CN116082045B - 氧化铟钛钽铈粉末及其制备方法和改善氧化铟钛钽铈性能的方法 - Google Patents
氧化铟钛钽铈粉末及其制备方法和改善氧化铟钛钽铈性能的方法 Download PDFInfo
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- CN116082045B CN116082045B CN202211616110.1A CN202211616110A CN116082045B CN 116082045 B CN116082045 B CN 116082045B CN 202211616110 A CN202211616110 A CN 202211616110A CN 116082045 B CN116082045 B CN 116082045B
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- indium
- cerium oxide
- solution
- ions
- tantalum
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- -1 Indium titanium tantalum cerium oxide Chemical compound 0.000 title claims abstract description 139
- 239000000843 powder Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 34
- 238000001354 calcination Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 229910001449 indium ion Inorganic materials 0.000 claims abstract description 14
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 9
- 229910001460 tantalum ion Inorganic materials 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 238000000227 grinding Methods 0.000 abstract description 12
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 4
- 229910003437 indium oxide Inorganic materials 0.000 abstract description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 135
- 239000002243 precursor Substances 0.000 description 38
- 239000007787 solid Substances 0.000 description 36
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 30
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 239000007788 liquid Substances 0.000 description 20
- 238000000926 separation method Methods 0.000 description 18
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- FYNXQOUDSWHQQD-UHFFFAOYSA-N tantalum(5+) pentanitrate Chemical compound [Ta+5].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYNXQOUDSWHQQD-UHFFFAOYSA-N 0.000 description 14
- 238000002156 mixing Methods 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 229910044991 metal oxide Inorganic materials 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 150000004706 metal oxides Chemical class 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000010008 shearing Methods 0.000 description 5
- 239000013077 target material Substances 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000012702 metal oxide precursor Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 4
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 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 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 3
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 235000015895 biscuits Nutrition 0.000 description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 2
- 229920000136 polysorbate Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WUSPVAHLRCJNMG-UHFFFAOYSA-D tantalum(5+) pentasulfate Chemical compound [Ta+5].[Ta+5].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WUSPVAHLRCJNMG-UHFFFAOYSA-D 0.000 description 2
- ZIRLXLUNCURZTP-UHFFFAOYSA-I tantalum(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Ta+5] ZIRLXLUNCURZTP-UHFFFAOYSA-I 0.000 description 2
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 239000004264 Petrolatum Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 239000004147 Sorbitan trioleate Substances 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- SQKWGPOIVHMUNF-UHFFFAOYSA-K cerium(3+);trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Ce+3] SQKWGPOIVHMUNF-UHFFFAOYSA-K 0.000 description 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- YDRFJPRPCBJKCM-UHFFFAOYSA-L dichlorocopper ethanol Chemical compound C(C)O.[Cu](Cl)Cl YDRFJPRPCBJKCM-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 125000005358 mercaptoalkyl group Chemical group 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 1
- 229940066842 petrolatum Drugs 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229950008882 polysorbate Drugs 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- UDWXLZLRRVQONG-UHFFFAOYSA-M sodium hexanoate Chemical compound [Na+].CCCCCC([O-])=O UDWXLZLRRVQONG-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- IJRHDFLHUATAOS-DPMBMXLASA-M sodium ricinoleate Chemical compound [Na+].CCCCCC[C@@H](O)C\C=C/CCCCCCCC([O-])=O IJRHDFLHUATAOS-DPMBMXLASA-M 0.000 description 1
- WYPBVHPKMJYUEO-NBTZWHCOSA-M sodium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Na+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O WYPBVHPKMJYUEO-NBTZWHCOSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229950004959 sorbitan oleate Drugs 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
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Abstract
本发明属于半导体技术领域,公开了一种氧化铟钛钽铈粉末的制备方法,将含铟离子、钛离子、钽离子、铈离子的溶液和碱性沉淀剂反应,过滤得到沉淀,将沉淀经研磨、煅烧后制得氧化铟钛钽铈粉末;所述溶液中铟离子的浓度为0.4~1.5M;溶液和碱性沉淀剂反应的反应终点为溶液pH为中性。该方法制备出的氧化铟钛钽铈粉末中氧化钛、氧化钛、氧化铈和氧化铟的粒子分散均匀,用于靶材制作后氧化铈的分布均匀性极高,有效增加靶材的性能。同时,本发明还提供了该靶材的用途。
Description
技术领域
本发明涉及半导体技术领域,具体涉及一种氧化铟钛钽铈粉末及其制备方法和改善氧化铟钛钽铈性能的方法。
背景技术
ITO靶材对于显示器产业是一个核心的部件,随着人们对大尺寸高清晰度的重视程度提升,显示器厂商对显示器所需的ITO靶材要求也越来越高,而粉体制备是ITO靶材制备过程的关键工序,氧化铟钛钽铈粉末又是ITO靶材的其中一种重要的类型,因此氧化铟钛钽铈粉末的质量是ITO靶材质量的关键因素。
D1:中国专利202111548177.1公开了一种氧化铟铈钛钽粉体及其制备方法,属于铟铈钛钽氧化物的制备领域。所述氧化铟铈钛钽粉体的化学式为In1-x-y-zTaxTiyCezO,其中,x、y、z的值为0.001-0.2;D50=1.28-1.54μm,D10≥0.71μm,D90≤4.45μm,粒度分布系数P=(D90-D10)/D50≤2.51,含水量:0.36%-0.55%。
上述专利的制备方法是通过将氧化钛、氧化钛、氧化铈和氧化铟通过分散剂混合分步进行湿法研磨,再进行喷雾造粒、混料和筛分得到想要的氧化铟铈钛钽粉体;其生产出的粉体粒径均匀,粒度分布小,成分均一,避免了大粒径稀有金属元素掺入氧化铟引起的成分不均一的问题。
但是由于ITO靶材的质量要求升高,上述专利的制备方法制备出的氧化铟铈钛钽粉末出现一个小小的缺陷,那就是氧化铈的粒子分散不够均匀,导致生产出来的ITO靶材不能满足更高的技术要求。
为了解决上述缺陷,寻找更适合的氧化铟铈钛钽粉体制备方法,经过多方面的资料查询,找到了可借鉴的专利文件中国专利201410609324.5(D2),该专利公开了一种铟锡金属氧化物的制备方法,包括:将第一碱性沉淀剂和含有锡离子的溶液进行第一反应,得到含有锡的沉淀物;将第二碱性沉淀剂、含有铟离子的溶液和所述含有锡的沉淀物进行第二反应,得到含有铟和锡的沉淀物;将所述含有铟和锡的沉淀物进行煅烧,得到铟锡金属氧化物。
上述专利启示了采用含有金属离子的溶液和碱性沉淀剂反应生成含有氢氧化的金属沉淀物,然后通过对金属沉淀物进行煅烧得到金属氧化物的技术方案;
但是,本申请人经过研究后认为,采用分步法进行沉淀,需要采用强力搅拌才能得到性能符合我司性能要求的靶材。
D3:CN113287635A公开一种用于抗菌、防霉的掺杂金属氧化物纳米颗粒、分散体或粉体及其制备方法。所述抗菌、防霉的掺杂金属氧化物纳米颗粒、分散体或粉体由以下制备方法制备,包括:1)提供掺杂金属氧化物前驱体溶液和沉淀剂溶液;2)所述掺杂金属氧化物前驱体溶液和所述沉淀剂溶液在高剪切的强混合状态下反应得到所述掺杂金属氧化物颗粒;3)所述掺杂金属氧化物颗粒经后处理和分散形成分散体或再经干燥得到粉体;所述掺杂金属氧化物中,主相金属为过渡金属元素,掺杂元素为主族元素或副族元素中的一种或两种以上。
该方案说明书公开了:所述掺杂金属氧化物前驱体溶液为主相金属钛和/或锌的盐、含氧酸或络合物溶液与掺杂元素A和/或B的盐、含氧酸或络合物溶液形成的混合溶液;所述掺杂元素A和/或B以其化合物、离子、单质或其任意组合的形式提供和/或存在于所述掺杂金属氧化物前驱体和/或沉淀剂中;
配制一定量的0.15mol/L-0.5mol/L的硫酸氧钛、氯化锌、氯化镧、氯化铁、醋酸锌、硝酸镧、硫酸锌、硝酸锌、硝酸钕的水溶液备用;配制一定量的0.15mol/L-0.5mol/L的醋酸铜、氯化铜乙醇溶液备用;采用六水合氯化铈和六水合硝酸亚铈配制一定量的0.15mol/L-0.5mol/L的氯化亚铈、硝酸亚铈水溶液备用;配制一定量的0.4-0.8mol/L的氢氧化钠、氢氧化钾、氨水的水溶液备用。四氯化钛由于其快速放热反应而不能直接溶于水,所述放热反应产生原钛酸而释放出大量热。因此使用盐酸和水(体积比1:19,36%HCl:H2O)及四氯化钛的混合物,溶解过程在冰冷温度下并剧烈搅拌的情况下进行,最后再调配成0.3mol/L-0.5mol/L的钛盐溶液备用。
在生产过程中,我们发现如下问题:
1.氢氧化钛、氢氧化钽受pH影响较大,如果不精确的控制工艺,导致前驱体的物质比例无法达标;
2.即使氢氧化钛、氢氧化钽完全回收,溶液浓度对产品物理性质影响明显,如孔隙率、电阻率等。
所以,本案解决的技术问题是:如何提高氧化铟钛钽铈在制备过程中的物质比例的准确性,如何提高氧化铟钛钽铈的物理性质。
发明内容
本发明的目的之一在于,提供一种氧化铟钛钽铈粉末的制备方法,该方法制备出的氧化铟钛钽铈粉末中氧化钛、氧化钛、氧化铈和氧化铟的粒子分散均匀,用于靶材制作后氧化铈的分布均匀性极高,有效增加靶材的性能。
同时,本发明还提供了该靶材的用途。
在本发明未做特殊说明的情况下,M为mol/L,%为质量百分比。
为实现上述目的,本发明提供了一种氧化铟钛钽铈粉末的制备方法,其特征在于,将含铟离子、钛离子、钽离子、铈离子的溶液和碱性沉淀剂反应,过滤得到沉淀,将沉淀经研磨、煅烧后制得氧化铟钛钽铈粉末;
所述溶液中铟离子的浓度为0.4~1.5M;
溶液和碱性沉淀剂反应的反应终点为溶液pH为中性。
在实际应用中,所述铟离子的浓度可选择为0.4M、0.5M、0.6M、0.7M、0.8M、0.9M、1.0M、1.1M、1.2M、1.3M、1.4M或1.5M;
本发明所述的中性为本领域技术人员常规意义上所认为的中性,比如可为6.8-7.3;可选的pH值为6.9、7.0、7.1或7.2。
本发明所述的溶液一般是指水溶液,但是并不排斥其他共溶剂的加入,如一元醇、二元醇等;这里的共溶剂只需要和水能互溶或者能够在设定的比例的情况下能够完全互溶即可。
还可以进一步在上述溶液中加入少量的表面活性剂,烷基三烷氧基硅烷,(甲基)丙烯酰氧基烷基三烷氧基硅烷,丙烯酰氧基烷基三烷氧基硅烷,(甲基)丙烯酰氧基烷基烷基二烷氧基硅烷,丙烯酰氧基烷基烷基二烷氧基硅烷,(甲基)丙烯酰氧基烷基二烷基烷氧基硅烷,丙烯酰氧基烷基二烷基烷氧基硅烷,巯基烷基三烷氧基硅烷,γ-甲基丙烯酰氧基丙基三甲氧基硅烷,芳基三烷氧基硅烷,乙烯基硅烷,3-缩水甘油醚基丙基三烷氧基硅烷,聚醚硅烷,γ-氨基丙基三乙氧基硅烷,γ-缩水甘油氧丙基三甲氧基硅烷,γ-(甲基丙烯酰氧)丙基三甲氧基硅烷,γ-巯丙基三甲氧基硅烷,γ-氨乙基氨丙基三甲氧基硅烷,双-[丙基三乙氧基硅烷],N-(β-氨乙基)-γ-(氨丙基)-甲基二甲氧基硅烷,N-(β-氨乙基)-γ-(氨丙基)-三甲氧基硅烷,γ-氨乙基-氨丙基三甲氧基硅烷,十六烷基三甲氧基硅烷,或它们的组合;以及十二烷基硫酸钠,十二醇硫酸钠,月桂酸钠,油酸钠,石油酸钠,硬脂酸钠,松脂酸钠,异辛酸钠,亚油酸钠,己酸钠,蓖麻酸钠,醋酸乙酯,醋酸钠,二辛脂磺酸钠,吐温(聚氧乙烯山梨糖醇酐单油酸酯),司盘80(失水山梨醇油酸酯),司盘85(山梨糖醇酐三油酸酯),普朗尼克(pluronic),聚山梨酯,聚N-乙烯基吡咯烷酮,聚乙二醇,聚氧乙烯,双-2-羟乙基油胺,十六烷基三甲基溴化铵,羟丙基纤维素,羟丙基甲基纤维素,麦芽糖,蔗糖,柠檬酸,(乙烯)乙二醇,丙烯酸,甲基丙烯酸,β-羟基丙烯酸乙酯,正硅酸乙酯和它们的混合物;在一些资料中记载,这些表面活性剂可提高沉淀颗粒的分散性,本发明并未对此进行进一步研究和实验,但是任何方案使用了表面活性剂的时候都应该视为在本发明的保护范围内。
在本发明的沉淀反应过程中,一般需要进行搅拌,还可以在搅拌的同时辅以超声、振荡或剪切等形式进行组合;在一些现有的技术材料中记载,所述搅拌可以由机械搅拌器和/或磁力搅拌器实现。所述高剪切条件是指所述流体的雷诺数在2000~200000、5000~150000、8000~100000范围内。采用较高的雷诺数可以提高混合程度、加快反应速度、缩短反应时间、减小颗粒粒径、减轻颗粒聚集等。通过搅拌和剪切产生的剪切力来实现高剪切条件,达到好的强混合状态,如已公开的专利申请号为PCT/SG02/00061的国际专利申请的公开说明书所述采用旋转填充床形式的超重力反应器来实现流体被强剪切后的强混合;也可以通过采用如《高校化学工程学报》2012年26卷4期558页描述的螺旋盘管反应器来实现流体在反应器中特殊流动,即物料在螺旋盘管反应器中进行的反应达到径向全混流,轴向平推流的良好混合状态。这些实施方式的优点是可实现生产的连续化。也可以采用如PCT/CN2010/071651的国际专利申请的公开说明书所述的微通道管式装置,同样可以达到径向全混流,轴向平推流的良好混合状态,然后再对已达到液-液微观混合良好的液体在搅拌釜中进一步搅拌混合来实现半间歇式的强混合状态。
就目前的实验过程来看,本发明采用单一机械搅拌就能够达到本发明的实验目的,在其他方案中,如果采用了上述的分散方案,也应该视为在本发明的保护范围内。
在上述的氧化铟钛钽铈粉末的制备方法中,所述溶液中铟离子、钛离子、钽离子、铈离子的摩尔比为1:0.001-0.05:0.001-0.05:0.001-0.05;优选为1:0.002-0.02:0.002-0.02:0.002-0.02。
在上述的氧化铟钛钽铈粉末的制备方法中,所述溶液中的阴离子为氯离子、硫酸根离子、硝酸根离子中的一种或多种。
在上述的氧化铟钛钽铈粉末的制备方法中,所述碱性沉淀剂为NaOH、KOH、氨水中的一种或多种。当然,在实际的实验过程中,实验者还可以进一步的采用其他的碱性沉淀剂来进行实验。
在上述的氧化铟钛钽铈粉末的制备方法中,所述碱性沉淀剂以滴加的方式加入到溶液中,所述碱性沉淀剂的浓度为2.0M~6.0M,优选为2.0M~5.0M。在一些实施案例中,所述的碱性沉淀剂的浓度为2.0M、3.0M、4.0M、5.0M或6.0M;
优选地,所述溶液中铟离子的浓度为0.8~1.2M,较优选地,所述溶液中铟离子的浓度为0.9~1.1M。
在本发明中,溶液和碱性沉淀剂反应的反应终点为溶液pH为7,研磨后的粉末粒径为:D50为0.1μm-0.5μm,D90为0.5μm-1.0μm;
煅烧的温度为700-900℃,煅烧时间为6-10h。
同是,本发明还公开了一种氧化铟钛钽铈粉末,采用如上任一所述方法制备得到。
最后,本发明还公开了一种改善氧化铟钛钽铈性能的方法,采用如上任一所述的方法制备氧化铟钛钽铈。
有益效果
与现有技术相比,本发明提供了一种氧化铟钛钽铈粉末的制备方法,具有以下优势:
(1)通过采用铟、钛、钽、铈原液和强碱性沉淀剂混合反应生成氢氧化铟、钛、钽、铈沉淀物,再通过烘干、研磨、煅烧等工序制备出粒子均匀程度更高的氧化铟钛钽铈粉末;
(2)通过特定的铟、钛、钽、铈的原子比使得制备过程中氢氧化钛不会被酸或碱大量带走,保留了所需的钛离子的量,从而煅烧后生成的氧化铟钛钽铈粉末中氧化钛的量可以满足靶材制备的要求;
(3)对氧化铟钛钽铈前驱体的粒径进行控制,从而使得煅烧后生成的氧化铟钛钽铈粉末具有更好的粒子均匀性。
(4)选择主金属离子的浓度,可有效控制靶材的孔隙率、电阻率等。
具体实施方式
下面结合实施例,对本发明作进一步的描述,但不构成对本发明的任何限制,任何在本发明权利要求范围所做的有限次的修改,仍在本发明的权利要求范围内。
为了详细说明本发明的技术内容,以下结合实施方式作进一步说明。
实施例1
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、50ml的0.2mol/L硝酸钛溶液、50ml的0.2mol/L硝酸钽溶液和50ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为5.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到粒径D50为0.242μm、D90为0.624μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在800℃进行煅烧8h,即得所述氧化铟钛钽铈粉末。
实施例2
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到粒径D50为0.238μm、D90为0.681μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
实施例3
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、200ml的0.2mol/L硝酸钛溶液、100ml的0.2mol/L硝酸钽溶液和50ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加、摩尔浓度为5.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到粒径D50为0.276μm、D90为0.676μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在900℃进行煅烧9h,即得所述氧化铟钛钽铈粉末。
实施例4
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、150ml的0.2mol/L硝酸钛溶液、50ml的0.2mol/L硝酸钽溶液和25ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到粒径D50为0.291μm、D90为0.607μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在850℃进行煅烧8h,即得所述氧化铟钛钽铈粉末。
实施例5
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将2000ml的0.5mol/L硫酸铟溶液、100ml的0.5mol/L硫酸钛溶液、100ml的0.5mol/L硫酸钽溶液和100ml的0.5mol/L硫酸铈溶液进行混合,再向其中滴加、摩尔浓度为6.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、80℃烘干、研磨后,得到粒径D50为0.248μm、D90为0.635μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在730℃进行煅烧10h,即得所述氧化铟钛钽铈粉末。
实施例6
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将667ml的1.5mol/L硫酸铟溶液、10ml的0.1mol/L硫酸钛溶液、10ml的0.1mol/L硫酸钽溶液和10ml的0.1mol/L硫酸铈溶液进行混合,再向其中滴加、摩尔浓度为2.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、60℃烘干、研磨后,得到粒径D50为0.251μm、D90为0.662μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在700℃进行煅烧8h,即得所述氧化铟钛钽铈粉末。
实施例7
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将667ml的1.5mol/L氯化铟溶液、40ml的0.3mol/L氯化钛溶液、50ml的0.2mol/L氯化钽溶液和40ml的0.2mol/L氯化铈溶液进行混合,再向其中滴加、摩尔浓度为3.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、75℃烘干、研磨后,得到粒径D50为0.264μm、D90为0.682μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在880℃进行煅烧6h,即得所述氧化铟钛钽铈粉末。
实施例8
一种氧化铟钛钽铈粉末,由以下步骤制得:
步骤1:将1000ml的1.0mol/L氯化铟溶液、70ml的0.4mol/L氯化钛溶液、60ml的0.5mol/L氯化钽溶液和50ml的0.3mol/L氯化铈溶液进行混合,再向其中滴加、摩尔浓度为3.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、75℃烘干、研磨后,得到粒径D50为0.265μm、D90为0.681μm的氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在880℃进行煅烧6h,即得所述氧化铟钛钽铈粉末。
实施例9
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将950ml的1.05mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
实施例10
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将920ml的1.09mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
实施例11
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将880ml的1.14mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
实施例12
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将850ml的1.18mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
实施例13
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将650ml的1.54mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
对比例1
一种氧化铟钛钽铈粉末,制备方法大体同实施例1,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、50ml的0.2mol/L硝酸钛溶液、50ml的0.2mol/L硝酸钽溶液和50ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为5.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为8的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在800℃进行煅烧8h,即得所述氧化铟钛钽铈粉末。
对比例2
一种氧化铟钛钽铈粉末,制备方法大体同实施例1,由以下步骤制得:
步骤1:将1000ml的1.0mol/L硝酸铟溶液、50ml的0.2mol/L硝酸钛溶液、50ml的0.2mol/L硝酸钽溶液和50ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为5.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为10的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在800℃进行煅烧8h,即得所述氧化铟钛钽铈粉末。
对比例3
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将3000ml的0.33mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
对比例4
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将500ml的2.0mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
对比例5
一种氧化铟钛钽铈粉末,制备方法大体同实施例2,由以下步骤制得:
步骤1:将400ml的2.5mol/L硝酸铟溶液、20ml的0.2mol/L硝酸钛溶液、20ml的0.2mol/L硝酸钽溶液和20ml的0.2mol/L硝酸铈溶液进行混合,再向其中滴加摩尔浓度为4.0mol/L的氢氧化钠沉淀剂进行反应得到pH值为7的溶液A;
步骤2:将溶液A经过固液分离得到固体,将固体依次经过纯水洗涤、70℃烘干、研磨后,得到氧化铟钛钽铈前驱体;
步骤3:将氧化铟钛钽铈前驱体在780℃进行煅烧7h,即得所述氧化铟钛钽铈粉末。
结果测试
测试方法1:ICP发射光谱仪测试氧化铟钛钽铈粉末中各物质的含量
结果如表1所示
表1:实施例1-8和对比例1-5粉末中各氧化物的含量测试结果:
测试方法2:靶材的物理性能的测试
将实施例和对比例的氧化铟钛钽铈粉末制备成为靶材,靶材的制作方法大致为:
将氧化铟钛钽铈粉末进行模压、冷等静压成型得到靶材素坯;再将靶材素坯烧结即可得到氧化铟钛钽铈靶材。
针对制备的靶材,测试其电阻率和孔隙率(100nm-300nm)。
测试结果如下表2
表2实施例和对比例的物理性能的测试结果
电阻率(mΩ﹒cm) | 孔隙率(个/2600um2) | |
实施例2 | 1.33 | 9 |
实施例8 | 1.37 | 10 |
实施例9 | 1.30 | 8 |
实施例10 | 1.19 | 6 |
实施例11 | 1.16 | 6 |
实施例12 | 1.23 | 7 |
实施例13 | 1.45 | 10 |
对比例3 | 1.74 | 12 |
对比例4 | 1.66 | 11 |
对比例5 | 1.69 | 11 |
结果分析:
1.参考实施例2、实施例9-13可以发现,当硝酸铟溶液浓度在1.05-1.14mol/L时,其整体的孔隙率和电导率(即电阻率的降低)是有明显改善的。
2.参考实施例2和对比例3-5可以发现,硝酸铟溶液浓度过高或过低,对于电导率和孔隙率都是有害的,我们认为,过低的浓度导致沉淀发生团聚,不利于沉淀的均布;过高的浓度导致沉淀浓度过大,如果要达到和实施例2相类似的结果需要以更有力、更快的速度进行搅拌分散。
3.参考实施例2和对比例1和2可以发现,pH偏碱性,会导致钛流失。
通过以上实施例和对比例可以得到,控制铟金属离子的浓度、pH值,可有效降低靶材的孔隙率和电阻率,从而提高靶材的性能
本文所呈现的实施例仅是根据所有可能的实施例的组合选择的实施方式。所附的权利要求不应受说明本发明的实施方式所限制。在权利要求中所用的一些数值范围包括在其之内的子范围,这些范围中的变化也应为所附的权利要求覆盖。
Claims (7)
1.一种氧化铟钛钽铈粉末的制备方法,其特征在于,将含铟离子、钛离子、钽离子、铈离子的溶液和碱性沉淀剂反应,过滤得到沉淀,将沉淀经研磨、煅烧后制得氧化铟钛钽铈粉末;
所述溶液中铟离子的浓度为0.8~1.2M;
溶液和碱性沉淀剂反应的反应终点为溶液pH为中性;
所述溶液中铟离子、钛离子、钽离子、铈离子的摩尔比为1:0.001-0.05:0.001-0.05:0.001-0.05;
研磨后的粉末粒径为:D50为0.1μm-0.5μm,D90为0.5μm-1.0μm;
煅烧的温度为700-900℃,煅烧时间为6-10h。
2.根据权利要求1所述的氧化铟钛钽铈粉末的制备方法,其特征在于,所述溶液中铟离子、钛离子、钽离子、铈离子的摩尔比为1:0.002-0.02:0.002-0.02:0.002-0.02。
3.根据权利要求1所述的氧化铟钛钽铈粉末的制备方法,其特征在于,所述溶液中的阴离子为氯离子、硫酸根离子、硝酸根离子中的一种或多种。
4.根据权利要求1所述的氧化铟钛钽铈粉末的制备方法,其特征在于,所述碱性沉淀剂为NaOH、KOH、氨水中的一种或多种。
5.根据权利要求1所述的氧化铟钛钽铈粉末的制备方法,其特征在于,所述碱性沉淀剂以滴加的方式加入到溶液中,所述碱性沉淀剂的浓度为2.0M~6.0M。
6.根据权利要求1所述的氧化铟钛钽铈粉末的制备方法,其特征在于,所述溶液中铟离子的浓度为0.9~1.1M。
7.一种氧化铟钛钽铈粉末,其特征在于,采用如权利要求1-6任一所述方法制备得到。
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