷基。r及s各獨立為0~2的整數。
R20及R21為各可相同或相異。作為R20及R21,以氫原子或碳數1~3的直鏈或分支鏈烷基為佳,以氫原子或甲基為較佳,以甲基為特佳。
作為R20及R21為碳數1~4的直鏈或分支鏈烷基時的具體例子,可舉出甲基、乙基、n-丙基、異丙基、n-丁基、sec-丁基、tert-丁基、及異丁基。
一般式(10)所示化合物含有R22為碳數1~16的直鏈或分支鏈伸烷基。R22為直鏈或分支鏈伸烷基的碳數以1~10為佳,以2~8為較佳。且,所謂直鏈伸烷
基為伸甲基或α,ω-直鏈伸烷基,分支鏈伸烷基為伸甲基、及α,ω-直鏈伸烷基以外之伸烷基。R22以直鏈伸烷基者為佳。
作為R22為碳數1~16的直鏈或分支鏈伸烷基時的例子,可舉出伸甲基、1,2-伸乙基、1,1-伸乙基、丙烷-1,3-二基、丙烷-1,2-二基、丙烷-1,1-二基、丙烷-2,2-二基、丁烷-1,4-二基、丁烷-1,3-二基、丁烷-1,2-二基、丁烷-1,1-二基、丁烷-2,2-二基、丁烷-2,3-二基、戊烷-1,5-二基、戊烷-1,4-二基、己烷-1,6-二基、庚烷-1,7-二基、辛烷-1,8-二基、2-乙基己烷-1,6-二基、壬烷基-1,9-二基、癸烷-1,10-二基、十一烷-1,11-二基、十二烷-1,12-二基、十三烷-1,13-二基、十四烷-1,14-二基、十五烷-1,15-二基、及十六烷-1,16-二基等。
對於一般式(10)所示化合物,s及r各獨立為0~2的整數。對於式(10)所示化合物,由合成及獲得之容易性來看,s及r以1或2者為佳,以2為較佳。
(環狀矽氮烷化合物)
作為矽烷化劑,以環狀矽氮烷化合物亦佳。以下對於環狀矽氮烷化合物做說明。
作為環狀矽氮烷化合物,可舉出2,2,5,5-四甲基-2,5-矽雜-1-氮雜環戊烷、2,2,6,6-四甲基-2,6-矽雜-1-氮雜環己烷等環狀二矽氮烷化合物;2,2,4,4,6,6-六甲基環三矽氮烷、2,4,6-三甲基-2,4,6-三乙烯基環三矽氮烷等環狀
三矽氮烷化合物;2,2,4,4,6,6,8,8-八甲基環四矽氮烷等環狀四矽氮烷化合物等。
彼等中亦以環狀二矽氮烷化合物為佳,以2,2,5,5-四甲基-2,5-矽雜-1-氮雜環戊烷及2,2,6,6-四甲基-2,6-矽雜-1-氮雜環己烷為較佳。作為環狀二矽氮烷化合物,雖有如2,2,5,5-四甲基-2,5-矽雜-1-氮雜環戊烷之5員環結構或如2,2,6,6-四甲基-2,6-矽雜-1-氮雜環己烷的6員環結構,但以5員環結構為佳。
[金屬雜質]
作為於本實施態樣所使用的處理前矽烷化劑藥液中所含有的金屬雜質,並無特別限定,例如可舉出含有選自由周期律表的第4族、第5族、第6族、第7族、第8族、第9族及第10族所成群的至少1種金屬元素的金屬雜質等。作為該金屬元素,其中亦以選自由Fe、Cu、Al、Zn、Co、Li、Na、K、Ca、Cr、Mn、Pb、Ni、Ru、Rh、Pd、Re、Os、Ir、Pt、W及Mo所成群的至少1種金屬元素為佳,其中特別由從藉由本實施態樣的矽烷化劑藥液之調製方法進行處理前矽烷化劑藥液中容易除去者的觀點來看,以選自由Fe、Cu、Al及Zn所成群的至少1種金屬元素為較佳。這些金屬雜質可由金屬元素所成的單體。本說明書中所謂「含有金屬元素」的意思表示可由該金屬元素所成的單體,亦可具有該金屬元素之金屬化合物。此對於「金屬元素」為例如「Al元素」等具體金屬元素而言
亦為相同。
[其他成分]
本實施態樣中所使用的處理前矽烷化劑藥液以不妨礙本發明之目的的範圍下,可含有上述矽烷化劑及金屬雜質以外的其他成分。
作為其他成分並無特別限定,例如可舉出有機溶劑等,雖在矽烷化劑非液體時含有有機溶劑者為佳,但僅可在基板表面暴露矽烷化劑者即可,可不含有有機溶劑。含有有機溶劑時,當然可與處理前矽烷化劑藥液與經處理之矽烷化劑藥液中所含有的有機溶劑相同。
作為可含於處理前矽烷化劑藥液之有機溶劑,雖無特別限定,但對於本實施態樣,以預先與離子交換樹脂膜接觸的有機溶劑同種之有機溶劑者為佳。
[經處理之矽烷化劑藥液]
本實施態樣中,藉由上述金屬雜質減低步驟所得之矽烷化劑藥液(經處理之矽烷化劑藥液)為含於處理前矽烷化劑藥液的金屬雜質之濃度被減低者。
藉由本實施態樣之矽烷化劑藥液的調製方法所得之矽烷化劑藥液(經處理之矽烷化劑藥液)因如上述其金屬雜質濃度已被減低,故可適合作為基板表面處理液使用,特別適合作為半導體裝置等製造之基板表面處理液使用。
≪表面處理方法≫
將藉由本發明之第一態樣之矽烷化劑藥液的調製方法所得的矽烷化劑藥液暴露在基板表面,將該基板表面進行疏水化的表面處理方法亦為本發明之一。對於該表面處理方法,矽烷化劑藥液可作為上述基板表面處理液使用。
基板的材質並無特別限定,可選自種種無機基板及有機基板,可依據所使用的矽烷化劑種類而決定。基板表面雖無特別限定,例如可藉由過去已知的方法等施予表面改質處理。
作為將矽烷化劑藥液暴露於基板表面的方法,可無特別限制下使用過去公知的方法。例如可舉出將矽烷化劑氣化後作為蒸汽,將該蒸汽於基板表面上進行接觸的方法、將含有矽烷化劑的基板表面處理液藉由噴霧法、旋轉塗佈法、浸塗法、輥塗佈法等於基板表面進行接觸的方法等。
上述方法之中,由可容易均勻地處理基板表面之觀點來看,將含有矽烷化劑的基板表面處理液於基板表面進行接觸的方法為佳。
對於本實施態樣,於基板表面暴露矽烷化劑藥液後,於矽烷化劑藥液所含有的有機溶劑等殘存於基板表面上時,除去該殘存物為佳。除去殘存物的方法並無特別限定,例如可舉出於基板表面吹入氮或乾燥空氣等氣體的方法或配合要除去的溶劑之沸點,將基板以適當溫度進
行加熱的方法等。
對於本實施態樣之表面處理方法,藉由在矽烷化劑之水解所產生的羥基彼此間產生之脫水縮合,可形成於基板表面含有矽化合物之皮膜(薄膜),藉由該皮膜可使基板表面疏水化。
藉由本實施態樣之表面處理方法,因可使基板表面進行疏水化,故例如可對於在表面形成微細圖型的基板,藉由將該表面進行疏水化,可抑制圖型倒落。
[實施例]
以下藉由實施例進一步具體說明本發明,但本發明並未限定於以下實施例。
[實施例1、2]
作為矽烷化劑使用三甲基矽基二甲基胺(TMSDMA),將該TMSDMA100%的液體作為處理前矽烷化劑藥液使用。將離子交換樹脂膜(DFA1SRPESW44;PALL公司製作)設置於過濾裝置上,在進行氮氣淨化的手套箱中(氮中)以丙二醇單甲基醚乙酸酯(PEGMEA)浸漬。其後,將處理前矽烷化劑藥液以約200ml/分鐘的流速透過前述離子交換樹脂膜,每1000ml過濾時,取樣100ml的操作重複3次。於處理前矽烷化劑藥液及3次取樣液所含有的金屬雜質量藉由ICP-MS進行測定,得到3次測定之平均值。該測定進行2次。
[比較例1]
未將離子交換樹脂膜預先與PEGMEA接觸以外,以與實施例1相同方式下測定金屬雜質量。
[金屬雜質殘存率之測定]
與實施例、比較例同樣地,測定處理前矽烷化劑之金屬雜質量,藉由金屬雜質減低步驟所得之經處理之矽烷化劑藥液所含有的金屬雜質量B,以處理前矽烷化劑藥液所含有的金屬雜質之量A除後所得之值B/A的百分率係為金屬雜質殘存率。其結果如表1所示。
表1中之數值單位為%。
由表1得知,在預先將離子交換樹脂膜與PEGMEA接觸的實施例1中,將藉由金屬雜質減低步驟所得之經處理之矽烷化劑藥液所含有的金屬雜質量B,以處理前矽烷化劑藥液所含有的金屬雜質量A除的值B/A之百分率所示金屬雜質殘存率對於Cu而言為23~42.4%,對於Al而言為45.6~63.5%,對於Zn而言為4.15~4.35%,金屬雜質的濃度經減低,該減低程度與未預先將
離子交換樹脂膜與PEGMEA接觸的比較例1相比,得知具有顯著優異性。
又,得知對於將處理前矽烷化劑藥液的使用量為約4倍的實施例2,與實施例1為幾乎相同程度下減低金屬雜質濃度。
Claims (9)
- 一種矽烷化劑藥液的調製方法,其特徵為含有使用預先使其與有機溶劑接觸的離子交換樹脂膜而減低處理前矽烷化劑藥液中之金屬雜質的步驟,前述有機溶劑為不具有與前述矽烷化劑進行反應的官能基之有機溶劑。
- 如請求項1之矽烷化劑藥液的調製方法,其中前述金屬雜質含有選自由Fe、Cu、Al及Zn所成群的至少1種。
- 如請求項1之矽烷化劑藥液的調製方法,其中前述離子交換樹脂膜在與前述有機溶劑接觸前進行氮氣淨化者。
- 如請求項1之矽烷化劑藥液的調製方法,其中前述有機溶劑為烷二醇烷基醚乙酸酯。
- 如請求項4之矽烷化劑藥液的調製方法,其中前述烷二醇烷基醚乙酸酯為丙二醇單甲基醚乙酸酯(PEGMEA)。
- 如請求項1之矽烷化劑藥液的調製方法,其中於前述矽烷化劑藥液所含的矽烷化劑為下述一般式(1)所示矽化合物;(R1)aSi(H)bX1 4-a-b (1)(式中,R1各彼此獨立表示含有一部分或全部的氫原子可由氟原子所取代的碳數1~18之1價烴基的1價有機基,X1各彼此獨立表示與矽原子鍵結的原子為氮之1價 官能基,a為1~3的整數,b為0~2的整數,a與b之合計為1~3)。
- 如請求項1之矽烷化劑藥液的調製方法,其中前述處理前矽烷化劑藥液僅由矽烷化劑及金屬雜質所成。
- 如請求項1之矽烷化劑藥液的調製方法,其中前述矽烷化劑藥液為基板表面處理液。
- 一種表面處理方法,其特徵為於基板表面暴露藉由如請求項1~8中任1項的矽烷化劑藥液之調製方法所得的矽烷化劑藥液,將前述基板表面經疏水化者。
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