TW202235511A - 金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法 - Google Patents
金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法 Download PDFInfo
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- metal oxide
- mass
- oxide film
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 161
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 161
- 239000000203 mixture Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- -1 carboxylic acid halides Chemical class 0.000 claims abstract description 51
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 26
- 239000004094 surface-active agent Substances 0.000 claims description 20
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
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- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
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- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 4
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011651 chromium Substances 0.000 claims description 3
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- 229910052738 indium Inorganic materials 0.000 claims description 3
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- 239000011733 molybdenum Substances 0.000 claims description 3
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- 239000010937 tungsten Substances 0.000 claims description 3
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
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- 229910052720 vanadium Inorganic materials 0.000 claims description 2
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- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F1/00—Originals for photomechanical production of textured or patterned surfaces, e.g., masks, photo-masks, reticles; Mask blanks or pellicles therefor; Containers specially adapted therefor; Preparation thereof
- G03F1/20—Masks or mask blanks for imaging by charged particle beam [CPB] radiation, e.g. by electron beam; Preparation thereof
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on 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 aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/08—Copolymers of styrene
- C09D125/14—Copolymers of styrene with unsaturated esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/45—Anti-settling agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
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Abstract
本發明提供一種金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法,上述金屬氧化物膜形成性組合物提供於400℃以下進行加熱時體積收縮得到抑制之金屬氧化物膜。
本發明之金屬氧化物膜形成性組合物含有:金屬氧化物奈米團簇、封端劑、基材及溶劑,上述金屬氧化物奈米團簇之尺寸為5 nm以下,上述封端劑包含選自由烷氧基矽烷、酚、醇、羧酸及羧醯鹵所組成之群中之至少1種,於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。
Description
本發明係關於一種金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法。
一般而言,半導體裝置製造等中之蝕刻加工中,將光阻劑或電子束抗蝕劑等抗蝕劑材料塗佈於被蝕刻基體表面,將藉由微影技術而形成圖案之抗蝕膜作為蝕刻遮罩進行蝕刻,藉此,於被蝕刻基體上形成特定之圖案。
此處,根據被蝕刻基體之蝕刻速率之不同,存在抗蝕膜對被蝕刻基體之蝕刻選擇性之問題,故存在抗蝕膜作為蝕刻遮罩未充分發揮作用之情形。因此,於對此種被蝕刻基體進行蝕刻之情形時,設置被稱為硬罩之蝕刻遮罩,將蝕刻遮罩對被蝕刻基體之蝕刻選擇性維持為較高。作為硬罩,例如公知有包含含有氧化鋯奈米粒子等金屬氧化物奈米粒子之金屬氧化物膜之硬罩(參照專利文獻1)。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本專利特表2020-503409號公報
[發明所欲解決之問題]
包含金屬氧化物奈米粒子之先前之金屬氧化物膜係對包含含有金屬氧化物奈米粒子之組合物之塗膜進行加熱而形成。本發明人等進行研究,結果判明,先前之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮較大,故於450℃之高溫下進行正式焙燒時面內均勻性變低,其結果為,於使用正式焙燒後之金屬氧化物膜作為乾式蝕刻時之硬罩之情形時,難以均勻地進行乾式蝕刻。
本發明係鑒於此種先前之情況而成者,其目的在於提供一種金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法,上述金屬氧化物膜形成性組合物提供於400℃以下進行加熱時體積收縮得到抑制之金屬氧化物膜。
[解決問題之技術手段]
本發明人等為了解決上述問題而反覆銳意研究。其結果為,發現藉由如下金屬氧化物膜形成性組合物而可解決上述問題,從而完成本發明,該金屬氧化物膜形成性組合物含有特定尺寸之金屬氧化物奈米團簇、特定之封端劑、基材及溶劑,且於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。具體而言,本發明提供以下者。
本發明之第一形態係一種金屬氧化物膜形成性組合物,其係含有金屬氧化物奈米團簇、封端劑、基材及溶劑者,且
上述金屬氧化物奈米團簇之尺寸為5 nm以下,
上述封端劑包含選自由烷氧基矽烷、酚、醇、羧酸、及羧醯鹵所組成之群中之至少1種,
於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。
本發明之第二形態係一種金屬氧化物膜之製造方法,其包括:
形成包含第1形態之金屬氧化物膜形成性組合物之塗膜之塗膜形成步驟;及
對上述塗膜進行加熱之加熱步驟。
本發明之第三形態係一種降低金屬氧化物膜之體積收縮率之方法,該金屬氧化物膜係形成包含金屬氧化物膜形成性組合物之塗膜,並對上述塗膜進行加熱而獲得者,
上述方法包括以含有金屬氧化物奈米團簇、封端劑、基材及溶劑之方式構成上述金屬氧化物膜形成性組合物,
上述金屬氧化物奈米團簇之尺寸為5 nm以下,
上述封端劑包含選自由烷氧基矽烷、酚、醇、羧酸、及羧醯鹵所組成之群中之至少1種,
於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。
[發明之效果]
根據本發明,可提供一種金屬氧化物膜形成性組合物、使用其之金屬氧化物膜之製造方法、及降低金屬氧化物膜之體積收縮率之方法,上述金屬氧化物膜形成性組合物提供於400℃以下進行加熱時體積收縮得到抑制之金屬氧化物膜。
<金屬氧化物膜形成性組合物>
本發明之金屬氧化物膜形成性組合物含有:金屬氧化物奈米團簇、封端劑、基材及溶劑。本發明之金屬氧化物膜形成性組合物可提供一種於400℃以下進行加熱時體積收縮得到抑制之金屬氧化物膜。
於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上,較佳為30質量%以上,更佳為40質量%以上。若該比率為上述範圍內,則可將無機成分質量之比率設定為較高,其結果為,獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。該比率之上限並無特別限制,可為90質量%,可為80質量%,亦可為75質量%。
[金屬氧化物奈米團簇]
於本說明書中,金屬氧化物奈米團簇係指金屬氧化物之聚集體,且為包含由金屬氧化物形成之複數個面之聚集體。再者,金屬氧化物奈米團簇包含金屬氧化物,不包含封端劑。若本發明之金屬氧化物膜形成性組合物同時含有封端劑及金屬氧化物奈米團簇,則獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。
藉由對金屬氧化物奈米團簇進行X射線繞射測定,而檢測到相當於上述面之繞射峰。金屬氧化物奈米團簇可包含結晶、微晶或非晶質。根據金屬氧化物奈米團簇中包含之成分不同,而於金屬氧化物奈米團簇之X射線繞射圖案中檢測到源於金屬原子之面(結晶面)之峰、較寬之突起或較寬之暈圈圖案。於在某試樣之X射線繞射圖案中不僅未檢測到峰,甚至連較寬之突起或較寬之暈圈圖案亦未檢測到之情形時,本說明書中判斷該試樣中不包含金屬氧化物奈米團簇。
金屬氧化物奈米團簇之尺寸為5 nm以下,較佳為4 nm以下,更佳為3 nm以下。金屬氧化物奈米團簇之尺寸之下限並無特別限制,例如可為0.5 nm以上,可為1 nm以上,亦可為2 nm以上。認為若金屬氧化物奈米團簇之尺寸超過5 nm,則獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮不易得到抑制,故於450℃之高溫下進行正式焙燒時面內均勻性易變低,結果為,於使用正式焙燒後之金屬氧化物膜作為乾式蝕刻時之硬罩之情形時,易變得難以均勻地進行乾式蝕刻。於本說明書中,金屬氧化物奈米團簇之尺寸係指根據藉由X射線散射強度分佈測定而檢測到之光譜中之散射峰之半高寬並利用Halder-Wagner法而算出之值。
作為金屬氧化物奈米團簇中包含之金屬,並無特別限制,例如可例舉:鋅、釔、鉿、鋯、鑭、鈰、釹、釓、鈥、鎦、鉭、鈦、矽、鋁、銻、錫、銦、鎢、銅、釩、鉻、鈮、鉬、釕、銠、錸、銥、鍺、鎵、鉈、鎂,就製膜性、穩定性等觀點而言,較佳為鋅、釔、鉿、及鋯,更佳為鋯。上述金屬可單獨使用1種,亦可併用2種以上。
金屬氧化物奈米團簇之使用量並無特別限制,相對於金屬氧化物膜形成性組合物中之除溶劑以外之成分之總計,例如為45~75質量%,較佳為50~72質量%。若金屬氧化物奈米團簇之使用量為上述範圍內,則獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。
[封端劑]
推測於本發明之金屬氧化物膜形成性組合物中,金屬氧化物奈米團簇之一部分或全部被封端劑覆蓋。封端劑包含選自由烷氧基矽烷、酚、醇、羧酸、及羧醯鹵所組成之群中之至少1種。若本發明之金屬氧化物膜形成性組合物同時含有金屬氧化物奈米團簇及封端劑,則獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。
作為封端劑之具體例,可例舉:正丙基三甲氧基矽烷、正丙基三乙氧基矽烷、正辛基三甲氧基矽烷、正辛基三乙氧基矽烷、正十二烷基三甲氧基矽烷、正十二烷基三乙氧基矽烷、正十六烷基三甲氧基矽烷、正十六烷基三乙氧基矽烷、正十八烷基三甲氧基矽烷、正十八烷基三乙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、苯乙基苯基三甲氧基矽烷、苯乙基乙基三乙氧基矽烷、3-{2-甲氧基[聚(伸乙氧基)]}丙基三甲氧基矽烷、3-{2-甲氧基[聚(伸乙氧基)]}丙基三乙氧基矽烷、3-{2-甲氧基[三(伸乙氧基)]}丙基三甲氧基矽烷、3-{2-甲氧基[三(伸乙氧基)]}丙基三乙氧基矽烷、乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、烯丙基三甲氧基矽烷、烯丙基三乙氧基矽烷、1-己烯基三甲氧基矽烷,1-己烯基三乙氧基矽烷、1-辛烯基三甲氧基矽烷、1-辛烯基三乙氧基矽烷、3-胺基丙基三甲氧基矽烷、3-胺基丙基三乙氧基矽烷、3-巰丙基三甲氧基矽烷、3-巰丙基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、3-丙烯醯基丙基三乙氧基矽烷、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、3-異氰酸基丙基三甲氧基矽烷、3-異氰酸基丙基三乙氧基矽烷、3-縮水甘油氧基丙基三甲氧基矽烷、及3-縮水甘油氧基丙基三乙氧基矽烷等烷氧基矽烷;乙醇、正丙醇、異丙醇、正丁醇、正庚醇、正己醇、正辛醇、油醇、正十二醇、正十八醇、苄醇、苯酚、及三乙二醇單甲醚等酚類或醇類;辛酸、乙酸、丙酸、2-[2-(甲氧基乙氧基)乙氧基]乙酸、油酸、月桂酸、苯甲酸、2-丙烯醯氧基乙基琥珀酸、2-丙烯醯氧基乙基鄰苯二甲酸等酸類;及該等酸類之醯氯等該等酸類之醯鹵類,較佳為作為酚類、醇類或酸類例舉之化合物。
封端劑之使用量並無特別限制,相對於金屬氧化物膜形成性組合物中之除溶劑以外之成分之總計,例如為10~35質量%,較佳為18~28質量%。若封端劑之使用量為上述範圍內,則有機成分質量之比率不會變得過高,其結果為,獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。
於上述金屬氧化物膜形成性組合物之固形物成分中,上述金屬氧化物奈米團簇相對於上述金屬氧化物奈米團簇與上述封端劑之總計之質量比例如為50質量%以上,較佳為55質量%以上,更佳為60質量%以上,進而更佳為65質量%以上。上述質量比之上限例如為95質量%以下,較佳為90質量%以下。
[基材]
為了調整塗膜形成性或塗佈性,本發明之金屬氧化物膜形成性組合物含有基材。基材可單獨使用1種,亦可併用2種以上。作為基材,並無特別限制,可使用樹脂等聚合物或低分子化合物等非聚合物。
基材之質量平均分子量(以下稱為「Mw」)於不阻礙本發明之目的之範圍內並無特別限制,較佳為700以上40000以下,更佳為900以上30000以下,進而更佳為1000以上20000以下。若Mw為上述範圍內,則塗膜形成性及塗佈性易變得良好。又,藉由使用Mw為4000以下之聚合物或非聚合物,而對凹凸基板之間隙填充性易變得良好。再者,於本說明書中,作為Mw,採用藉由凝膠滲透層析法(GPC)所獲得之聚苯乙烯換算值。
[丙烯酸系樹脂(a-IV)]
作為丙烯酸系樹脂(a-IV),可使用包含來自(甲基)丙烯酸之結構單元、及/或來自(甲基)丙烯酸酯等其他單體之結構單元者。(甲基)丙烯酸為丙烯酸或甲基丙烯酸。作為提供丙烯酸系樹脂(a-IV)中之結構單元之單體,典型而言,較佳為使用下述式(a-4-1)所表示之化合物。
上述式(a-4-1)中,R
a9為氫原子或甲基。R
a10為氫原子或1價有機基。關於該有機基,該有機基中可包含雜原子等除烴基以外之鍵或取代基。又,該有機基可為直鏈狀、支鏈狀、環狀之任一者。R
a11為-O-或-NR
a12-所表示之基。R
a12為氫原子或碳原子數1以上6以下之烷基。
作為R
a10之有機基中之除烴基以外之取代基,只要不損害本發明之效果,則並無特別限制,可例舉:鹵素原子、羥基、巰基、硫基、氰基、異氰基、氰酸基、異氰酸基、硫氰酸基、異硫氰酸基、矽烷基、矽烷醇基、烷氧基、烷氧羰基、胺甲醯基、硫胺甲醯基、硝基、亞硝基、羧基、羧酸酯基、醯基、醯氧基、亞磺酸基、磺基、磺酸根基、膦基、氧膦基、膦醯基、膦酸基、羥基亞胺基、烷基醚基、烷基硫醚基、芳醚基、芳基硫醚基、胺基(-NH
2、-NHR、-NRR':R及R'分別獨立地表示烴基)等。上述取代基中包含之氫原子可被烴基取代。又,上述取代基中包含之烴基可為直鏈狀、支鏈狀、及環狀之任一者。
又,作為R
a10之有機基可具有丙烯醯氧基、甲基丙烯醯氧基、環氧基、氧雜環丁基等反應性之官能基。
丙烯醯氧基或甲基丙烯醯氧基等具有不飽和雙鍵等之醯基例如可藉由使包含具有環氧基之結構單元之丙烯酸系樹脂(a-IV)中之環氧基之至少一部分與丙烯酸或甲基丙烯酸等不飽和羧酸發生反應而製造。
可於使環氧基之至少一部分與不飽和羧酸發生反應之後,使藉由反應而生成之基與多元酸酐發生反應。
作為多元酸酐之具體例,可例舉:馬來酸酐、琥珀酸酐、伊康酸酐、鄰苯二甲酸酐、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、偏苯三甲酸酐、均苯四甲酸二酐、二苯甲酮四羧酸二酐、3-甲基六氫鄰苯二甲酸酐、4-甲基六氫鄰苯二甲酸酐、3-乙基六氫鄰苯二甲酸酐、4-乙基六氫鄰苯二甲酸酐、四氫鄰苯二甲酸酐、3-甲基四氫鄰苯二甲酸酐、4-甲基四氫鄰苯二甲酸酐、3-乙基四氫鄰苯二甲酸酐、及4-乙基四氫鄰苯二甲酸酐等。
又,藉由使丙烯酸系樹脂(a-IV)所具有之來自丙烯酸或甲基丙烯酸等不飽和羧酸之結構單元與具有環氧基及不飽和雙鍵之化合物發生反應,而可向丙烯酸系樹脂(a-IV)導入不飽和雙鍵。作為具有環氧基及不飽和雙鍵之化合物,例如可使用(甲基)丙烯酸縮水甘油酯或後文中敍述之式(a-4-1a)~(a-4-1o)所表示之化合物。
作為R
a10,較佳為烷基、芳基、環烷基、聚環烷基、環烷基烷基、聚環烷基烷基、芳烷基或雜環基,該等基可被鹵素原子、羥基、烷基或雜環基取代,該等基可與氧原子鍵結形成環氧基。又,於該等基包含伸烷基部分之情形時,伸烷基部分可被醚鍵、硫醚鍵、酯鍵中斷。
於烷基為直鏈狀或支鏈狀者之情形時,其碳原子數較佳為1以上20以下,更佳為1以上15以下,尤佳為1以上10以下。作為較佳之烷基之例,可例舉:甲基、乙基、正丙基、異丙基、正丁基、異丁基、第二丁基、第三丁基、正戊基、異戊基、第二戊基、第三戊基、正己基、正庚基、正辛基、異辛基、第二辛基、第三辛基、正壬基、異壬基、正癸基、異癸基等。
於環烷基、聚環烷基、環烷基烷基、聚環烷基烷基、及除該等基以外之含脂環式基之基中,作為該等基中包含之脂環式基之較佳例,可例舉:環戊基、及環己基等單環之脂環式基或金剛烷基、降𦯉基、異𦯉基、三環壬基、三環癸基、四環十二烷基、二環-[2.1.1]-己基、二環-[2.2.1]-庚基、二環-[2.2.2]-辛基、二環-[3.3.0]-辛基、二環-[4.3.0]-壬基、及二環-[4.4.0]-癸基等聚環烷基。
作為式(a4-1)所表示之具有環烷基、聚環烷基、環烷基烷基、聚環烷基烷基、及除該等基以外之含脂環式基之基作為R
a10之化合物之較佳例,可例舉下述式(a-4-1a)~(a-4-1h)所表示之化合物。該等之中,較佳為下述式(a-4-1c)~(a-4-1h)所表示之化合物,更佳為下述式(a-4-1c)或下述式(a-4-1d)所表示之化合物。
上述式中,R
a20表示氫原子或甲基,R
a21表示單鍵或碳原子數1~6之2價脂肪族飽和烴基,R
a22表示氫原子或碳原子數1~5之烷基。作為R
a21,較佳為單鍵、直鏈狀或支鏈狀之伸烷基,例如:亞甲基、伸乙基、伸丙基、四亞甲基、乙基伸乙基、五亞甲基、六亞甲基。作為R
a22,例如較佳為甲基、乙基。
較佳為含有包含來自聚環烷基(甲基)丙烯酸酯(A-1)之結構單元及/或來自(甲基)丙烯酸芳烷基酯(A-2)之結構單元之丙烯酸系樹脂。於丙烯酸系樹脂包含來自(A-1)之結構單元之情形時,就本發明之效果之方面而言,較佳為例如包含來自作為上述式(a-4-1c)~(a-4-1h)之任一者所表示之具有單鍵作為R
a21之化合物的(A-1)之結構單元。
於式(a-4-1)所表示之化合物具有含環氧基之鏈狀基作為R
a10之情形時,作為式(a-4-1)所表示之化合物之具體例,可例舉:(甲基)丙烯酸縮水甘油酯、(甲基)丙烯酸2-甲基縮水甘油酯、(甲基)丙烯酸3,4-環氧基丁酯、(甲基)丙烯酸6,7-環氧基庚酯等(甲基)丙烯酸環氧烷基酯類。
又,式(a-4-1)所表示之化合物可為含脂環式環氧基之(甲基)丙烯酸酯。構成脂環式環氧基之脂環式基可為單環,亦可為多環。作為單環之脂環式基,可例舉環戊基、環己基等環烷基。又,作為多環之脂環式基,可例舉降𦯉基、異𦯉基、三環壬基、三環癸基、四環十二烷基等聚環烷基。
作為於式(a-4-1)所表示之化合物為包含脂環式環氧基之(甲基)丙烯酸酯之情形時之具體例,例如可例舉下述式(a-4-1i)~(a-4-1m)所表示之化合物。
又,作為式(a-4-1)所表示之化合物之其他具體例,可例舉:(甲基)丙烯酸、(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸2-羥基-3-苯氧基丙酯、琥珀酸2-(甲基)丙烯醯氧基乙酯、鄰苯二甲酸2-(甲基)丙烯醯氧基乙酯、鄰苯二甲酸2-(甲基)丙烯醯氧基乙基-2-羥基乙酯、酸性磷酸單2-(甲基)丙烯醯氧基乙酯、酸性磷酸二2-(甲基)丙烯醯氧基乙酯、(甲基)丙烯酸2-羥基丁酯、六氫鄰苯二甲酸2-(甲基)丙烯醯氧基乙酯、二(甲基)丙烯酸甘油酯、(甲基)丙烯酸2-羥基-3苯氧基丙酯、雙酚A二縮水甘油醚(甲基)丙烯酸加成物、O-苯基苯酚縮水甘油醚(甲基)丙烯酸酯、1,4-丁二醇二縮水甘油醚二(甲基)丙烯酸酯、1,6-己二醇二縮水甘油醚二(甲基)丙烯酸酯、二丙二醇二縮水甘油醚二(甲基)丙烯酸酯、季戊四醇聚縮水甘油醚(甲基)丙烯酸酯、1,3-丙二醇二縮水甘油醚(甲基)丙烯酸酯、環己烷二甲醇二縮水甘油醚(甲基)丙烯酸酯、1,6-己二醇二縮水甘油醚(甲基)丙烯酸酯、甘油聚縮水甘油醚(甲基)丙烯酸酯、乙二醇二縮水甘油醚(甲基)丙烯酸酯、聚乙二醇二縮水甘油醚(甲基)丙烯酸酯、二丙二醇二縮水甘油醚(甲基)丙烯酸酯、聚丙二醇二縮水甘油醚(甲基)丙烯酸酯、(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸1-丙烯醯氧基乙酯、1,2,3-丙三醇1,3-二(甲基)丙烯酸酯、(甲基)丙烯酸2-羧基乙酯等(甲基)丙烯酸系單體。
作為提供丙烯酸系樹脂(a-IV)中之結構單元之化合物,就本發明之效果之方面而言,較佳可例舉:(甲基)丙烯酸、琥珀酸2-(甲基)丙烯醯氧基乙酯、鄰苯二甲酸2-(甲基)丙烯醯氧基乙酯、鄰苯二甲酸2-(甲基)丙烯醯氧基乙基-2-羥基乙酯、(甲基)丙烯酸碳原子數1~5之烷基酯、(甲基)丙烯酸聚環烷基酯(A-1)或(甲基)丙烯酸芳烷基酯(A-2)。作為上述(A-1),例如可例舉上述式(a-4-1c)~(a-4-1h)之任一者所表示之具有單鍵作為R
a21之化合物,作為上述(A-2),例如可例舉(甲基)丙烯酸苄酯。
於丙烯酸系樹脂(a-IV)中,來自上述較佳之化合物之結構單元之量於不阻礙本發明之目的之範圍內並無特別限制,相對於全部結構單元之量,例如為10質量%以上,較佳為30質量%以上。上限只要適當設定即可,例如可為100質量%以下,亦可為90質量%以下。
又,丙烯酸系樹脂(a-IV)可為使除(甲基)丙烯酸酯以外之單體聚合而成者。作為此種單體,可例舉:(甲基)丙烯醯胺類、不飽和羧酸類、烯丙基化合物、乙烯醚類、乙烯酯類、苯乙烯類等,較佳為乙烯醚類或苯乙烯類。該等單體可單獨使用或將2種以上加以組合而使用。
作為(甲基)丙烯醯胺類,可例舉:(甲基)丙烯醯胺、N-烷基(甲基)丙烯醯胺、N-芳基(甲基)丙烯醯胺、N,N-二烷基(甲基)丙烯醯胺、N,N-芳基(甲基)丙烯醯胺、N-甲基-N-苯基(甲基)丙烯醯胺、N-羥基乙基-N-甲基(甲基)丙烯醯胺等。
作為不飽和羧酸類,可例舉:丁烯酸等單羧酸;馬來酸、富馬酸、檸康酸、中康酸、伊康酸等二羧酸;該等二羧酸之酐等。
作為烯丙基化合物,可例舉:乙酸烯丙酯、己酸烯丙酯、辛酸烯丙酯、月桂酸烯丙酯、棕櫚酸烯丙酯、硬脂酸烯丙酯、苯甲酸烯丙酯、乙醯乙酸烯丙酯、乳酸烯丙酯等烯丙酯類;烯丙氧基乙醇等。
作為乙烯醚類,可例舉:己基乙烯醚、辛基乙烯醚、癸基乙烯醚、乙基己基乙烯醚、甲氧基乙基乙烯醚、乙氧基乙基乙烯醚、氯乙基乙烯醚、1-甲基-2,2-二甲基丙基乙烯醚、2-乙基丁基乙烯醚、羥基乙基乙烯醚、二乙二醇乙烯醚、二甲基胺基乙基乙烯醚、二乙基胺基乙基乙烯醚、丁基胺基乙基乙烯醚、苄基乙烯醚、四氫呋喃甲基乙烯醚等烷基乙烯醚;乙烯基苯基醚、乙烯基甲苯基醚、乙烯基氯苯基醚、乙烯基-2,4-二氯苯基醚、乙烯基萘基醚、乙烯基蒽基醚等乙烯基芳基醚等。
作為乙烯酯類,可例舉:丁酸乙烯酯、異丁酸乙烯酯、三甲基乙酸乙烯酯、二乙基乙酸乙烯酯、戊酸乙烯酯、己酸乙烯酯、氯乙酸乙烯酯、二氯乙酸乙烯酯、甲氧基乙酸乙烯酯、丁氧基乙酸乙烯酯、乙烯基乙酸苯酯、乙醯乙酸乙烯酯、乳酸乙烯酯、乙烯基丁酸β-苯基酯、苯甲酸乙烯酯、水楊酸乙烯酯、氯苯甲酸乙烯酯、四氯苯甲酸乙烯酯、萘甲酸乙烯酯等。
作為苯乙烯類,可例舉:苯乙烯;甲基苯乙烯、二甲基苯乙烯、三甲基苯乙烯、乙基苯乙烯、二乙基苯乙烯、異丙基苯乙烯、丁基苯乙烯、己基苯乙烯、環己基苯乙烯、癸基苯乙烯、苄基苯乙烯、氯甲基苯乙烯、三氟甲基苯乙烯、乙氧基甲基苯乙烯、乙醯氧基甲基苯乙烯等烷基苯乙烯;甲氧基苯乙烯、4-甲氧基-3-甲基苯乙烯、二甲氧基苯乙烯等烷氧基苯乙烯;氯苯乙烯、二氯苯乙烯、三氯苯乙烯、四氯苯乙烯、五氯苯乙烯、溴苯乙烯、二溴苯乙烯、碘苯乙烯、氟苯乙烯、三氟苯乙烯、2-溴-4-三氟甲基苯乙烯、4-氟-3-三氟甲基苯乙烯等鹵苯乙烯等。
本發明之金屬氧化物膜形成性組合物包含金屬氧化物奈米團簇,故即使基材為丙烯酸系樹脂亦可賦予基板加工所需之耐蝕刻性,但就耐蝕刻性之提昇等方面而言,可追加使用包含芳香環之聚合物、包含芳香環之非聚合物或該等兩者作為基材。
作為包含芳香環之非聚合物,可例舉具有聯苯茀骨架、聯萘茀骨架、亞甲基二萘骨架、四苯并萘骨架或杯芳烴骨架之化合物(X)。該等化合物可具有取代基,作為取代基之例,就硬化性等方面而言,較佳為丙烯醯基、甲基丙烯醯基、乙烯基氧基、苯乙烯基、烯丙基、炔丙基、二縮水甘油基胺基、二炔丙基胺基等聚合性基或包含上述聚合性基之有機基。
作為包含芳香環之聚合物,可例舉:
・具有構成化合物(X)之骨架作為重複結構之樹脂、
・具有苯骨架、萘骨架、聯苯骨架、及/或蒽骨架作為重複結構之樹脂、
・化合物(X)之縮合體
等。縮合體係藉由使化合物(X)與選自由醛類、具有烷氧基之化合物類、具有烷醯氧基之化合物類、三㗁烷類、及茀酮類所組成之群中之1種以上發生作用而獲得。又,作為包含芳香環之聚合物,可使用公知之酚醛清漆樹脂等。
[酚醛清漆樹脂(a-II)]
作為酚醛清漆樹脂(a-II),可使用自先前以來感光性組合物中調配之各種酚醛清漆樹脂。作為酚醛清漆樹脂(a-II),較佳為藉由使具有酚性羥基之芳香族化合物(以下簡稱為「酚類」)與醛類於酸觸媒下進行加成縮合而獲得者。
(酚類)
作為製作酚醛清漆樹脂(a-II)時使用之酚類,例如可例舉:苯酚;鄰甲酚、間甲酚、對甲酚等甲酚類;2,3-二甲苯酚、2,4-二甲苯酚、2,5-二甲苯酚、2,6-二甲苯酚、3,4-二甲苯酚、3,5-二甲苯酚等二甲苯酚類;鄰乙基苯酚、間乙基苯酚、對乙基苯酚等乙基苯酚類;2-異丙基苯酚、3-異丙基苯酚、4-異丙基苯酚、鄰丁基苯酚、間丁基苯酚、對丁基苯酚、以及對第三丁基苯酚苯酚等烷基苯酚類;2,3,5-三甲基苯酚、及3,4,5-三甲基苯酚等三烷基苯酚類;間苯二酚、鄰苯二酚、對苯二酚、對苯二酚單甲醚、鄰苯三酚、及間苯三酚等多酚類;烷基間苯二酚、烷基鄰苯二酚、及烷基對苯二酚等烷基多酚類(任一烷基均為碳原子數1以上4以下);α-萘酚;β-萘酚;羥基聯苯;以及雙酚A等。該等酚類可單獨使用,亦可將2種以上加以組合而使用。
(醛類)
作為製作酚醛清漆樹脂(a-II)時使用之醛類,例如可例舉:甲醛、多聚甲醛、糠醛、苯甲醛、硝基苯甲醛、及乙醛等。該等醛類可單獨使用,亦可將2種以上加以組合而使用。
(酸觸媒)
作為製作酚醛清漆樹脂(a-II)時使用之酸觸媒,例如可例舉:鹽酸、硫酸、硝酸、磷酸、及亞磷酸等無機酸類;甲酸、草酸、乙酸、二乙基硫酸、及對甲苯磺酸等有機酸類;以及乙酸鋅等金屬鹽類等。該等酸觸媒可單獨使用,亦可將2種以上加以組合而使用。
基材之使用量並無特別限制,相對於金屬氧化物膜形成性組合物中之除溶劑以外之成分之總計,例如為0.5~35質量%,較佳為1~25質量%,更佳為2~15質量%。若基材之使用量為上述範圍內,則有機成分質量之比率不會變得過高,其結果為,獲得之金屬氧化物膜於400℃以下之低溫下進行加熱時體積收縮易得到抑制。
於上述金屬氧化物膜形成性組合物之固形物成分中,上述金屬氧化物奈米團簇相對於上述金屬氧化物奈米團簇與上述基材之總計之質量比例如為45質量%以上,較佳為50質量%以上,更佳為60質量%以上,進而更佳為65質量%以上。上述質量比之上限例如為95質量%以下,較佳為90質量%以下。
[溶劑]
為了調整塗佈性或黏度,本發明之金屬氧化物膜形成性組合物含有溶劑。作為溶劑,典型而言,使用有機溶劑。有機溶劑之種類只要可使金屬氧化物膜形成性組合物中包含之成分均勻地溶解或分散,則並無特別限制。
作為可用作溶劑之有機溶劑之較佳例,可例舉:乙二醇單甲醚、乙二醇單乙醚、乙二醇正丙醚、乙二醇單正丁醚、二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇單正丙醚、二乙二醇單正丁醚、三乙二醇單甲醚、三乙二醇單乙醚、丙二醇單甲醚、丙二醇單乙醚、丙二醇單正丙醚、丙二醇單正丁醚、二丙二醇單甲醚、二丙二醇單乙醚、二丙二醇單正丙醚、二丙二醇單正丁醚、三丙二醇單甲醚、三丙二醇單乙醚等(聚)伸烷基乙二醇單烷基醚類;乙二醇單甲醚乙酸酯、乙二醇單乙醚乙酸酯、二乙二醇單甲醚乙酸酯、二乙二醇單乙醚乙酸酯、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯等(聚)伸烷基乙二醇單烷基醚乙酸酯類;二乙二醇二甲醚、二乙二醇甲基乙基醚、二乙二醇二乙醚、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-甲基碳酸甲酯、乙酸3-甲基-3-甲氧基丁酯、丙酸3-甲基-3-甲氧基丁酯、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、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-側氧丁酸乙酯等其他酯類;甲苯、二甲苯等芳香族烴類;N-甲基吡咯啶酮、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺等醯胺類等。該等有機溶劑可單獨使用或將2種以上加以組合而使用。
本發明之金屬氧化物膜形成性組合物中之溶劑之使用量並無特別限制。就金屬氧化物膜形成性組合物之塗佈性方面等而言,溶劑之使用量相對於金屬氧化物膜形成性組合物整體,例如為30~99.9質量%,較佳為50~98質量%。
[界面活性劑]
為了提昇塗佈性、消泡性、調平性等,本發明之金屬氧化物膜形成性組合物可進而含有界面活性劑(表面調整劑)。界面活性劑可單獨使用1種,亦可併用2種以上。作為界面活性劑,例如可例舉:矽酮系界面活性劑、氟系界面活性劑。
作為矽酮系界面活性劑,具體而言可例舉:BYK-077、BYK-085、BYK-300、BYK-301、BYK-302、BYK-306、BYK-307、BYK-310、BYK-320、BYK-322、BYK-323、BYK-325、BYK-330、BYK-331、BYK-333、BYK-335、BYK-341、BYK-344、BYK-345、BYK-346、BYK-348、BYK-354、BYK-355、BYK-356、BYK-358、BYK-361、BYK-370、BYK-371、BYK-375、BYK-380、BYK-390(BYK Chemie公司製造)等。
作為氟系界面活性劑,具體而言,可例舉:F-114、F-177、F-410、F-411、F-450、F-493、F-494、F-443、F-444、F-445、F-446、F-470、F-471、F-472SF、F-474、F-475、F-477、F-478、F-479、F-480SF、F-482、F-483、F-484、F-486、F-487、F-172D、MCF-350SF、TF-1025SF、TF-1117SF、TF-1026SF、TF-1128、TF-1127、TF-1129、TF-1126、TF-1130、TF-1116SF、TF-1131、TF-1132、TF-1027SF、TF-1441、TF-1442(DIC公司製造);Polyfox系列之PF-636、PF-6320、PF-656、PF-6520(OMNOVA公司製造)等。
界面活性劑之使用量並無特別限制,就金屬氧化物膜形成性組合物之塗佈性、消泡性、調平性方面等而言,相對於金屬氧化物膜形成性組合物中之除溶劑以外之成分之總計,例如為0.01~0.15質量%,較佳為0.05~0.1質量%。
[其他成分]
本發明之金屬氧化物膜形成性組合物中可視需要含有分散劑、熱聚合抑制劑、消泡劑、矽烷偶合劑、著色劑(顏料、染料)、無機填料、有機填料、交聯劑、酸產生劑等添加劑。任一添加劑均可使用先前公知者。作為界面活性劑,可例舉:陰離子系、陽離子系、非離子系等化合物,作為熱聚合抑制劑,可例舉:氫醌、氫醌單乙醚等,作為消泡劑,可例舉:矽酮系、氟系化合物等。
本發明之金屬氧化物膜形成性組合物之製造方法並無特別限制,例如可例舉於溶劑之存在下利用封端劑對金屬氧化物奈米團簇進行處理之後,向獲得之漿料中添加基材、任意溶劑、任意界面活性劑、及任意其他成分之方法。具體而言,本發明之金屬氧化物膜形成性組合物例如可以後文中敍述之實施例所示之方式進行製造。
<金屬氧化物膜之製造方法>
本發明之金屬氧化物膜之製造方法包括形成包含本發明之金屬氧化物膜形成性組合物之塗膜之塗膜形成步驟及對上述塗膜進行加熱之加熱步驟。
上述塗膜例如可藉由於半導體基板等基板上塗佈金屬氧化物膜形成性組合物而形成。作為塗佈方法,可例舉使用輥式塗佈機、反向塗佈機、棒式塗佈機等接觸轉印型塗佈裝置或旋轉器(旋轉式塗佈裝置、旋轉塗佈機)、浸漬塗佈機、噴霧塗佈機、狹縫式塗佈機、淋幕式平面塗裝機等非接觸型塗佈裝置之方法。又,可將金屬氧化物膜形成性組合物之黏度調整為適當之範圍之後,藉由噴墨法、網版印刷法等印刷法進行金屬氧化物膜形成性組合物之塗佈,形成經圖案化而形成所需形狀之塗膜。
作為基板,較佳為包含金屬膜、金屬碳化膜、金屬氧化膜、金屬氮化膜或金屬氧化氮化膜者。構成上述基板之金屬可例舉:矽、鈦、鎢、鉿、鋯、鉻、鍺、銅、鋁、銦、鎵、砷、鈀、鐵、鉭、銥、鉬或該等之合金等,較佳為包含矽、鍺、鎵。又,基板表面可具有凹凸形狀,亦可為凹凸形狀經圖案化而形成之有機系材料。
其次,視需要將溶劑等揮發成分去除而使塗膜乾燥。乾燥方法並無特別限制,例如可例舉利用加熱板於80℃以上140℃以下,較佳為90℃以上130℃以下之溫度下以60秒以上150秒以下之範圍內之時間進行乾燥之方法。可於利用加熱板進行加熱之前,使用真空乾燥裝置(VCD)於室溫下進行減壓乾燥。
以此方式形成塗膜之後,對塗膜進行加熱。進行加熱時之溫度並無特別限制,較佳為400℃以上,更佳為420℃以上,進而更佳為430℃以上。上限只要適當設定即可,例如可為600℃以下,就控制乾式蝕刻時之蝕刻速率方面或面內均勻性之方面而言,較佳為550℃以下。典型而言,加熱時間較佳為30秒以上150秒以下,更佳為60秒以上120秒。加熱步驟可於單一之加熱溫度下進行,亦可包含加熱溫度不同之複數個階段。
以如上方式形成之金屬氧化物膜例如可較佳地用作金屬硬罩或圖案反轉用材料。
<降低金屬氧化物膜之體積收縮率之方法>
降低本發明之金屬氧化物膜之體積收縮率之方法如上所述,換言之,係降低形成包含金屬氧化物膜形成性組合物之塗膜,並對上述塗膜進行加熱而獲得的金屬氧化物膜之體積收縮率之方法,包括以使上述金屬氧化物膜形成性組合物成為本發明之金屬氧化物膜形成性組合物之方式構成。藉由該方法,可降低於400℃以下進行加熱時金屬氧化物膜之體積收縮率,可維持於400℃以上、尤其是450℃以上之溫度下進行加熱時之面內均勻性。本發明之金屬氧化物膜形成性組合物如上所述。
[實施例]
以下藉由實施例對本發明進行進一步詳細說明,本發明並不受限於該等實施例。
[金屬氧化物膜形成性組合物之製備]
以下各分散液之製備係參照日本專利特開2018-193481號公報之段落[0223]之記載進行。
・Z-2分散液之製備
基於日本專利特開2018-193481號公報之段落[0223]之記載,對冷卻至室溫獲得之ZrO
2之漿料進行離心分離而獲得濕濾餅A。將濕濾餅A之重量之0.2倍之2-丙烯醯氧基乙基琥珀酸(參照下述式)添加於濕濾餅A中進行攪拌。再沈澱之後,藉由離心分離而獲得濕濾餅B。對濕濾餅B進行一晩減壓乾燥,獲得粉末。以成為固形物成分濃度48質量%之方式向獲得乾燥粉末中添加丙二醇單甲醚乙酸酯(以下稱為「PGMEA」)進行再分散之後,進行過濾,從而獲得Z-2分散液。
・對Z-2分散液之TG-DTA測定
將Z-2分散液放置於鉑製樣品盤,進行TG-DTA(Thermogravimetric-differential thermal analysis,熱重-差熱分析)測定。將以10℃/min自室溫升溫至200℃,於200℃下保持5 min時之質量設為固形物成分質量。其次,將以10℃/min自200℃升溫至710℃,達到710℃時之質量設為無機成分質量。根據該等測定結果,藉由式:有機成分重量=固形物成分重量-無機成分重量而算出有機成分重量,藉由式:無機成分質量/(無機成分質量+有機成分質量)算出無機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%),結果為77質量%。又,藉由式:有機成分質量/(無機成分質量+有機成分質量)而算出有機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%),結果為23質量%。
・Z-2分散液中包含之金屬氧化物奈米團簇之尺寸之測定
使用Z-2分散液作為試樣,藉由X射線繞射裝置(SmartLab,Rigaku股份有限公司製造)進行XRD(X ray diffraction,X射線繞射)測定。利用附屬軟體PDXL對獲得之結果進行解析,利用Halder-Wagner法求出金屬氧化物奈米團簇之尺寸(微晶尺寸),結果為8 nm。
・Z-1分散液之製備
除將用以獲得ZrO
2之漿料之水與異丙氧化鋯(IV)異丙醇(Zr(OCH(CH
3)
2)
4(HOCH(CH
3)
2)之莫耳比改變為1:3以外,以與上述「Z-2分散液之製備」相同之方式進行操作,從而獲得Z-1分散液。
・對Z-1分散液之TG-DTA測定
除使用Z-1分散液代替Z-2分散液以外,以與上述「對Z-2分散液之TG-DTA測定」相同之方式進行操作,結果為,無機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%)算出為73質量%,有機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%)算出為27質量%。
・Z-1分散液中包含之金屬氧化物奈米團簇之尺寸之測定
除使用Z-1分散液代替Z-2分散液以外,以與上述「Z-2分散液中包含之金屬氧化物奈米團簇之尺寸之測定」相同之方式進行操作,結果為,金屬氧化物奈米團簇之尺寸(微晶尺寸)為2.5 nm。
・Z-3分散液之製備
除將2-丙烯醯氧基乙基琥珀酸改變為2-丙烯醯氧基乙基鄰苯二甲酸以外,以與上述「Z-1分散液之製備」相同之方式進行操作,從而獲得Z-3分散液。
・對Z-3分散液之TG-DTA測定
除使用Z-3分散液代替Z-1分散液以外,以與上述「對Z-1分散液之TG-DTA測定」相同之方式進行操作,結果為,無機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%)算出為77質量%,有機成分質量相對於無機成分質量與有機成分質量之總計之比率(質量%)算出為23質量%。
・Z-3分散液中包含之金屬氧化物奈米團簇之尺寸之測定
除使用Z-3分散液代替Z-1分散液以外,以與上述「Z-1分散液中包含之金屬氧化物奈米團簇之尺寸之測定」相同之方式進行操作,結果為,金屬氧化物奈米團簇之尺寸(微晶尺寸)為2.5 nm。
・樹脂液之製備
將50質量份包含來自甲基丙烯酸之結構單元20莫耳%及來自苯乙烯之結構單元80莫耳%之丙烯酸系樹脂(新中村化學公司製造,NCF-3(商品名),Mw=10000)與50質量份甲氧基丙酮加以混合,從而獲得樹脂液。
・界面活性劑液之製備
將1質量份市售之界面活性劑(BYK Chemie公司製造,BYK-333(商品名))與99質量份PGMEA加以混合,從而獲得界面活性劑液。
以表1所示之比率(單位:質量份)向Z-1分散液、Z-2分散液或Z-3分散液中首先添加樹脂液,其次添加界面活性劑液,最後添加溶劑PGMEA,進行攪拌,並利用Φ0.2 μm之膜濾器進行過濾,從而獲得組合物。再者,於表1中,括弧內之數字表示固形物成分之比率(單位:質量份)。
[無機成分質量之比率]
於表1中,「無機成分質量之比率」係針對組合物之固形物成分,表示無機成分質量相對於無機成分質量與有機成分質量之總計之比率。具體而言,算出Z-1分散液、Z-2分散液或Z-3分散液之無機成分質量相對於Z-1分散液、Z-2分散液或Z-3分散液之固形物成分質量、樹脂液中之丙烯酸系樹脂之質量及界面活性劑液中之界面活性劑之質量之總計之比率(質量%)。將結果示於表1。
[表1]
實施例1 | 實施例2 | 實施例3 | 比較例1 | |
Z-1分散液 金屬氧化物奈米團簇之尺寸:2.5 nm | 2 (1.1) | 1.44 (0.792) | ||
Z-2分散液 金屬氧化物奈米團簇之尺寸:8 nm | 2 (1.1) | |||
Z-3分散液 金屬氧化物奈米團簇之尺寸:2.5 nm | 2 (1.1) | |||
樹脂液 | 0.08 (0.04) | 0.64 (0.32) | 0.08 (0.04) | 0.08 (0.04) |
界面活性劑液 | 0.08 (0.0008) | 0.08 (0.0008) | 0.08 (0.0008) | 0.08 (0.0008) |
溶劑(PMGEA) | 17.84 | 17.84 | 17.84 | 17.84 |
封端劑之種類﹡ | A | A | B | A |
無機成分質量之比率(質量%) | 70 | 50 | 70 | 70 |
﹡A:2-丙烯醯氧基乙基琥珀酸 B:2-丙烯醯氧基乙基鄰苯二甲酸 |
[金屬氧化物膜之製作]
向6英吋之矽晶圓上滴加組合物,花費2秒加速至500 rpm之後,以500 rpm進行10秒鐘旋轉塗佈。其後,使用加熱板,於100℃下進行120秒鐘預烘烤,並於下述各焙燒溫度下進行90秒鐘後烘烤,從而獲得金屬氧化物膜。再者,下述「室溫」表示於室溫下放置90秒鐘,意為實際上不進行後烘烤。
焙燒溫度:室溫、200℃、250℃、300℃、350℃、400℃、450℃、500℃、600℃
[膜厚之測定]
利用SEM(Scanning electron microscope,掃描式電子顯微)觀察獲得之金屬氧化物膜之剖面,並對膜厚進行測定。將結果示於表2。再者,於表2中,於上述「金屬氧化物膜之製作」中,將焙燒溫度設定為室溫之情形時之膜厚設為100%來表示其他焙燒溫度時之膜厚。
[表2]
焙燒溫度 | 實施例1 | 實施例2 | 實施例3 | 比較例1 |
室溫 | 100% | 100% | 100% | 100% |
200 | 98% | 98% | 98% | 95% |
250 | 96% | 92% | 92% | 85% |
300 | 95% | 92% | 88% | 77% |
350 | 93% | 86% | 86% | 77% |
400 | 87% | 81% | 80% | 74% |
450 | 76% | 68% | 73% | 70% |
500 | 67% | 64% | 68% | 66% |
600 | 65% | 63% | 63% | 62% |
由表2可知,確認實施例中於400℃以下進行加熱時體積收縮得到抑制,與此相對,比較例中於400℃以下進行加熱時體積收縮顯著。
Claims (8)
- 一種金屬氧化物膜形成性組合物,其係含有金屬氧化物奈米團簇、封端劑、基材及溶劑者,且 上述金屬氧化物奈米團簇之尺寸為5 nm以下, 上述封端劑包含選自由烷氧基矽烷、酚、醇、羧酸、及羧醯鹵所組成之群中之至少1種, 於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。
- 如請求項1之金屬氧化物膜形成性組合物,其中於上述金屬氧化物膜形成性組合物之固形物成分中,上述金屬氧化物奈米團簇相對於上述金屬氧化物奈米團簇與上述封端劑之總計之質量比為50質量%以上。
- 如請求項1或2之金屬氧化物膜形成性組合物,其進而含有界面活性劑。
- 如請求項1或2之金屬氧化物膜形成性組合物,其中上述金屬氧化物奈米團簇中包含之金屬為選自由鋅、釔、鉿、鋯、鑭、鈰、釹、釓、鈥、鎦、鉭、鈦、矽、鋁、銻、錫、銦、鎢、銅、釩、鉻、鈮、鉬、釕、銠、錸、銥、鍺、鎵、鉈、及鎂所組成之群中之至少1種。
- 一種金屬氧化物膜之製造方法,其包括: 形成包含如請求項1至4中任一項之金屬氧化物膜形成性組合物之塗膜之塗膜形成步驟;及 對上述塗膜進行加熱之加熱步驟。
- 如請求項5之製造方法,其中上述加熱步驟中之加熱溫度為400℃以上。
- 如請求項5或6之製造方法,其中上述金屬氧化物膜為金屬硬罩。
- 一種降低金屬氧化物膜之體積收縮率之方法,該金屬氧化物膜係形成包含金屬氧化物膜形成性組合物之塗膜,並對上述塗膜進行加熱而獲得者, 上述方法包括以含有金屬氧化物奈米團簇、封端劑、基材及溶劑之方式構成上述金屬氧化物膜形成性組合物, 上述金屬氧化物奈米團簇之尺寸為5 nm以下, 上述封端劑包含選自由烷氧基矽烷、酚、醇、羧酸、及羧醯鹵所組成之群中之至少1種, 於上述金屬氧化物膜形成性組合物之固形物成分中,無機成分質量相對於無機成分質量與有機成分質量之總計之比率為25質量%以上。
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