CN117886604A - 一种氧化钇稳定化氧化锆粉体的制备方法 - Google Patents
一种氧化钇稳定化氧化锆粉体的制备方法 Download PDFInfo
- Publication number
- CN117886604A CN117886604A CN202311752279.4A CN202311752279A CN117886604A CN 117886604 A CN117886604 A CN 117886604A CN 202311752279 A CN202311752279 A CN 202311752279A CN 117886604 A CN117886604 A CN 117886604A
- Authority
- CN
- China
- Prior art keywords
- yttrium
- solution
- zirconium
- stabilized zirconia
- yttria
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 41
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 41
- -1 yttrium ions Chemical class 0.000 claims abstract description 31
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000008139 complexing agent Substances 0.000 claims abstract description 20
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 15
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 4
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 4
- 229940093429 polyethylene glycol 6000 Drugs 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 4
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910021525 ceramic electrolyte Inorganic materials 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002001 electrolyte material Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 239000012720 thermal barrier coating Substances 0.000 claims description 3
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 235000013877 carbamide Nutrition 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000004220 glutamic acid Substances 0.000 claims description 2
- 235000013922 glutamic acid Nutrition 0.000 claims description 2
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 2
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 claims description 2
- IBSDADOZMZEYKD-UHFFFAOYSA-H oxalate;yttrium(3+) Chemical compound [Y+3].[Y+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O IBSDADOZMZEYKD-UHFFFAOYSA-H 0.000 claims description 2
- LRVUGEZGBKPRRZ-UHFFFAOYSA-L oxygen(2-);zirconium(4+);dichloride Chemical compound [O-2].[Cl-].[Cl-].[Zr+4] LRVUGEZGBKPRRZ-UHFFFAOYSA-L 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000002431 foraging effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 7
- GNKHOVDJZALMGA-UHFFFAOYSA-N [Y].[Zr] Chemical compound [Y].[Zr] GNKHOVDJZALMGA-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 238000000975 co-precipitation Methods 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 229910002080 8 mol% Y2O3 fully stabilized ZrO2 Inorganic materials 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- RVRKDGLTBFWQHH-UHFFFAOYSA-N yttrium zirconium Chemical compound [Y][Zr][Y] RVRKDGLTBFWQHH-UHFFFAOYSA-N 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3246—Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/449—Organic acids, e.g. EDTA, citrate, acetate, oxalate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Composite Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种氧化钇稳定化氧化锆粉体的制备方法。一种氧化钇稳定化氧化锆粉体的制备方法,包括如下步骤:S1、将锆源无机盐溶解在水中,然后加入钇源无机盐,获得含锆和钇离子的澄清水溶液;S2、取络合剂溶解在水和乙醇的混合溶液中,再加入澄清水溶液中,混合均匀获得胶状水溶液;S3、将分散剂的水溶液加入溶胶状水溶液中,搅拌至溶液澄清;S4、将碱性沉淀剂溶液滴入溶液中,直至锆钇离子完全沉淀后,再静止陈化,过滤、洗涤并真空冷冻干燥获得干燥粉;S5、将干燥粉进行焙烧,冷却至室温,获得目标产物。本发明提出的制备方法可以更容易地控制氧化钇稳定化氧化锆的颗粒形状及尺寸,且此方法操作简单、原料易得、利于工业化生产。
Description
技术领域:
本发明涉及无机非金属材料制备技术领域,具体涉及一种氧化钇稳定化氧化锆粉体的制备方法。
背景技术:
氧化锆陶瓷材料在工业上具有广泛的应用。由于氧化锆在高温时会发生相转变,通常在使用氧化锆作为功能陶瓷时需要添加一定量的稳定剂,常用的稳定剂有氧化钇、氧化钙、氧化镁等,其中以氧化钇尤为多。实际应用的氧化钇稳定化氧化锆材料还会再添加其它金属或非金属元素,而其性能的优劣经常受初始氧化钇稳定氧化锆粉体的影响,包括初始粉体的粒径大小、稳定剂分布均匀性等因素,而这些因素与初始粉体的制备方法密切相关。
氧化钇稳定化氧化锆的制备方主要有:水热法、溶胶凝胶法、共沉淀法、机械混合法等。(1)水热沉淀法是在工业生产上较常采用的方法。通过对含有锆源、钇源以及沉淀剂的水溶液加热、加压,在经历较长的反应时间后,反应沉淀物发生溶解-重结晶过程,最终经洗涤干燥后便得到氧化钇稳定氧化锆粉体。由于水热沉淀法存在对设备要求高,工艺参数控制难、生产周期较长的缺点,在工业上较少使用。(2)溶胶凝胶法通常是在含有锆盐、钇盐的水溶液中加入螯合剂生成溶胶,然后再经凝胶化后获得含有锆钇元素的有机前驱体,最后经过煅烧得到氧化钇稳定氧化锆粉体。该方法的缺点是溶胶在凝胶过程中存在着周期长、干燥时易发生团聚导致收缩率大、操作复杂等,导致工业化程度较低。(3)共沉淀法是工业上最常用的方法之一,通常是将含有锆和钇的无机盐溶解在水中,再加入沉淀剂将锆钇离子从溶液中沉淀析出,通过收集并洗涤沉淀物再经煅烧便可获得氧化钇稳定氧化锆粉末。共沉淀法具有工艺简单、成本低廉等优点。但是氧化钇稳定化氧化锆的颗粒形状及尺寸不易控制,亟待解决该问题。
发明内容:
为了解决现有技术存在的问题,本发明提出一种氧化钇稳定化氧化锆粉体的制备方法,本发明利用络合剂、分散剂的作用将锆、钇离子络合后均匀分布在溶液中,控制溶液的pH值,加入沉淀剂,获得无硬团聚的锆钇前驱体粉末,最终经煅烧工艺得到氧化钇稳定化氧化锆纳米粉体,该制备方法可以更容易地控制氧化钇稳定化氧化锆的颗粒形状及尺寸,且此方法操作简单、原料易得、利于工业化生产。
本发明的目的是提供一种氧化钇稳定化氧化锆粉体的制备方法,包括如下步骤:
S1、将锆源无机盐溶解在水中,然后按钇:锆摩尔比为0.15~0.50:1的比例加入钇源无机盐,获得含锆和钇离子的澄清水溶液;
S2、取络合剂溶解在水和乙醇的混合溶液中,再加入步骤S1得到的澄清水溶液中,混合均匀获得含锆和钇离子络合成的溶胶状水溶液;
S3、将分散剂的水溶液加入步骤S2得到的溶胶状水溶液中,搅拌至溶液澄清;
S4、将pH值为10的碱性沉淀剂溶液滴入步骤S3得到的溶液中,并且保持步骤S3的溶液始终处于搅拌状态中,温度为50℃~70℃;直至锆钇离子完全沉淀后,再静止陈化5~7小时,过滤、洗涤并真空冷冻干燥获得干燥粉;
S5、将步骤S4得到的干燥粉进行焙烧,焙烧工艺为:以4~6℃/min的升温速率升至350℃~450℃,保温0.5~1.5小时,再以4~6℃/min的升温速率升至900℃~1100℃,保温5~7小时,随后冷却至室温,获得目标产物氧化钇稳定化氧化锆粉体。
本发明提出通过共沉淀制备氧化钇稳定化氧化锆的方法,其利用络合剂、分散剂、沉淀剂获得无团聚的锆钇有机前驱体粉末,最终经煅烧工艺得到氧化钇稳定化氧化锆纳米粉体。
优选地,步骤S1所述的锆源无机盐选自硝酸锆、硝酸氧锆和二氯氧锆中的一种。锆离子的摩尔浓度为0.15~0.25mol/L。
优选地,步骤S1所述的钇源无机盐选自草酸钇、硝酸钇、乙酸钇和碳酸钇中的一种。钇离子的摩尔浓度为0.03~0.04mol/L。
优选地,步骤S2所述的络合剂选自柠檬酸、谷氨酸、乙二胺四乙酸二钠和酒石酸中的一种,所述的络合剂与锆离子的摩尔比为(0.2~1):1。
进一步优选,步骤S2所述的混合溶液中水和乙醇的体积比为2:(0.5~1)。络合剂溶于水和乙醇的混合溶剂中得到摩尔浓度为0.3~0.4mol/L的络合剂溶液。
优选地,步骤S3所述的分散剂选自聚乙二醇6000、十二烷基苯磺酸钠和十六烷基三甲基溴化铵中的一种,所述的分散剂在分散剂的水溶液中的质量分数占比为0.2%~1%。
优选地,步骤S4所述的碱性沉淀剂选自碳酸氢铵、碳酸铵、氨水、氢氧化钠和尿素中的一种,碱性沉淀剂与锆离子的摩尔比为(1~2):1。
优选地,步骤S5焙烧工艺为:以5℃/min的升温速率升至400℃,保温1小时,再以5℃/min的升温速率升至1000℃,保温6小时。
本发明还保护根据上述制备方法得到的氧化钇稳定化氧化锆粉体,所述的氧化钇稳定化氧化锆粉体粒径大小为50~200nm,比表面积为10~100m2/g。
本发明还保护所述的氧化钇稳定化氧化锆粉体在制备热障涂层用材料、固态陶瓷电解质材料或其它功能陶瓷材料中的应用。
本发明跟现有技术相比具有如下优点:
1、本发明利用络合剂和分散剂将锆钇离子均匀分散在乙醇/水混合溶剂中获得含锆钇离子的溶胶状溶液,再通过中和沉淀获得高分散度的锆钇前驱体,并经过滤洗涤以及真空冷冻干燥,最终经煅烧工艺得到氧化钇稳定化氧化锆粉体。
2、本发明制备的氧化钇稳定化氧化锆纳米粉体为全稳定化氧化锆粉体,粒径大小为50~200nm,比表面积为10~100m2/g,可应用于热障涂层用材料、固体氧化物燃料电池的固态陶瓷电解质材料以及其它功能陶瓷等领域。
附图说明:
图1为实施例1所制备的氧化钇稳定化氧化锆的扫描电子显微镜图。
图2为实施例1所制备的氧化钇稳定化氧化锆的X射线衍射图。
图3为实施例1所制备的氧化钇稳定化氧化锆的激光粒径分布图。
具体实施方式:
下面将结合本发明实施例,对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。除特别说明,本发明使用的设备和试剂为本技术领域常规市购产品。
实施例1
一种氧化钇稳定化氧化锆粉体的制备方法,包括如下步骤:
(1)在室温常压下,称取32.23g八水合二氯氧锆和1.8g氧化钇溶解在去离子水中,溶解完全后溶液总体积为500mL,配制成含钇锆离子的溶液,其中锆离子的摩尔浓度为0.2mol/L,钇离子的摩尔浓度为0.032mol/L;
(2)称取6.8g乙二胺四乙酸二钠,溶解在体积比为3:1的乙醇/水溶液中,总体积为50mL;将此乙二胺四乙酸二钠溶液倒入步骤(1)含钇锆离子的溶液中,在60℃水浴中磁力搅拌0.5小时至混合溶液呈无色澄清溶胶状溶液;
(3)称取2.5g聚乙二醇6000,并溶解在50mL的水中;将此溶液倒入步骤(2)中的溶液中,保持60℃水浴中磁力搅拌0.5小时至溶液澄清,获得含有聚乙二醇6000分散后的锆钇溶胶状溶液;
(4)称取16g碳酸氢铵并配置成100mL的水溶液,将此溶液使用注射泵缓慢向步骤(3)的溶液滴加,滴加速率为3mL/min,滴加完全后继续在60℃水浴中磁力搅拌0.5小时,再从水浴锅中取出并静置0.5小时,得到透明胶状体(含大量水的锆钇凝胶体);
(5)将步骤(4)得到的透明胶状体冻干,再将该冻干物经真空冷冻干燥机干燥6小时(真空度为10Pa),得到白色粉体;将该白色粉体在空气气氛下,以5℃/min的升温速率升至400℃,保温1小时,再以5℃/min的升温速率升至1000℃,保温6小时,随后炉冷至室温,即可获得氧化钇稳定化氧化锆的纳米粉体。
对该实施例制备得到的氧化钇稳定氧化锆纳米粉体进行检测,粉体的微观形貌如图1所示为其扫描电镜照片,氧化钇稳定化氧化锆的粉末X射线衍射图谱如图2所示,激光动态光散射法测得的二次粒径分布图如图3所示,由图1~3可以得出:本实施例制备的氧化钇稳定氧化锆纳米粉体的微观形貌为不规则纳米颗粒状,大小为80~100nm左右,粉体的多晶X射线衍射的晶型为立方晶型8YSZ,粉体颗粒的二次粒径为D50=0.127μm,呈单分散性分布。
实施例2:
与实施例1相同,不同之处在于:
步骤(1)中钇:锆摩尔比为0.15:1,锆离子的摩尔浓度为0.15mol/L,钇离子的摩尔浓度为0.03mol/L。
步骤(2)中使用柠檬酸作为络合剂,络合剂与锆离子的摩尔比为0.2:1。络合剂溶于水和乙醇的混合溶剂中得到摩尔浓度为0.3mol/L的络合剂溶液。
步骤(3)中使用十二烷基苯磺酸钠作为分散剂,分散剂在水溶液中的质量分数为0.5%。
步骤(4)中使用氨水作为沉淀剂,沉淀剂与锆离子的摩尔比为1:1,保持步骤S3的溶液始终处于搅拌状态中,温度为50℃;直至锆钇离子完全沉淀后,再静止陈化5小时,过滤、洗涤并真空冷冻干燥获得干燥粉;
步骤(5)中焙烧工艺为:以4℃/min的升温速度升至350℃,保温1.5小时,再以4℃/min的升温速率升至900℃,保温7小时。
实施例3:
与实施例1相同,不同之处在于:
步骤(1)中钇:锆摩尔比为0.5:1,锆离子的摩尔浓度为0.25mol/L,钇离子的摩尔浓度为0.04mol/L。
步骤(2)中使用酒石酸作为络合剂,络合剂与锆离子的摩尔比为0.5:1。络合剂溶于水和乙醇的混合溶剂中得到摩尔浓度为0.4mol/L的络合剂溶液。
步骤(3)中使用十六烷基三甲基溴化铵作为分散剂,分散剂在水溶液中的质量分数为0.2%。
步骤(4)中沉淀剂与锆离子的摩尔比为2:1,保持步骤S3的溶液始终处于搅拌状态中,温度为70℃;直至锆钇离子完全沉淀后,再静止陈化7小时,过滤、洗涤并真空冷冻干燥获得干燥粉;
步骤(5)中焙烧工艺为:以6℃/min的升温速度升至450℃,保温0.5小时,再以6℃/min的升温速率升至1100℃,保温5小时。
以上实施例的说明只是用于帮助理解本发明的技术方案及其核心思想,应当指出,对于本技术领域的技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。
Claims (10)
1.一种氧化钇稳定化氧化锆粉体的制备方法,其特征在于,包括如下步骤:
S1、将锆源无机盐溶解在水中,然后按钇:锆摩尔比为0.15~0.50:1的比例加入钇源无机盐,获得含锆和钇离子的澄清水溶液;
S2、取络合剂溶解在水和乙醇的混合溶液中,再加入步骤S1得到的澄清水溶液中,混合均匀获得含锆和钇离子络合成的溶胶状水溶液;
S3、将分散剂的水溶液加入步骤S2得到的溶胶状水溶液中,搅拌至溶液澄清;
S4、将pH值为10的碱性沉淀剂溶液滴入步骤S3得到的溶液中,并且保持步骤S3的溶液始终处于搅拌状态中,温度为50℃~70℃;直至锆钇离子完全沉淀后,再静止陈化5~7小时,过滤、洗涤并真空冷冻干燥获得干燥粉;
S5、将步骤S4得到的干燥粉进行焙烧,焙烧工艺为:以4~6℃/min的升温速率升至350℃~450℃,保温0.5~1.5小时,再以4~6℃/min的升温速率升至900℃~1100℃,保温5~7小时,随后冷却至室温,获得目标产物氧化钇稳定化氧化锆粉体。
2.根据权利要求1所述的制备方法,其特征在于,步骤S1所述的锆源无机盐选自硝酸锆、硝酸氧锆和二氯氧锆中的一种。
3.根据权利要求1所述的制备方法,其特征在于,步骤S1所述的钇源无机盐选自草酸钇、硝酸钇、乙酸钇和碳酸钇中的一种。
4.根据权利要求1所述的制备方法,其特征在于,步骤S2所述的络合剂选自柠檬酸、谷氨酸、乙二胺四乙酸二钠和酒石酸中的一种,所述的络合剂与锆离子的摩尔比为(0.2~1):1。
5.根据权利要求4所述的制备方法,其特征在于,步骤S2所述的混合溶液中水和乙醇的体积比为2:(0.5~1)。
6.根据权利要求1所述的制备方法,其特征在于,步骤S3所述的分散剂选自聚乙二醇6000、十二烷基苯磺酸钠和十六烷基三甲基溴化铵中的一种,所述的分散剂在分散剂的水溶液中的质量分数占比为0.2%~1%。
7.根据权利要求1所述的制备方法,其特征在于,步骤S4所述的碱性沉淀剂选自碳酸氢铵、碳酸铵、氨水、氢氧化钠和尿素中的一种,碱性沉淀剂与锆离子的摩尔比为(1~2):1。
8.根据权利要求1所述的制备方法,其特征在于,步骤S5焙烧工艺为:以5℃/min的升温速率升至400℃,保温1小时,再以5℃/min的升温速率升至1000℃,保温6小时。
9.权利要求1所述的制备方法得到的氧化钇稳定化氧化锆粉体,其特征在于,所述的氧化钇稳定化氧化锆粉体粒径大小为50~200nm,比表面积为10~100m2/g。
10.权利要求9所述的氧化钇稳定化氧化锆粉体在制备热障涂层用材料、固态陶瓷电解质材料或其它功能陶瓷材料中的应用。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311752279.4A CN117886604A (zh) | 2023-12-19 | 2023-12-19 | 一种氧化钇稳定化氧化锆粉体的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311752279.4A CN117886604A (zh) | 2023-12-19 | 2023-12-19 | 一种氧化钇稳定化氧化锆粉体的制备方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN117886604A true CN117886604A (zh) | 2024-04-16 |
Family
ID=90646423
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311752279.4A Pending CN117886604A (zh) | 2023-12-19 | 2023-12-19 | 一种氧化钇稳定化氧化锆粉体的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117886604A (zh) |
-
2023
- 2023-12-19 CN CN202311752279.4A patent/CN117886604A/zh active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Shukla et al. | Reduced activation energy for grain growth in nanocrystalline yttria-stabilized zirconia | |
Hirano et al. | Preparation of monodispersed cerium (IV) oxide particles by thermal hydrolysis: influence of the presence of urea and Gd doping on their morphology and growth | |
CN110330333B (zh) | 一种制备纳米级钇稳定氧化锆复合粉体的方法 | |
CN109574073A (zh) | 一种高分散纳米氧化锆粉末的制备方法 | |
CN102923770B (zh) | 一种钇稳定纳米二氧化锆粉体的制备方法 | |
CN109437892A (zh) | 一种氧化锆陶瓷涂层及其制备方法 | |
CN105967687B (zh) | 一种颗粒级配的氧化锆粉体制备及陶瓷烧结方法 | |
CN108511797B (zh) | 一种Li7La3Zr2O12固体电解质制备方法 | |
CN106986381A (zh) | 一种松散含氢氧化锆或氧化锆纳米粉体的制备方法 | |
CN111960466B (zh) | 一种纳米氧化锆空心球的制备方法 | |
CN100417598C (zh) | 一种氧化钐掺杂稳定氧化锆纳米材料的制备方法 | |
CN1285511C (zh) | 柠檬酸燃烧法直接合成y2o3纳米材料的方法 | |
Yu et al. | Doping concentration of Eu3+ as a fluorescence probe for phase transformation of zirconia | |
CN102807239A (zh) | 一种镧系稀土掺杂纳米yag复合粉体的制备方法 | |
CN109336572A (zh) | 一种制备氧化物陶瓷的冷压烧结方法 | |
CN110963530B (zh) | 一种钽酸钇粉体的制备方法 | |
CN109111230A (zh) | 一种氧化钇-氧化镁纳米复合粉体及其制备方法 | |
Zhang et al. | Stirring speed assisted homogenization of precipitation reaction for enhanced optical performance of Y2O3 transparent ceramics | |
CN106241853B (zh) | 一种氧化钇纳米材料的制备方法 | |
CN109279893A (zh) | 钬铥双掺钆镓石榴石激光透明陶瓷制备方法 | |
CN108046217B (zh) | 纳米复合金属氧化物的制备方法 | |
CN117886604A (zh) | 一种氧化钇稳定化氧化锆粉体的制备方法 | |
CN104973624B (zh) | 一种网状四方相氧化锆纳米粉体的制备方法 | |
CN108609652A (zh) | 一种利用熔盐制备二氧化锆纳米粉体的方法 | |
CN112125663B (zh) | 一种单分散的氧化钇稳定氧化锆纳米粉体的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |