TW202136278A - 表面處理劑及表面處理方法 - Google Patents
表面處理劑及表面處理方法 Download PDFInfo
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- TW202136278A TW202136278A TW109142349A TW109142349A TW202136278A TW 202136278 A TW202136278 A TW 202136278A TW 109142349 A TW109142349 A TW 109142349A TW 109142349 A TW109142349 A TW 109142349A TW 202136278 A TW202136278 A TW 202136278A
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- Prior art keywords
- surface treatment
- group
- carbon atoms
- treatment agent
- atom
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- 239000012756 surface treatment agent Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims description 41
- 238000004381 surface treatment Methods 0.000 title claims description 25
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 25
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 125000000962 organic group Chemical group 0.000 claims abstract description 21
- 125000001153 fluoro group Chemical group F* 0.000 claims abstract description 17
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 16
- 125000004429 atom Chemical group 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims description 56
- 125000004432 carbon atom Chemical group C* 0.000 claims description 53
- 238000006884 silylation reaction Methods 0.000 claims description 19
- 239000004065 semiconductor Substances 0.000 claims description 17
- 239000004094 surface-active agent Substances 0.000 description 28
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- 229920001296 polysiloxane Polymers 0.000 description 17
- -1 1,1-diethylpropyl Chemical group 0.000 description 16
- 125000000217 alkyl group Chemical group 0.000 description 16
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- 238000011156 evaluation Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
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- 125000004417 unsaturated alkyl group Chemical group 0.000 description 3
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- ODNRTOSCFYDTKF-UHFFFAOYSA-N 1,3,5-trimethylcyclohexane Chemical compound CC1CC(C)CC(C)C1 ODNRTOSCFYDTKF-UHFFFAOYSA-N 0.000 description 2
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- HNRMPXKDFBEGFZ-UHFFFAOYSA-N 2,2-dimethylbutane Chemical compound CCC(C)(C)C HNRMPXKDFBEGFZ-UHFFFAOYSA-N 0.000 description 2
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- 229910000577 Silicon-germanium Inorganic materials 0.000 description 2
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- 229940116423 propylene glycol diacetate Drugs 0.000 description 1
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
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- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
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- MRAZYSAHIPFJGX-UHFFFAOYSA-N trimethyl(1h-pyrazol-5-yl)silane Chemical compound C[Si](C)(C)C1=CC=NN1 MRAZYSAHIPFJGX-UHFFFAOYSA-N 0.000 description 1
- WLADIVUISABQHN-UHFFFAOYSA-N trimethyl(piperidin-1-yl)silane Chemical group C[Si](C)(C)N1CCCCC1 WLADIVUISABQHN-UHFFFAOYSA-N 0.000 description 1
- NQLVIKZJXFGUET-UHFFFAOYSA-N trimethyl(pyrrolidin-1-yl)silane Chemical compound C[Si](C)(C)N1CCCC1 NQLVIKZJXFGUET-UHFFFAOYSA-N 0.000 description 1
- DSPOVSQQYMUIGB-UHFFFAOYSA-N trimethyl(triazol-2-yl)silane Chemical compound C[Si](C)(C)N1N=CC=N1 DSPOVSQQYMUIGB-UHFFFAOYSA-N 0.000 description 1
- QHUNJMXHQHHWQP-UHFFFAOYSA-N trimethylsilyl acetate Chemical compound CC(=O)O[Si](C)(C)C QHUNJMXHQHHWQP-UHFFFAOYSA-N 0.000 description 1
- 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
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 1
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- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
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Abstract
一種表面處理劑,其含有矽烷化劑(A)與溶劑(S),其中矽烷化劑(A)包含通式(A-1)所示的化合物(A1),式中,Ra1
為1價有機基或氫原子,Ra2
為1價有機基,Ra1
及Ra2
中之與式中的氮原子鍵結的原子中,Si原子被除外,Ra3
為可被氟原子取代之脂肪族烴基或氫原子,Ra4
為可被氟原子取代之脂肪族烴基。
Description
本發明關於表面處理劑及表面處理方法。
本案係基於2019年12月6日在日本申請的特願2019-221093號主張優先權,在此援用其內容。
近年來,半導體裝置的高積體化及微小化之傾向升高,基板上的無機圖型之微細化及高縱橫比化正在進展。然而另一方面,發生所謂圖型倒塌之問題。此圖型倒塌係在基板上使多數的無機圖型並列形成時,鄰接的圖型彼此互相依靠而接近,在某些情況下圖型從基部折損或剝離之現象。若發生如此的圖型倒塌,則引起製品的良率及可靠性之降低。
已知此圖型倒塌係在圖型形成後的洗淨處理中,於洗淨液乾燥時,因該洗淨液的表面張力而發生者。亦即,在乾燥過程中去除洗淨液時,以洗淨液的表面張力為基礎的應力作用於圖型間,而發生圖型倒塌。
基於如此之背景,有提案採用如專利文獻1或專利文獻2中之保護膜形成用藥液。藉由此等文獻中的記載之藥液,可將凹凸圖型之表面予以撥水化,結果可抑制圖型倒塌。
又,雖然與圖型倒塌不同,但是為了使成為蝕刻遮罩的樹脂圖型與基板之密著性提升而防止因顯像液所致的樹脂圖型之一部分損失,進行使用六甲基二矽氮烷(HMDS)等之矽烷化劑將基板之表面撥水化(矽烷化)(例如,參照專利文獻3之[發明背景])。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2016-66785號公報
[專利文獻2]日本特開2012-033873號公報
[專利文獻3]日本特表平11-511900號公報
[發明所欲解決的課題]
基板上的無機圖型之微細化及高縱橫比化係越來越進展,洗淨・乾燥時的圖型倒塌變更容易發生。對於其,即使以如上述之習知的表面處理劑來撥水化處理圖型表面或基板表面,也會無法充分地抑制圖型倒塌。
因此,要求能更有效果地抑制圖型倒塌之表面處理劑。此外,於洗淨處理後,由於必須去除表面處理劑,故亦必須能容易去除。
本發明係鑒於上述情事而完成者,目的在於提供圖型倒塌的抑制效果優異,且從被處理體的去除性亦優異之表面處理劑及表面處理方法。解決課題的手段
為了解決上述課題,本發明採用以下之構成。
本發明之第1態樣為一種表面處理劑,其含有矽烷化劑(A)與溶劑(S),前述矽烷化劑(A)包含下述通式(A-1)所示的化合物(A1);
[式中,Ra1
為碳原子數1~10的1價有機基或氫原子;Ra2
為碳原子數1~10的1價有機基;Ra1
及Ra2
可互相鍵結而形成環;惟,Ra1
及Ra2
中之與式中的氮原子鍵結的原子中,Si原子被除外;Ra3
為可被氟原子取代之碳原子數1~4的脂肪族烴基或氫原子;Ra4
為可被氟原子取代之碳原子數1~4的脂肪族烴基]。
本發明之第2態樣為一種表面處理方法,其使用前述第1態樣之表面處理劑,進行被處理體之表面處理。
[發明的效果]
根據本發明,可提供圖型倒塌的抑制效果高,且從被處理體的去除性亦優異之表面處理劑及表面處理方法。
[實施發明的形態]
(表面處理劑)
本實施形態之表面處理劑含有矽烷化劑(A)與溶劑(S)。
本實施形態之表面處理劑例如係用於處理具有圖型的半導體基板之表面。
<矽烷化劑(A)>
矽烷化劑(A)(以下亦稱為「(A)成分」)係將被處理體(例如半導體基板)之表面矽烷化,用於提高被處理體(例如半導體基板)之表面的撥水性之成分。
本實施形態之表面處理劑中的矽烷化劑(A)包含下述通式(A-1)所示的化合物(A1)(以下亦稱為「(A1)成分」)。
≪化合物(A1)≫
化合物(A1)為下述通式(A-1)所示的化合物。
[式中,Ra1
為碳原子數1~10的1價有機基或氫原子;Ra2
為碳原子數1~10的1價有機基;Ra1
及Ra2
可互相鍵結而形成環;惟,Ra1
及Ra2
中之與式中的氮原子鍵結的原子中,Si原子被除外;Ra3
為可被氟原子取代之碳原子數1~4的脂肪族烴基或氫原子;Ra4
為可被氟原子取代之碳原子數1~4的脂肪族烴基]。
上述式(A-1)中,Ra1
為碳原子數1~10的1價有機基或氫原子。作為碳原子數1~10的1價有機基,可舉出可具有取代基的1價烴基。尚且,所謂「可具有取代基」,包含以1價基取代氫原子(-H)之情況與以2價基取代亞甲基(-CH2
-)之情況的兩者。
作為該1價取代基,可舉出羧基、羥基、胺基、磺基、鹵素原子、烷氧基、烷氧基羰基等。
作為該2價取代基,可舉出-O-、-C(=O)-O-、-C(=O)-、-O-C(=O)-O-、-C(=O)-NH-、-NH-、-CH=N-、-CH=N-CH=、-NH-C(=NH)-、-S-、-S(=O)2
-、-S(=O)2
-O-等。尚且,該2價取代基中的H可被烷基、醯基等取代基所取代。
作為該1價烴基,可舉出直鏈狀或支鏈狀的烷基、直鏈狀或支鏈狀的烯基或環狀的烴基。
該直鏈狀的烷基係碳原子數較佳為1~5,碳原子數更佳為1~4,碳原子數尤佳為1或2。具體而言,可舉出甲基、乙基、正丙基、正丁基、正戊基等。於此等之中,較佳為甲基、乙基或正丁基,更佳為甲基或乙基,尤佳為甲基。
該支鏈狀的烷基係碳原子數較佳為3~8,碳原子數更佳為3~5。具體而言,可舉出異丙基、異丁基、第三丁基、異戊基、新戊基、1,1-二乙基丙基、2,2-二甲基丁基等,較佳為異丙基。
該直鏈狀的烯基係碳原子數較佳為2~10,碳原子數更佳為2~5,碳原子數尤佳為2~4。具體而言,可舉出乙烯基、丙烯基(烯丙基)、丁炔基等。
作為該支鏈狀的烯基,具體而言,可舉出1-甲基-乙烯基、1-甲基丙烯基、2-甲基丙烯基等。
該環狀的烴基可為脂肪族烴基或芳香族烴基,且也可為多環式基或單環式基。
作為單環式基之脂肪族烴基,較佳為從單環烷中去掉1個氫原子後之基。作為該單環烷,較佳為碳原子數3~6者,具體而言可舉出環戊烷、環己烷等。
作為多環式基之脂肪族烴基,較佳為從多環烷中去掉1個氫原子後之基,作為該多環烷,較佳為碳原子數7~10者,具體而言可舉出金剛烷、降莰烷等。
該芳香族烴基為具有至少1個芳香環的烴基。
此芳香環只要是具有4n+2個π電子的環狀共軛系統,則沒有特別的限定,具體而言可舉出苯等之芳香族烴環;構成前述芳香族烴環的碳原子之一部分經雜原子所取代之芳香族雜環等。作為芳香族雜環中的雜原子,可舉出氧原子、硫原子、氮原子等。作為芳香族雜環,具體而言可舉出吡啶環、噻吩環等。
作為該芳香族烴基,具體而言,可舉出從前述芳香族烴環或芳香族雜環中去掉1個氫原子後之基(芳基或雜芳基);從包含2個以上芳香環的芳香族化合物(例如噻吩等)中去掉1個氫原子後之基;前述芳香族烴環或芳香族雜環的氫原子之1個經伸烷基所取代之基(例如苄基等之芳基烷基等)等。鍵結於前述芳香族烴環或芳香族雜環的伸烷基之碳原子數較佳為1~4,更佳為碳原子數1~2,特佳為碳原子數1。
上述式(A-1)中,Ra2
為碳原子數1~10的1價有機基。作為該1價有機基,可舉出與上述Ra1
同樣者。
Ra1
為碳原子數1~10的1價有機基時,於該有機基中,與式(A-1)中的氮原子鍵結的原子可為雜原子,但不是Si原子鍵結之情況。於Ra2
中亦同樣。
Ra1
及Ra2
可互相鍵結而形成環。作為Ra1
及Ra2
互相鍵結形成的環,具體而言可舉出下述環構造。*表示與上述式(A-1)中的Si原子之鍵結鍵。
上述式(A-1)中,Ra1
係於上述之中,較佳為碳原子數1~10的1價有機基。亦即,上述式(A-1)中,Ra1
及Ra2
較佳皆為碳原子數1~10的1價有機基。作為該1價有機基,更佳為碳原子數1~10之直鏈狀或支鏈狀的烷基,尤佳為碳原子數1~10之直鏈狀的烷基。
作為該直鏈狀的烷基,碳原子數較佳為1~5,碳原子數更佳為1~4,碳原子數尤佳為1或2。具體而言,較佳為甲基或乙基,更佳為甲基。
上述式(A-1)中,Ra3
為可被氟原子取代之碳原子數1~4的脂肪族烴基或氫原子。
於可被氟原子取代之碳原子數1~4的脂肪族烴基中,氟原子之數係沒有特別的限定,該脂肪族烴基中的氫原子全部可被氟原子取代。其中,氟原子之數較佳為0~2,該脂肪族烴基中的氫原子更佳為未被氟原子取代。
作為Ra3
中的碳原子數1~4的脂肪族烴基,具體而言,於上述Ra1
中之直鏈狀或支鏈狀的烷基、直鏈狀或支鏈狀的烯基所例示者之中,可舉出碳原子數為1~4者等。
上述式(A-1)中,Ra4
為可被氟原子取代之碳原子數1~4的脂肪族烴基。作為Ra4
,具體而言,可舉出與上述Ra3
中的可被氟原子取代之碳原子數1~4的脂肪族烴基同樣者。
上述式(A-1)中,Ra3
係於上述之中,較佳為可被氟原子取代之碳原子數1~4的脂肪族烴基。亦即,上述式(A-1)中,Ra3
及Ra4
較佳皆為可被氟原子取代之碳原子數1~4的脂肪族烴基,更佳皆為碳原子數1~4的脂肪族烴基,尤佳皆為碳原子數1~4之直鏈狀或支鏈狀的烷基,特佳皆為碳原子數1~4之直鏈狀的烷基。
作為該直鏈狀的烷基,碳原子數較佳為1或2,具體而言,較佳為甲基或乙基,更佳為甲基。
(A1)成分係於上述之中,較佳為下述通式(A-1-1)所示的化合物。
[式中,Ra1
為碳原子數1~10的1價有機基或氫原子;Ra2
為碳原子數1~10的1價有機基;Ra1
及Ra2
可互相鍵結而形成環;惟,Ra1
及Ra2
中之與式中的氮原子鍵結的原子中,Si原子被除外]。
上述式(A-1-1)中,Ra1
及Ra2
係與上述式(A-1)中的Ra1
及Ra2
相同。
作為(A1)成分之合適具體例,可舉出N,N-(二甲基矽烷基)二甲基胺、N,N-(二甲基矽烷基)二乙基胺、N,N-(二甲基矽烷基)咪唑、N,N-(二甲基矽烷基)三唑、N,N-(二甲基矽烷基)氮丙啶、N,N-(二甲基矽烷基)氧氮丙啶、N,N-(二甲基矽烷基)嗎啉,其中較佳為N,N-(二甲基矽烷基)二甲基胺或N,N-(二甲基矽烷基)二乙基胺,更佳為N,N-(二甲基矽烷基)二甲基胺。
本實施形態之表面處理劑中的(A1)成分可單獨使用1種,也可併用2種以上。
作為本實施形態之表面處理劑中的(A1)成分之含量的下限值,相對於表面處理劑全量,較佳為0.1~50質量%,更佳為0.5~30質量%,尤佳為1.0~20質量%,特佳為5.0~10質量%。
若(A1)成分之含量為上述較佳的下限值以上,則可更提高被處理體之表面的撥水性。
另一方面,若(A)成分之含量為上述較佳的上限值以下,則容易得到操作性更加優異的表面處理劑。
本實施形態之表面處理劑中的(A1)成分之莫耳濃度較佳為0.01~5.0M,更佳為0.1~1.0M。
若(A1)成分之莫耳濃度為上述較佳的下限值以上,則可更提高被處理體之表面的撥水性。
若(A1)成分之莫耳濃度為上述較佳的上限值以下,則容易得到操作性更加優異的表面處理劑。
本實施形態之表面處理劑中的矽烷化劑(A)可含有上述(A1)成分以外的矽烷化劑(A2)(以下亦稱為「(A2)成分」)。
・(A1)成分以外的矽烷化劑(A2)
作為(A2)成分,並沒有特別的限定,可使用上述(A1)成分以外之習知的一切矽烷化劑。例如可使用下述通式(1)~(3)各自表示的矽烷化劑。尚且,於下述通式(1)~(3)中,烷基為碳數1~5,環烷基為碳數5~10,烷氧基為碳數1~5,雜環烷基為碳數5~10。
[式(3)中,X表示O、CHR7
、CHOR7
、CR7
R7
或NR8
,R6
、R7
各自獨立地表示氫原子、飽和或不飽和烷基、飽和或不飽和環烷基、三烷基矽烷基、三烷基矽烷氧基、烷氧基、苯基、苯乙基或乙醯基,R8
表示氫原子、烷基或三烷基矽烷基]。
作為上述式(1)所示的矽烷化劑,可舉出N,N-二甲基胺基三甲基矽烷(TMSDMA)、N,N-二乙基胺基三甲基矽烷、第三丁基胺基三甲基矽烷、烯丙基胺基三甲基矽烷、三甲基矽烷基乙醯胺、三甲基矽烷基哌啶、三甲基矽烷基咪唑、三甲基矽烷基嗎啉、3-三甲基矽烷基-2-㗁唑啉酮、三甲基矽烷基吡唑、三甲基矽烷基吡咯啶、2-三甲基矽烷基-1,2,3-三唑、1-三甲基矽烷基-1,2,4-三唑等。
作為上述式(2)所示的矽烷化劑,可舉出四甲基二矽氮烷(TMDS)、六甲基二矽氮烷(HMDS)、N-甲基六甲基二矽氮烷、1.2-二-N-辛基四甲基二矽氮烷、1,2-二乙烯基四甲基二矽氮烷、七甲基二矽氮烷、九甲基三矽氮烷、參(二甲基矽烷基)胺等。
又,作為上述式(3)所示的矽烷化劑,可舉出三甲基矽烷基乙酸酯、三甲基矽烷基丙酸酯、三甲基矽烷基丁酸酯、三甲基矽氧基-3-戊烯-2-酮等。
本實施形態之表面處理劑中的(A2)成分可單獨使用1種,也可併用2種以上。
作為本實施形態之表面處理劑中的(A2)成分之含量,只要不損害本發明的效果,則沒有特別的限制,例如較佳為0.001質量%以上30質量%以下,更佳為0.1質量%以上15質量%以下。
於本實施形態之表面處理劑中,(A)成分中的(A1)成分之比例,相對於(A)成分之總含量,較佳為25質量%以上,更佳為50質量%以上,尤佳為75質量%以上,也可為100質量%。
若(A)成分中的(A1)成分之比例為25質量%以上,則可更提高被處理體之表面的撥水性,且亦可更提高表面處理劑之去除性。
<溶劑(S)>
本實施形態之表面處理劑含有溶劑(S)(以下亦稱為「(S)成分」)。(S)成分係用於將各成分溶解・混合而成為均勻的溶液。(S)成分只要能將各成分溶解・混合,則可無特別限制地使用作為表面處理劑的溶劑所一般使用者。
作為(S)成分,例如可舉出正己烷、正庚烷、正辛烷、正壬烷、正癸烷、正十一烷、正十二烷、正十三烷、正十四烷、正十五烷、正十六烷、正十七烷、正十八烷、正十九烷、正二十烷等之直鏈狀飽和脂肪族烴類;2-甲基戊烷、3-甲基戊烷、2,2-二甲基丁烷、2,3-二甲基丁烷、2-甲基己烷、3-甲基己烷、2,3-二甲基戊烷、2,4-二甲基戊烷、2,2,3-三甲基戊烷、2,2,4-三甲基戊烷、3,4-二乙基己烷、2,6-二甲基辛烷、3,3-二甲基辛烷、3,5-二甲基辛烷、4,4-二甲基辛烷、3-乙基-3-甲基庚烷、2-甲基壬烷、3-甲基壬烷、4-甲基壬烷、5-甲基壬烷、2-甲基十一烷、3-甲基十一烷、2,2,4,6,6-五甲基庚烷、2,2,4,4,6,8,8-七甲基壬烷等之支鏈狀飽和脂肪族烴類;十氫萘、環己烷、甲基環己烷、乙基環己烷、1,2-二甲基環己烷、1,3-二甲基環己烷、1,4-二甲基環己烷、丙基環己烷、異丙基環己烷、1,2-甲基乙基環己烷、1,3-甲基乙基環己烷、1,4-甲基乙基環己烷、1,2,3-三甲基環己烷、1,2,4-三甲基環己烷、1,3,5-三甲基環己烷等之環狀飽和脂肪族烴類;二甲基亞碸等之亞碸類;二甲基碸、二乙基碸、雙(2-羥基乙基)碸、四亞甲基碸等之碸類;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-二乙基乙醯胺等之醯胺類;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-吡咯啶酮等之內醯胺類;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-咪唑啉酮等之咪唑啉酮類;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、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、三乙二醇二甲基醚、四乙二醇二甲基醚、丙二醇單甲基醚等之其他醚類;乙二醇單甲基醚乙酸酯、乙二醇單乙基醚乙酸酯、乙二醇單丁基醚乙酸酯、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之(聚)烷二醇單烷基醚乙酸酯類;2-羥基丙酸甲酯、2-羥基丙酸乙酯、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-甲基丁酸甲酯、3-甲氧基丁基乙酸酯、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、乙酸正丙酯、乙酸異丙酯、乙酸正丁酯、乙酸異丁酯、乙酸正戊酯、乙酸正己酯、乙酸正庚酯、乙酸正辛酯、甲酸正戊酯、乙酸異戊酯、丙酸正丁酯、丁酸乙酯、丁酸正丙酯、丁酸異丙酯、丁酸正丁酯、正辛酸甲酯、癸酸甲酯、丙酮酸甲酯、丙酮酸乙酯、丙酮酸正丙酯、乙醯乙酸甲酯、乙醯乙酸乙酯、2-側氧基丁酸乙酯、己二酸二甲酯、丙二醇二乙酸酯、碳酸伸丙酯等之其他酯類;甲基乙基酮、環己酮、2-庚酮、3-庚酮等之酮類;β-丙內酯、γ-丁內酯、δ-戊內酯等之內酯類;苯、甲苯、二甲苯、1,3,5-三甲基苯、萘等之芳香族烴類;對薄荷烷、二苯基薄荷烷、檸檬烯、萜品烯、莰烷、降莰烷、蒎烷等之萜烯類等。
本實施形態之表面處理劑係相對於表面處理劑全量,(S)成分之含量較佳為50~99.9質量%,更佳為70~98質量%,尤佳為80~96質量%。
<其他成分>
本實施形態之表面處理劑係在不損害本發明的效果之範圍內,可含有上述成分以外之其他成分。作為其他成分,可舉出酸或鹼等之pH調整劑、界面活性劑等。
≪界面活性劑≫
作為界面活性劑,例如可舉出氟系界面活性劑或聚矽氧系界面活性劑。
作為氟系界面活性劑,於具體例中可舉出BM-1000、BM-1100(皆BM化學公司製)、Megafac F142D、Megafac F172、Megafac F173、Megafac F183(皆DIC公司製)、Fluorad FC-135、Fluorad FC-170C、Fluorad FC-430、Fluorad FC-431(皆住友3M公司製)、Surflon S-112、Surflon S-113、Surflon S-131、Surflon S-141、Surflon S-145(皆旭硝子公司製)、SH-28PA、SH-190、SH-193、SZ-6032、SF-8428(皆東麗聚矽氧公司製)等之市售的氟系界面活性劑。
作為聚矽氧系界面活性劑,於具體例中,可較宜使用未改質聚矽氧系界面活性劑、聚醚改質聚矽氧系界面活性劑、聚酯改質聚矽氧系界面活性劑、烷基改質聚矽氧系界面活性劑、芳烷基改質聚矽氧系界面活性劑及反應性聚矽氧系界面活性劑等。
作為聚矽氧系界面活性劑,可使用市售的聚矽氧系界面活性劑。作為市售的聚矽氧系界面活性劑之具體例,可舉出Paintad M(東麗-道康寧公司製)、Topica K1000、Topica K2000、Topica K5000(皆高千穗產業公司製)、XL-121(聚醚改質聚矽氧系界面活性劑,CLARIANT公司製)、BYK-310(聚酯改質聚矽氧系界面活性劑,BYK化學公司製)等。
本實施形態之表面處理劑含有界面活性劑時,界面活性劑可單獨使用1種,也可併用2種以上。
本實施形態之表面處理劑中的界面活性劑之含量,只要不損害本發明的效果,則沒有特別的限制,例如較佳為0.001質量%以上10質量%以下。
以上說明的本實施形態之表面處理劑由於包含(A1)成分作為矽烷化劑,故可更提高被處理體之表面的撥水性,可更提高圖型倒塌的抑制效果。此外,由於(A1)成分係容易藉由加熱而去除,故本實施形態之表面處理劑係從被處理體的去除性亦優異。
本實施形態之表面處理劑係有用於處理具有圖型的半導體基板之表面的表面處理劑。
(表面處理方法)
本實施形態之表面處理方法係使用上述表面處理劑,進行被處理體之表面處理之表面處理方法。
作為表面處理目的之代表例,可舉出將在被處理體上形成的無機圖型之表面撥水化,防止洗淨處理中的圖型倒塌。
本實施形態之表面處理方法具有將被處理體之表面撥水化(矽烷化)之撥水化處理步驟。
<撥水化處理步驟>
作為本實施形態中的撥水化處理步驟,可舉出將上述表面處理劑賦予至被處理體之表面之方法。
作為將表面處理劑賦予至被處理體之表面之方法,可例示噴霧法、旋轉塗佈法、浸漬法等。將表面處理劑賦予至被處理體之表面的時間係沒有特別的限定,例如可例示1秒~5分鐘。
關於被處理體之表面的撥水性,於表面處理後,水對於被處理體之表面的接觸角較佳成為40~120˚,更佳成為70~110˚,尤佳為90~110˚。
作為用於撥水化處理步驟之裝置,只要是能對於被處理體賦予表面處理劑之裝置,則沒有特別的限定。作為如此的裝置,可例示對於被處理體,藉由噴霧法、旋轉塗佈法、浸漬法等能賦予表面處理劑之裝置。
作為成為表面處理之對象的「被處理體」,可例示用於半導體裝置製作的基板,例如可舉出矽(Si)基板、氮化矽(SiN)基板、矽氧化膜(Ox)基板、碳化矽(SiC)基板、鎢(W)基板、碳化鎢(WC)基板、鈷(Co)基板、氮化鈦(TiN)基板、氮化鉭(TaN)基板、鍺(Ge)基板。矽鍺(SiGe)基板、鋁(Al)基板、鎳(Ni)基板、鈦(Ti)基板、釕(Ru)基板、銅(Cu)基板等。
若以矽(Si)基板為例進行說明,則可為自然氧化膜、熱氧化膜及氣相合成膜(CVD膜等)等之氧化矽膜形成於表面者,也可為在前述氧化矽膜上形成有圖型者。
所謂「表面」,除了基板本身之表面,還可舉出在基板上所設置的無機圖型之表面以及未圖型化的無機層之表面。
作為在基板上所設置的無機圖型,可例示藉由光阻法在基板上存在的無機層之表面,製作蝕刻遮罩,然後藉由蝕刻處理而形成的無機圖型。作為無機層,除了基板本身,還可例示由構成基板的元素之氧化物所成的層、由在基板之表面上形成的氮化矽、氮化鈦、鎢等之無機物所成的層等。作為如此的無機層,並沒有特別的限定,可例示半導體裝置之製造過程中形成的無機層。
前述圖型之形狀係沒有特別的限定,例如可為半導體製程中一般形成的圖型形狀。圖型形狀可為線圖型,也可為孔圖型,亦可為包含複數的柱之圖型。圖型形狀較佳為包含複數的柱之圖型。柱之形狀係沒有特別的限定,例可舉出圓柱形狀、多角柱形狀(四角柱形狀等)等。
[任意步驟]
本實施形態之表面處理方法係除了上述撥水化處理步驟之外,還可具有洗淨步驟、沖洗步驟及乾燥步驟。
例如,作為本實施形態之表面處理方法的一實施形態,一種表面處理方法,其具有:洗淨被處理體之表面之洗淨步驟;藉由上述表面處理劑,將前述經洗淨的被處理體撥水化(矽烷化)之撥水化處理步驟;以沖洗液沖洗前述經撥水化的被處理體之表面之步驟;及,將前述經沖洗的被處理體乾燥之乾燥步驟。
≪洗淨步驟≫
洗淨步驟係預先洗淨被處理體之表面之步驟。
洗淨方法係沒有特別的限定,例如作為半導體基板之洗淨方法,可舉出眾所周知的RCA洗淨法等。於此RCA洗淨法中,首先將半導體基板浸漬於過氧化氫與氫氧化銨之SC-1溶液中,從半導體基板去除微粒子及有機物。接著,將半導體基板浸漬於氟化氫水溶液中,去除基板表面的自然氧化膜。然後,將半導體基板浸漬於過氧化氫與稀鹽酸之SC-2溶液的酸性溶液中,去除在SC-1溶液中不溶的鹼離子或金屬雜質。
≪沖洗步驟≫
沖洗步驟係以沖洗液沖洗經撥水化(矽烷化)的被處理體之表面之步驟。
於沖洗步驟中,以後述之沖洗液沖洗經撥水化(矽烷化)的被處理體之表面。沖洗之方法係沒有特別的限定,可採用半導體製程中一般用於基板之洗淨的方法。作為如此之方法,例如可舉出將被處理體浸漬於沖洗液中之方法、使被處理體接觸沖洗液的蒸氣之方法、邊使被處理體旋轉邊將沖洗液供給至被處理體之方法等。其中,作為沖洗方法,較佳為邊使被處理體旋轉邊將沖洗液供給至被處理體之方法。前述方法中,作為旋轉的旋轉速度,例如可例示100rpm以上5000rpm以下。
・沖洗液
作為用於沖洗步驟之沖洗液,並沒有特別的限定,可使用一般用於半導體基板之沖洗步驟者。作為沖洗液,例如可舉出含有溶劑者。作為溶劑,可舉出與上述溶劑(S)同樣者或異丙醇、1-己醇等之醇系溶劑。
沖洗液係可代替前述溶劑,或也含有溶劑連同水。
沖洗液係可含有眾所周知的添加物等。作為眾所周知的添加劑,例如可舉出氟系界面活性劑或聚矽氧系界面活性劑。作為該氟系界面活性劑及聚矽氧系界面活性劑,可舉出與在上述表面處理劑所說明的氟系界面活性劑及聚矽氧系界面活性劑同樣者。
≪乾燥步驟≫
乾燥步驟係使被處理體乾燥之步驟。藉由進行乾燥步驟,可高效率地去除在沖洗步驟後殘留於被處理體的沖洗液。
被處理體之乾燥方法係沒有特別的限制,可使用旋轉乾燥、加熱乾燥、溫風乾燥、真空乾燥等之眾所周知的方法。例如,可適宜地例示惰性氣體(氮氣等)流動下的旋轉乾燥。
以上說明的本實施形態之表面處理方法,由於使用上述實施形態之表面處理劑,故圖型倒塌的抑制效果優異。
本實施形態之表面處理方法係有用於處理具有圖型的半導體基板之表面的方法。
[實施例]
以下,藉由實施例更詳細地說明本發明,惟本發明不受此等之例所限定。
<表面處理劑之調製>
(實施例1、比較例1~3)
混合表1所示的各成分,調製各例之表面處理劑。尚且,以各例之表面處理劑中的(A)成分之莫耳濃度成為0.62M之方式,調製各例之表面處理劑。
表1中,各縮寫符號各自具有以下之意義。[ ]內的數值為摻合量(質量%)。
(A1)-1:N,N-(二甲基矽烷基)二甲基胺(DMSDMA)
(A2)-1:N,N-二甲基胺基三甲基矽烷(TMSDMA)
(A2)-2:四甲基二矽氮烷(TMDS)
(A2)-3:六甲基二矽氮烷(HMDS)
(S)-1:丙二醇單甲基醚乙酸酯(PGMEA)
<表面處理方法1>
作為被處理體,使用表面材質為SiO2
的基板。以0.5%氟化氫水溶液洗淨該基板1分鐘後,將該基板在各例之表面處理劑中分別在室溫(25℃)下浸漬1分鐘。然後,以異丙醇沖洗基板表面,藉由氮氣流進行乾燥。
[撥水性之評價]
於經由上述<表面處理方法1>所表面處理的基板之表面,使用Dropmaster 700(協和界面科學公司製),將純水液滴(2.0μL)滴下至該基板之表面,測定滴下2秒後的水對於上述基板表面之接觸角。接觸角愈大,意指撥水性愈高。表2中顯示其結果。
[去除性之評價]
將經由上述[撥水性之評價]所評價的基板,在經加熱到300℃的熱板上加熱處理20分鐘。然後,使用Dropmaster 700(協和界面科學公司製),將純水液滴(2.0μL)滴下至該基板之表面,測定滴下2秒後的接觸角。求出該接觸角與上述[撥水性之評價]所測定的接觸角之差,用以下之基準評價各例之表面處理劑從上述基板之去除性。表2中顯示其結果。
尚且,關於比較例3之表面處理劑,由於撥水性非常低,故不進行去除性之評價。
<評價基準>
A:因加熱處理而接觸角降低4˚以上
B:因加熱處理所致的接觸角之降低未達4˚
<表面處理方法2>
作為被處理體,使用具有柱構造的矽圖型晶片(1cm×1cm)。將該晶片在各例之表面處理劑中分別在室溫(25℃)下浸漬1分鐘。然後,以異丙醇沖洗該晶片表面,藉由氮氣流進行乾燥。
[圖型倒塌抑制性之評價]
以SEM觀察經由上述<表面處理方法2>所表面處理的晶片之表面,算出該晶片的圖型倒塌之發生率,用以下之基準評價圖型倒塌的抑制性。表2中顯示其結果。
尚且,不以各例之表面處理劑來表面處理上述晶片,以異丙醇沖洗該晶片表面,藉由氮氣流進行乾燥時之該晶片的圖型倒塌之發生率為100%。
<評價基準>
A:圖型倒塌之發生率未達10%
B:圖型倒塌之發生率為10%以上
由表2所示的結果可確認:與比較例之表面處理劑比較下,實施例之表面處理劑係水的接觸角大,撥水性高。又,與比較例之表面處理劑比較下,可確認實施例之表面處理劑係加熱處理後的水之接觸角的變化量大,去除性亦優異。此外,可確認:經實施例之表面處理劑所表面處理的上述晶片係沖洗及乾燥後的圖型倒塌之發生率未達10%,圖型倒塌之抑制性亦優異。
Claims (4)
- 如請求項1之表面處理劑,其係用於處理具有圖型的半導體基板之表面。
- 一種表面處理方法,其使用如請求項1之表面處理劑,進行被處理體之表面處理。
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