JP5405031B2 - シリカ質膜の製造に用いる浸漬用溶液およびそれを用いたシリカ質膜の製造法 - Google Patents
シリカ質膜の製造に用いる浸漬用溶液およびそれを用いたシリカ質膜の製造法 Download PDFInfo
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- JP5405031B2 JP5405031B2 JP2008056198A JP2008056198A JP5405031B2 JP 5405031 B2 JP5405031 B2 JP 5405031B2 JP 2008056198 A JP2008056198 A JP 2008056198A JP 2008056198 A JP2008056198 A JP 2008056198A JP 5405031 B2 JP5405031 B2 JP 5405031B2
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- Prior art keywords
- dipping
- film
- substrate
- siliceous film
- solution
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- 238000007654 immersion Methods 0.000 title claims description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 229920001709 polysilazane Polymers 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 46
- 238000007598 dipping method Methods 0.000 claims description 42
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000002904 solvent Substances 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- -1 polyoxyethylene Polymers 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 150000005215 alkyl ethers Chemical class 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 26
- 238000002955 isolation Methods 0.000 description 23
- 235000012239 silicon dioxide Nutrition 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- 229910052581 Si3N4 Inorganic materials 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000005530 etching Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229920002120 photoresistant polymer Polymers 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- 150000002430 hydrocarbons Chemical group 0.000 description 4
- 230000010354 integration Effects 0.000 description 4
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 230000003449 preventive effect Effects 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- AFABGHUZZDYHJO-UHFFFAOYSA-N 2-Methylpentane Chemical compound CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 2
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- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
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- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- CFJYNSNXFXLKNS-UHFFFAOYSA-N p-menthane Chemical compound CC(C)C1CCC(C)CC1 CFJYNSNXFXLKNS-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VIDOPANCAUPXNH-UHFFFAOYSA-N 1,2,3-triethylbenzene Chemical compound CCC1=CC=CC(CC)=C1CC VIDOPANCAUPXNH-UHFFFAOYSA-N 0.000 description 1
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
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- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000003282 alkyl amino group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005247 gettering Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- MMBMIVSDYYPRHH-UHFFFAOYSA-N hydrogen peroxide Chemical compound OO.OO MMBMIVSDYYPRHH-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- QWTDNUCVQCZILF-UHFFFAOYSA-N iso-pentane Natural products CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229930004008 p-menthane Natural products 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- QJMMCGKXBZVAEI-UHFFFAOYSA-N tris(trimethylsilyl) phosphate Chemical compound C[Si](C)(C)OP(=O)(O[Si](C)(C)C)O[Si](C)(C)C QJMMCGKXBZVAEI-UHFFFAOYSA-N 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
- C03C1/008—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/60—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/62—Nitrogen atoms
-
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1212—Zeolites, glasses
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2203/00—Production processes
- C03C2203/20—Wet processes, e.g. sol-gel process
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Wood Science & Technology (AREA)
- Ceramic Engineering (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Description
最先端デバイスでは回路の高密度化が進んでいるため、微細なトレンチ内部であっても均一な膜質を得ることができる新たなプロセスが望まれていた。
凹凸を有する基板の表面上に、ポリシラザン化合物を含んでなる組成物を塗布する塗布工程、
塗布済み基板を前記の浸漬用溶液に浸漬させる浸漬工程、および
浸漬後の基板を加熱処理してポリシラザン化合物をシリカ質膜に転化させる硬化工程
を含んでなることを特徴とするものである。
本発明における浸漬用溶液は、後述するシリカ質膜の製造過程において、ポリシラザン組成物塗布済み基板を焼成前に浸漬するのに用いるものである。一般に、ポリシラザン組成物を加熱焼成することにより酸化反応が起こり、シリカ質膜が形成される。ここで、焼成前に本発明による浸漬用溶液で処理することにより、例えば基板上に形成された溝に充填されたポリシラザン組成物も表面部と同様に酸化され、均一なシリカ質膜が形成される。
過酸化水素は、一般的な酸化剤としてよく知られているものである。しかしながら、本発明においては、ポリシラザンの酸化、すなわちシリカ質膜の形成はもっぱら焼成によって達成されるのであり、浸漬用溶液中の過酸化水素によってポリシラザンの酸化が支配されるわけではない。むしろ、ポリシラザン組成物から形成される塗膜全体を均一に酸化させるために補助的に作用するものである。
本発明による浸漬用溶液は気泡付着防止剤を含んでなる。本発明において、浸漬用溶液中における気泡付着防止剤は、基板を浸漬用溶液に浸漬したときに付着する気泡を減少させる作用がある。浸漬用溶液中において基板に付着した気泡は、その後浸漬用溶液から取り出された後にも残留し、結果的に基板の表面積を増大させる。表面積が大きいほど環境から混入するダストなどが付着しやすくなり、最終的には形成されるシリカ質膜の欠陥になる可能性がある。本発明においては気泡付着防止剤によりこの気泡の発生を減少させ、最終的なシリカ質膜の品質を改良させることができる。さらには、焼成後のシリカ質膜をさらに均一化させる作用もある。
本発明による浸漬用溶液は、溶媒を含んでなる。この溶媒は、前記の過酸化水素および気泡付着防止剤を均一に溶解させるものである。なお、前記気泡付着防止剤として用いられるアルコールは液体であり、一般的に溶媒としても作用し得るものであるが、本発明においてアルコールは溶媒に含めないものとする。すなわち、本発明における「溶媒」は前記アルコール以外のものから選択されるものである。
本発明によるシリカ質膜の製造法は、(a)凹凸を有する基板の表面上に、ポリシラザン化合物を含んでなる組成物を塗布し、(b)塗布済み基板を前記した浸漬用溶液に浸漬させ、さらに(c)浸漬後の基板を加熱処理してポリシラザン化合物を二酸化シリコン膜に転化させることを含んでなる。
用いられる基板の表面材質は特に限定されないが、例えばベアシリコン、必要に応じて熱酸化膜や窒化珪素膜を成膜したシリコンウェハー、などが挙げられる。本発明においては。このような基板に対して、最終的に製造しようとする半導体素子などに対応した溝や孔が設けられた、凹凸を有する基板が用いられる。これらは、トレンチ・アイソレーション構造や、コンタクトホールなどに対応した凹凸であり、必要に応じて種々のものが選択される。
(a)芳香族化合物、例えば、ベンゼン、トルエン、キシレン、エチルベンゼン、ジエチルベンゼン、トリメチルベンゼン、トリエチルベンゼン等、(b)飽和炭化水素化合物、例えばn−ペンタン、i−ペンタン、n−ヘキサン、i−ヘキサン、n−ヘプタン、i−ヘプタン、n−オクタン、i−オクタン、n−ノナン、i−ノナン、n−デカン、i−デカン等、(c)脂環式炭化水素化合物、例えばエチルシクロヘキサン、メチルシクロヘキサン、シクロヘキサン、シクロヘキセン、p−メンタン、デカヒドロナフタレン、ジペンテン、リモネン等、(d)エーテル類、例えばジプロピルエーテル、ジブチルエーテル、ジエチルエーテル、メチルターシャリーブチルエーテル(以下、MTBEという)、アニソール等、および(e)ケトン類、例えばメチルイソブチルケトン(以下、MIBKという)等。これらのうち、(b)飽和炭化水素化合物、(c)脂環式炭化水素化合物(d)エーテル類、および(e)ケトン類がより好ましい。
塗布済みの基板は、必要に応じて基板表面に形成された塗布膜から過剰の有機溶媒を除去(乾燥)するために予備加熱(プリベーク)したあと、前記した浸漬用溶液に浸漬される。予備加熱はポリシラザンを硬化させることが目的ではないため、一般に低温で短時間加熱することにより行われる。具体的には70〜150℃、好ましくは100〜150℃で、1〜10分、好ましくは3〜5分加熱することにより行われる。
浸漬工程のあと、基板は加熱処理され、表面のポリシラザン組成物が硬化してシリカ質膜に転化される。このとき、加熱処理は好ましくは水蒸気、酸素、またはその混合ガスを含む雰囲気中、すなわち酸化雰囲気中で行われる。本発明においては、特に加熱処理を酸素を含む雰囲気下で焼成することが好ましい。ここで、酸素の含有率は体積を基準として1%以上であることが好ましく、10%以上であることがより好ましい。ここで、本発明の効果を損なわない範囲で、雰囲気中に窒素やヘリウムなどの不活性ガスが混在していてもよい。
本発明を諸例を用いて説明すると以下の通りである。
浸漬用溶液処理なし 16.9%
浸漬用溶液処理あり 8.0%
全工程終了後の成膜された基板を、溝の長手方向に対して直角の方向で切断した後、0.5%wt.フッ化水素酸水溶液に23℃で30秒浸漬し、その後純水でよく洗浄してから乾燥させた。基板断面の溝部分をSEMにより50000倍で、断面に垂直な方向の仰角30度上方から溝最深部を観察してエッチング量を評価した。浸漬なしのものはトレンチ底部のエッチング量が多く、トレンチ内部が不均一であった。浸漬用溶液処理ありのものは、トレンチ底部のエッチング量が少なく、トレンチ内部が均一な膜が良質な膜であった。
前記と同様にして、TEG基板上にポリシラザン組成物を塗布し、プリベークした後、浸漬用溶液に浸漬し、浸漬開始から5分後の基板表面上の気泡数を計測した。ここで、浸漬用溶液としては、30%の過酸化水素と10%のエタノールを含むもの(実施例)と、エタノールを含まない、30%過酸化水素水(比較例)を用いた。得られた結果は表1に示す通りであった。
気泡付着を評価した後、浸漬後、および焼成後の実施例および比較例のTEG基板表面の欠陥数を表面欠陥検査計(KLA−2115(商品名)、KLAテンコール社製)により評価した。焼成は、400℃、80%水蒸気雰囲気下で30分の条件でおこなった。得られた結果は表1に示す通りであった。なお、このとき参照例として浸漬用溶液に浸漬しないものについても同様の評価を行った。
Claims (10)
- シリカ質膜の製造過程において、ポリシラザン組成物塗布済み基板を焼成前に浸漬させるための浸漬用溶液であって、過酸化水素と、アルコール、界面活性剤、およびその混合物からなる群から選択される気泡付着防止剤と、前記アルコールとは異なる溶媒とを含んでなる浸漬用溶液であって、前記浸漬用溶液全体に対する前記過酸化水素の含有量が30〜60重量%であることを特徴とする浸漬用溶液。
- 前記アルコールが、炭素数1〜3の飽和炭化水素の水素が1〜3個の水酸基で置換されたモノオール、ジオール、またはトリオールである、請求項1に記載の浸漬用溶液。
- 前記アルコールが、メタノール、エタノール、n−プロパノール、イソプロパノール、およびそれらの混合物からなる群から選択される、請求項1または2に記載の浸漬用溶液。
- 前記界面活性剤がノニオン性界面活性剤である、請求項1に記載の浸漬用溶液。
- 前記ノニオン性界面活性剤がポリオキシエチレンアルキルエーテルである、請求項4に記載の浸漬用溶液。
- 前記アルコールとは異なる溶媒が水である、請求項1〜5のいずれか1項に記載の浸漬用溶液。
- 凹凸を有する基板の表面上に、ポリシラザン化合物を含んでなる組成物を塗布する塗布工程、
塗布済み基板を請求項1〜6のいずれか1項に記載の浸漬用溶液に浸漬させる浸漬工程、および
浸漬後の基板を加熱処理してポリシラザン化合物をシリカ質膜に転化させる硬化工程
を含んでなることを特徴とする、シリカ質膜の製造法。 - 前記塗布工程と浸漬工程との間に、さらに基板を予備加熱する工程を含んでなる、請求項7に記載のシリカ質膜の製造法。
- 前記硬化工程における加熱処理を水蒸気濃度1%以上の不活性ガスまたは酸素雰囲気下で行う、請求項7または8に記載のシリカ質膜の製造法。
- 前記硬化工程における加熱処理を400℃以上1,200℃以下の温度で行う、請求項7〜9のいずれか1項に記載のシリカ質膜の製造法。
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EP09716895.9A EP2264744B1 (en) | 2008-03-06 | 2009-03-03 | Dipping solution for use in production of siliceous film and process for producing siliceous film using the dipping solution |
PCT/JP2009/053931 WO2009110449A1 (ja) | 2008-03-06 | 2009-03-03 | シリカ質膜の製造に用いる浸漬用溶液およびそれを用いたシリカ質膜の製造法 |
US12/919,782 US20110014796A1 (en) | 2008-03-06 | 2009-03-03 | Dipping solution for use in production of siliceous film and process for producing siliceous film using the dipping solution |
KR1020107022181A KR101623764B1 (ko) | 2008-03-06 | 2009-03-03 | 실리카질 막의 제조에 사용하는 침지용 용액 및 이를 사용한 실리카질 막의 제조법 |
CN200980107577XA CN101965629A (zh) | 2008-03-06 | 2009-03-03 | 用于制备硅质膜的浸渍溶液和使用所述浸渍溶液制备硅质膜的方法 |
TW098106921A TWI538884B (zh) | 2008-03-06 | 2009-03-04 | 氧化矽質膜的製造方法 |
US13/920,617 US8603923B2 (en) | 2008-03-06 | 2013-06-18 | Dipping solution for use in production of siliceous film and process for producing siliceous film using the dipping solution |
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KR20110116966A (ko) | 2011-10-26 |
US20130277808A1 (en) | 2013-10-24 |
CN101965629A (zh) | 2011-02-02 |
WO2009110449A1 (ja) | 2009-09-11 |
JP2009212433A (ja) | 2009-09-17 |
US20110014796A1 (en) | 2011-01-20 |
EP2264744A1 (en) | 2010-12-22 |
EP2264744B1 (en) | 2018-05-02 |
EP2264744A4 (en) | 2016-11-09 |
US8603923B2 (en) | 2013-12-10 |
TW200946453A (en) | 2009-11-16 |
KR101623764B1 (ko) | 2016-05-24 |
TWI538884B (zh) | 2016-06-21 |
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