TW202132638A - 鎵前驅體的製造方法及使用其之積層體的製造方法 - Google Patents
鎵前驅體的製造方法及使用其之積層體的製造方法 Download PDFInfo
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- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 125
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 124
- 239000002243 precursor Substances 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 40
- 239000000758 substrate Substances 0.000 claims description 28
- 239000012159 carrier gas Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000012433 hydrogen halide Substances 0.000 claims description 2
- 229910000039 hydrogen halide Inorganic materials 0.000 claims description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 6
- 229940071870 hydroiodic acid Drugs 0.000 description 6
- 229910052594 sapphire Inorganic materials 0.000 description 6
- 239000010980 sapphire Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- -1 gallium halide Chemical class 0.000 description 5
- 229910001195 gallium oxide Inorganic materials 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003595 mist Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- YGSFNCRAZOCNDJ-UHFFFAOYSA-N propan-2-one Chemical compound CC(C)=O.CC(C)=O YGSFNCRAZOCNDJ-UHFFFAOYSA-N 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
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- 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
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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Abstract
本發明為一種鎵前驅體的製造方法,其係製作鎵前驅體的方法,其係包含:準備由含有酸及/或鹼之水溶液所構成的溶劑之步驟、將鎵浸漬於前述溶劑之步驟、將已浸漬於前述溶劑之前述鎵微細化之步驟及將前述已微細化之前述鎵溶解之步驟。藉此,能以高品質提供高生產性之鎵前驅體的製造方法。
Description
本發明係有關於一種有用於含鎵膜積層體的製造之鎵前驅體的製造方法及使用其之積層體的製造方法。
作為能以低溫、大氣壓形成磊晶膜等的方法,已知有霧化CVD法等使用水微粒子的成膜手法。
於專利文獻1中,係將乙醯丙酮鎵溶解於鹽酸等酸而形成前驅體,並將此前驅體霧化而生成原料微粒子,再將此原料微粒子與載流氣體混合而成的混合氣體供給至藍寶石等剛玉構造之基板的表面,使原料霧滴反應而於基板上磊晶生長單一配向之氧化鎵薄膜。
又,專利文獻2中記載一種使用鹵化鎵水溶液的方法,該鹵化鎵水溶液係以鹽酸、氫溴酸、氫氟酸、氫碘酸等,費時1至2週左右將鎵溶解而得。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本專利第5793732號公報
[專利文獻2]日本特開2018-070422號公報
[發明所欲解決之課題]
然而,專利文獻1之方法,由於前驅體使用有機錯合物,所得之膜的碳濃度較高,而無法獲得高品質的膜。
又,專利文獻2所記載之方法,由於溶解鎵需要長時間而不實用。
本發明係有鑑於如上述之問題而完成者,茲以提供一種在製造前驅體時不使用有機錯合物,而抑制所得膜中的碳濃度,得以製造高品質的膜,且藉由縮短前述前驅體製造時溶解鎵所需之時間,而以高生產性製造鎵前驅體的方法為目的。
[解決課題之手段]
為達成上述目的,本發明係提供一種鎵前驅體的製造方法,其係製作鎵前驅體的方法,其係包含:準備由含有酸及/或鹼之水溶液所構成的溶劑之步驟、將鎵浸漬於前述溶劑之步驟、將已浸漬於前述溶劑之前述鎵微細化之步驟及將前述已微細化之前述鎵溶解之步驟。
若為此種鎵前驅體製造方法,則可於短時間內溶解前述鎵,而能夠以高生產性製造不使用有機錯合物的鎵前驅體。
此時,將前述鎵微細化之步驟宜藉由超音波振動來進行。
如此,可容易使前述鎵微細化,同時可進一步促進前述鎵的溶解。
此時,在將前述鎵微細化之步驟以前,可進一步將前述鎵液化。
如此,可進一步縮短鎵的溶解時間。
此時,在將前述鎵溶解之步驟中,前述溶劑的溫度宜保持於30℃以上且未達100℃的溫度。
如此,可進一步促進鎵的溶解。
此時,可使用鹵化氫作為前述酸;且可使用氨作為前述鹼。
如此,可使鎵前驅體成為高純度者。
又,本發明係提供一種積層體的製造方法,其係包含含有鎵的膜之積層體的製膜方法,其係包含:將基體加熱之步驟、將以上述方法所製作的鎵前驅體,進一步用水稀釋而製作鎵前驅體溶液之步驟、將前述鎵前驅體溶液霧化之步驟、將前述經霧化之前述鎵前驅體溶液以載流氣體供給至前述基體之步驟及在前述基體上使前述經霧化之前述鎵前驅體溶液反應,而形成含有前述鎵的膜之步驟。
如此,能以高生產性獲得雜質較少之高品質的積層體。
[發明之效果]
根據本發明之鎵前驅體製造方法,能以高生產性製造高品質的鎵前驅體。
又,根據採用本發明之鎵前驅體製造方法的製膜方法,可容易且以低成本製造雜質較少之高品質的含鎵膜之積層體。
[實施發明之形態]
諸如上述,業界要求可抑制碳濃度之高品質的膜的製造方法,及以高生產性製造使用於膜的製造之鎵前驅體的方法。
而且,本案發明人為解決上述課題而致力累積多次研究的結果發現出一種藉由在製造前驅體時不使用有機錯合物,可抑制所得膜中的碳濃度而製造高品質的膜,且藉由縮短製造前述前驅體時溶解鎵所需的時間,而以高生產性製造鎵前驅體的方法,終至完成本發明。
亦即,本發明係提供一種鎵前驅體的製造方法,其係製作鎵前驅體的方法,其特徵為包含:準備由含有酸及/或鹼之水溶液所構成的溶劑之步驟、將鎵浸漬於前述溶劑之步驟、將已浸漬於前述溶劑之前述鎵微細化之步驟及將前述已微細化之前述鎵溶解之步驟。
根據本發明之鎵前驅體製造方法,能以高生產性製造高品質的鎵前驅體。又,根據採用本發明之鎵前驅體製造方法的製膜方法,可容易且以低成本製造雜質較少之高品質的含鎵膜之積層體。
以下,一邊參照圖1及圖2一邊就本發明詳細加以說明,惟本發明非限定於此。
本發明之鎵前驅體係使鎵溶解於由含有酸及/或鹼之水溶液所構成的溶劑而成的溶液。
本發明之鎵前驅體製造方法係具有以下特徵之製造方法:具有將已浸漬於溶劑的鎵微細化之步驟,與將前述已微細化之前述鎵溶解之步驟。此外,微細化之方法不特別限定,較佳藉由超音波振動予以微細化。
如圖1所示,首先將裝有溶劑102的容器103設置於超音波產生器104中,其中該溶劑102係至少含有鎵101與酸或鹼的任一種。超音波產生器104係例如具備水槽105、振動件106、介質107及加熱手段108。此外,鎵101與溶劑102,何者先置入容器103中均無妨。
鎵101係以在進行微細化之步驟以前先予以液化為佳。藉此,即更容易達到鎵101的微細化。
惟,在秤量鎵之際,若使用液化鎵時,由於鎵的浸潤性極強,較佳為非於其他容器等進行,而是將鎵直接置入至裝入溶劑102前的容器103中來進行。
由振動件106發出之超音波的頻率,只要可將鎵101微細化則不特別限定,例如較佳定為20kHz以上1000kHz以下。藉此,由於可將鎵101微細化成毫米單位至微米單位之直徑而使表面積增加,可促進在鎵表面的化學反應而能夠有效地予以溶解。
此外,介質107係供傳播由振動件106發出的超音波,傳遞至容器103內的溶劑102及鎵101,較佳使用水;藉由加熱手段108將其保持於30℃至100℃,更佳為30℃至60℃,可進一步促進溶劑102與鎵101的化學反應,而能夠更有效地將鎵101溶解。
溶劑102使用酸時,較佳使用氫鹵酸,更佳為氫氯酸、氫溴酸或氫碘酸,最佳為氫碘酸。使用氫碘酸時,可使用例如1~12N(濃度55~58%)的氫碘酸,可將其直接或者用純水稀釋而使用。
溶劑使用鹼時,較佳使用氨,可使用例如氫氧化銨。此時,可使用例如1~12N(濃度28~40%)的氫氧化銨,可將其直接或者用純水稀釋而使用。
又,亦可將上述酸與鹼混合,適宜調整溶劑102的pH而使用。
如此,藉由將鎵101完全溶解,可得到鎵前驅體。
鎵前驅體的鎵濃度可視目的而定來調整,而基於生產性觀點較佳定為0.1 mol/L至5 mol/L,更佳定為1 mol/L至3.5 mol/L左右。
其次,一邊參照圖2一邊針對使用藉由上述製造方法所製造的鎵前驅體之含鎵膜積層體的製造方法的一例加以說明,惟本發明非限定於此。
圖2示出本發明之積層體的製造方法所使用之裝置的一例。於本發明之積層體的製造方法中,係使用霧化CVD裝置200。霧化CVD裝置200係具備:載流氣體201、霧化器202a、霧化器202b、輸送配管203、閥204、閥205、輸送配管206、基體207、承座208、製膜室209、加熱手段210。
首先,在霧化器202a、202b內分別容納有作為原料的第1前驅體溶液212a、第2前驅體溶液212b,且使用週知之手段予以霧化(亦稱「霧滴化」),而形成霧滴。此外,本發明中所稱霧滴,係指分散於氣體中的液體微粒子,包含所稱霧、液滴者,亦有時稱為霧、液滴。
第1前驅體溶液212a與第2前驅體溶液212b的至少一者係使用將以上述記載之鎵前驅體製造方法所得之鎵前驅體用純水適當調整濃度的前驅體溶液。
前驅體溶液212a、212b中的鎵濃度不特別限定,可依據目的或規格適宜設定。較佳為0.001 mol/L以上至2 mol/L,更佳為0.01 mol/L以上0.7 mol/L以下。
此外,第1前驅體溶液212a與第2前驅體溶液212b的成分可相同或相異。例如要形成由鎵與鋁構成的二元系氧化物時等,可使用鎵前驅體溶液作為第1前驅體溶液212a,且使用鋁前驅體溶液作為第2前驅體溶液212b。
又,亦可對前驅體溶液212a、212b添加雜質。例如要形成氧化鎵時,可舉出錫、鍺、矽、鈦、鋯、釩或鈮等n型摻雜物,或銅、銀、錫、銥、銠等p型摻雜物等。可合宜使用含有此等摻雜物的錯合物或化合物,尤以使用鹵化錫為佳。
此等雜質原料,能以相對於前驅體溶液的鎵濃度為0.0001%~20%,更佳為0.001%~10%的比例使用。又,此等雜質可混於鎵前驅體溶液來使用,亦可個別準備鎵前驅體溶液作為第1前驅體溶液212a、準備雜質溶液作為第2前驅體溶液212b,以霧滴狀予以混合。
前驅體溶液212a、212b的霧化手段,只要可予以霧化或液滴化則不特別限定,可為週知之手段;於本發明中,較佳為使用超音波之霧化手段。
使用超音波所得之霧或液滴由於初速度為零且浮游於空中而較佳,例如其可非如噴霧般地噴灑,而是浮游於空間中以氣體形式輸送,無碰撞能量所致之損傷而極佳。
液滴大小不特別限定,可為數mm左右的液滴,較佳為50μm以下,更佳為0.1~10μm。
載流氣體201係與在霧化器202a、202b內形成的霧化之原料(前驅體溶液)混合,分別形成第1混合氣體213、第2混合氣體223,並朝製膜室209輸送。
供給至製膜室209的混合氣體,係在於製膜室209內藉由加熱手段210經加熱的基體207上進行反應,而形成膜。
於圖2所示個例中,係顯示霧化器202b與製膜室209以輸送配管206連接,且起自霧化器202a的輸送配管203在輸送配管206的中途匯集之構造,惟輸送配管203與輸送配管206亦可獨立地連接至製膜室209。又,不限於此,可將第1混合氣體213與第2混合氣體223導入至單一的緩衝槽(未圖示),並將在緩衝槽中混合的霧滴朝製膜室209輸送。
載流氣體201不特別限定,例如除空氣、氧氣、臭氧外,宜使用氮氣或氬氣等惰性氣體,或者氫氣或氫氮混合氣體等還原氣體。載流氣體的種類可為1種或2種以上。
載流氣體的流量,只要根據基體尺寸或製膜室的大小適宜設定即可,可採0.01~100 L/min左右。
此外,製膜可於大氣壓下、加壓下及減壓下之任一種條件下進行,而由裝置成本或生產性方面而言,較佳在大氣壓下進行。
又,雖未圖示,亦可添加稀釋氣體來調節經霧化之前驅體溶液與載流氣體的比例。稀釋氣體的流量只要適宜設定即可,可取例如載流氣體的0.1~10倍/分。
亦可將稀釋氣體朝例如霧化器202a、202b的下游側供給。又,稀釋氣體可使用與載流氣體相同者或不同者。
輸送配管203、206只要是對前驅體之溶劑或反應器與輸送配管之接合處的溫度等具有充分的穩定性者則不特別限定,可廣泛使用石英、聚乙烯、聚丙烯、氯乙烯、聚矽氧樹脂、胺基甲酸酯樹脂、氟樹脂等一般的樹脂製配管。
製膜室209的構造等不特別限定,可使用鋁或不鏽鋼等金屬;在超過此等金屬之耐熱溫度的更高溫下進行製膜時,亦可使用石英或碳化矽。在製膜室209的內部或外部設有供加熱基體207的加熱手段210。又,基體207可載置於設置在製膜室209內的承座208上。
此外,上述基體只要是可支持形成的膜者則不特別限定。基體的材料可為週知者,可為有機化合物或無機化合物。可舉出例如聚碸、聚醚碸、聚苯硫醚、聚醚醚酮、聚醯亞胺、聚醚醯亞胺、氟樹脂、鐵、鋁或不鏽鋼、金等金屬、矽、藍寶石、石英、玻璃、碳酸鈣、氧化鎵、SiC、ZnO、GaN等,但不限於此。
基體的形狀可舉出例如平板或圓板等的板狀、纖維狀、棒狀、圓柱狀、角柱狀、筒狀、螺旋狀、球狀、環狀等,任一者皆可使用。尤其是當基體為板狀體時,就其厚度,於本發明中不特別限定,較佳為50~2000μm,更佳為200~800μm。
於本發明中,上述基體較佳為包含具有剛玉構造之結晶物作為主成分的基體,或包含具有β-氧化鎵構造之結晶物作為主成分的基體。此處所稱主成分,係指含有50%以上的該成分之物質。
以具有剛玉構造之結晶為主成分的基板可舉出例如藍寶石(例如c面藍寶石基板)或α型氧化鎵等。
又,以具有β-氧化鎵構造之結晶物作為主成分的基體,可舉出例如β-Ga2
O3
基板,或含有Ga2
O3
與Al2
O3
且Al2
O3
多於0質量%且為60質量%以下的混晶體基板、於週知之基板上形成β-Ga2
O3
膜之基板等。
其他基體之實例可舉出具有六方晶構造之基體(例如SiC、ZnO、GaN、LiTaO3
)等。亦可在具有六方晶構造之基體上,直接或經由其他層(例如緩衝層)而形成膜。
[實施例]
以下利用實施例及比較例具體地說明本發明,惟本發明非限定於此等。
(實施例1)
在硼矽酸玻璃製燒杯中秤量經液化的鎵20g,對其添加濃度56.3%的氫碘酸145mL。將其設置於水溫保持在40℃的超音波產生器中,以頻率38kHz的超音波使鎵振動而予以微細化。於此狀態下放置至鎵完全溶解為止,而製成2 mol/L的鎵前驅體。
測定溶解所需時間,為2小時40分鐘。
(比較例1)
除未對鎵施加超音波振動以外,係與實施例1同樣地製作鎵前驅體。測定溶解所需時間,結果為276小時。
實施例1之結果,與比較例1相比,鎵前驅體的製造所需時間大幅縮短。
(實施例2)
藉由霧化CVD裝置,依以下條件進行氧化鎵的製膜。首先將實施例1中所製作的鎵前驅體用純水稀釋而以0.05 mol/L的前驅體溶液作為原料溶液,並將前述原料溶液填充於霧化器中。
其次,將直徑4吋(100mm)、厚度0.6mm的c面藍寶石基板載置於石英製承座上而設置於石英製管狀型製膜室內,並藉由加熱器將前述c面藍寶石基板溫度保持於450℃。
其次以2.4MHz的超音波振動件將霧化器內的前述原料溶液霧化。此後,分別對霧化器導入載流氣體之氮氣1.5 L/min,進而導入稀釋氣體之氮氣5 L/min而形成混合氣體,朝製膜室供給而進行製膜。
分別藉由XRD法及SIMS法評定所得膜的結晶性與碳濃度。
(比較例2)
除將乙醯丙酮鎵以稀鹽酸水溶液(鹽酸濃度2%)溶解而製備0.05 mol/L的前驅體溶液以外,係與實施例2同樣地進行製膜暨評定。
由上述結果可知,根據本發明,比起習知技術可特別改善鎵前驅體的生產性,且若使用以本發明之方法所得的鎵前驅體,可獲得品質高於習知技術的膜。
此外,本發明非限定於上述實施形態。上述實施形態僅為例示,與本發明申請專利範圍所記載之技術思想實質上具有相同構成且發揮相同作用效果者均包含於本發明技術範圍內。
101:鎵
102:溶劑
103:容器
104:超音波產生器
105:水槽
106:振動件
107:介質
108:加熱手段
200:霧化CVD裝置
201:載流氣體
202a:霧化器
202b:霧化器
203:輸送配管
204:閥
205:閥
206:輸送配管
207:基體
208:承座
209:製膜室
210:加熱手段
212a:第1前驅體溶液
212b:第2前驅體溶液
213:第1混合氣體
223:第2混合氣體
[圖1]為表示本發明之鎵前驅體的製造方法之一形態的圖。
[圖2]為表示本發明之製膜方法之一形態的圖。
101:鎵
102:溶劑
103:容器
104:超音波產生器
105:水槽
106:振動件
107:介質
108:加熱手段
Claims (7)
- 一種鎵前驅體的製造方法,其係製作鎵前驅體的方法,其特徵為包含: 準備由含有酸及/或鹼之水溶液所構成的溶劑之步驟、將鎵浸漬於前述溶劑之步驟、將已浸漬於前述溶劑之前述鎵微細化之步驟及將前述已微細化之前述鎵溶解之步驟。
- 如請求項1之鎵前驅體的製造方法,其中將前述鎵微細化之步驟係藉由超音波振動將前述鎵微細化。
- 如請求項1或2之鎵前驅體的製造方法,其中在將前述鎵微細化之步驟以前,進一步包含將前述鎵液化。
- 如請求項1至3中任一項之鎵前驅體的製造方法,其中在將前述鎵溶解之步驟中,係將前述溶劑的溫度保持於30℃以上且未達100℃。
- 如請求項1至4中任一項之鎵前驅體的製造方法,其中係使用鹵化氫作為前述酸。
- 如請求項1至5中任一項之鎵前驅體的製造方法,其中係使用氨作為前述鹼。
- 一種積層體的製造方法,其係包含含有鎵的膜之積層體的製膜方法,其特徵為包含: 將基體加熱之步驟、將以如請求項1至6中任一項之方法所製作的前述鎵前驅體,進一步用水稀釋而製作鎵前驅體溶液之步驟、將前述鎵前驅體溶液霧化之步驟、將前述經霧化之前述鎵前驅體溶液以載流氣體供給至前述基體之步驟及在前述基體上使前述經霧化之前述鎵前驅體溶液反應,而形成含有前述鎵的膜之步驟。
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