CN114014349B - 一种yag纳米粉体的制备方法 - Google Patents
一种yag纳米粉体的制备方法 Download PDFInfo
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- CN114014349B CN114014349B CN202111326010.0A CN202111326010A CN114014349B CN 114014349 B CN114014349 B CN 114014349B CN 202111326010 A CN202111326010 A CN 202111326010A CN 114014349 B CN114014349 B CN 114014349B
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- salt
- yttrium
- nano powder
- yag
- aluminum
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 16
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 13
- 150000003746 yttrium Chemical class 0.000 claims abstract description 12
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000001412 amines Chemical class 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- -1 alcohol amine Chemical class 0.000 claims description 21
- 229910052727 yttrium Inorganic materials 0.000 claims description 19
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 19
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 17
- 150000003839 salts Chemical class 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052723 transition metal Inorganic materials 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000003570 air Substances 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 229930091371 Fructose Natural products 0.000 claims description 5
- 239000005715 Fructose Substances 0.000 claims description 5
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 5
- 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 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- RUFPHBVGCFYCNW-UHFFFAOYSA-N 1-naphthylamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1 RUFPHBVGCFYCNW-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- HMFHBZSHGGEWLO-SOOFDHNKSA-N D-ribofuranose Chemical compound OC[C@H]1OC(O)[C@H](O)[C@@H]1O HMFHBZSHGGEWLO-SOOFDHNKSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- 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 claims description 2
- PYMYPHUHKUWMLA-LMVFSUKVSA-N Ribose Natural products OC[C@@H](O)[C@@H](O)[C@@H](O)C=O PYMYPHUHKUWMLA-LMVFSUKVSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- HMFHBZSHGGEWLO-UHFFFAOYSA-N alpha-D-Furanose-Ribose Natural products OCC1OC(O)C(O)C1O HMFHBZSHGGEWLO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 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 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical group OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 150000003624 transition metals Chemical class 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 10
- 230000002776 aggregation Effects 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004220 aggregation Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 10
- 238000001354 calcination Methods 0.000 description 7
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 6
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 description 6
- UBOOKRVGOBKDMM-UHFFFAOYSA-N 3h-imidazo[4,5-c]pyridine Chemical compound C1=NC=C2NC=NC2=C1 UBOOKRVGOBKDMM-UHFFFAOYSA-N 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 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 description 4
- IINACGXCEZNYTF-UHFFFAOYSA-K trichloroyttrium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Y+3] IINACGXCEZNYTF-UHFFFAOYSA-K 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- GZCGUPFRVQAUEE-VANKVMQKSA-N aldehydo-L-glucose Chemical compound OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)C=O GZCGUPFRVQAUEE-VANKVMQKSA-N 0.000 description 3
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 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 3
- JVYYYCWKSSSCEI-UHFFFAOYSA-N europium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JVYYYCWKSSSCEI-UHFFFAOYSA-N 0.000 description 3
- XWFVFZQEDMDSET-UHFFFAOYSA-N gadolinium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XWFVFZQEDMDSET-UHFFFAOYSA-N 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- LXXCECZPOWZKLC-UHFFFAOYSA-N praseodymium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O LXXCECZPOWZKLC-UHFFFAOYSA-N 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- GDQXQVWVCVMMIE-UHFFFAOYSA-N dinitrooxyalumanyl nitrate hexahydrate Chemical compound O.O.O.O.O.O.[Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GDQXQVWVCVMMIE-UHFFFAOYSA-N 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940000406 drug candidate Drugs 0.000 description 1
- 239000003777 experimental drug Substances 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
- C01F17/34—Aluminates, e.g. YAlO3 or Y3-xGdxAl5O12
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
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- 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
- C04B35/44—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 aluminates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
一种YAG纳米粉体的制备方法,包括如下步骤:将糖类和有机胺类置于容器中,在25‑180℃条件下搅拌混合2‑120min,熔融得到澄清透明混合液;向澄清透明混合液中加入钇盐和铝盐,继续在25‑180℃温度下加热搅拌5‑120min形成均匀的熔融混合物;将熔融混合物加热使得糖类脱水碳化得到黑褐色蓬松固体;将黑褐色蓬松固体于800‑1500℃热处理2‑40h得到YAG纳米粉体。该方法能简化工艺流程、缩短制备周期、降低生产成本,还能减少颗粒聚集的情况;制备出的纳米粉形状规则、粒径均一、粉体流动性和填充性好、纯度高。
Description
技术领域
本发明属于陶瓷材料制备技术领域,具体涉及一种YAG纳米粉体的制备方法。
背景技术
YAG(钇铝石榴石,Y3Al5O12)属于立方晶系,具有石榴石型结构,因具有高折射、光学各向同性等光学性能而被广泛用作光学材料。另外,在已知的透明陶瓷材料中,YAG凭借高强度、高温蠕变小、抗氧化、热导率低等优点被逐渐引起广泛关注和研究,是一种很有潜力的精细结构陶瓷材料。
YAG荧光粉是工业化生产白光LED的主要荧光材料(Yang,et.al.J.Lumin.,2018,204:157-161.;Lee,et.al.2018,199(5):24-30)。但由于受工艺与成本等因素的限制,YAG荧光粉在LED器件的大规模应用还有待继续发展。常规的固相法虽然工艺相对简单、成本较低、产量大,但是其煅烧温度高,团聚严重(Veith.,et.al.J.Mater.Chem.,1999,9:3069–3079.);溶胶-凝胶法获得的YAG颗粒均匀,粒度能达到纳米级,但工艺复杂、效率低、前驱体煅烧反应中容易产生硬团聚,不利于后期陶瓷烧结(Yang.,et.al.J.Alloy Compd.,2009,484:449–451.);沉淀法的优点在于焙烧温度较低、操作简单、成本低廉、易于实现大规模生产,但难以控制体系合适的pH值,使各个成分沉降均匀、难以洗涤(马飞.共沉淀法制备YAG:Ce3+纳米荧光粉[J].广州化工,2018,46(18):51-53.);水热法可以合成形貌较好、粒度分布均匀且分散性良好的YAG粉体,然而高温高压对设备要求较高且制备成本较高,难以实现大规模生产(Yang.,et.al.Mater.Lett.,2009,63:2271–2273.);喷雾干燥法制备的YAG具有良好流动性、填充性及高组分均匀性,该方法大多情况下需要通过添加多种粘结剂、分散剂和增塑剂,工艺流程繁琐,制备周期长,且极易引入杂质,影响YAG粉体及陶瓷性能(You.,et.al.Ceram.Int.,2013,39:3987–3992.)。
综上所述,目前采用传统方法制备出的YAG粉体均存在严重团聚、形状不规则,粉体流动性和填充性差、纯度无法保证,工艺流程复杂繁琐,制备周期长等问题,直接影响YAG粉体及陶瓷的性能。
发明内容
本发明的目的在于提供一种YAG纳米粉体的制备方法,该方法一方面能简化工艺流程、缩短制备周期、降低生产成本,另一方面还能减少颗粒聚集的情况;所制备出的YAG纳米粉可具有形状规则、粒径均一、粉体流动性和填充性好、纯度高等优点。
为实现上述目的,本发明采用的技术方案是:一种YAG纳米粉体的制备方法,包括如下步骤:
(1)将糖类和有机胺类按照一定比例混合置于容器中,在25-180℃加热条件下搅拌混合2-120min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入一定比例的钇盐和铝盐,继续在25-180℃温度下加热搅拌5-120min,使金属盐完全溶解形成均匀的熔融混合物;
(3)将均匀的熔融混合物加热使得糖类脱水碳化得到黑褐色蓬松固体;
(4)将黑褐色蓬松固体于800-1500℃热处理2-40h得到YAG纳米粉体。
进一步的,步骤(2)中,向澄清透明混合液中再加入稀土盐或过渡金属盐。
优选的,步骤(1)中,糖类为葡萄糖、蔗糖、果糖、乳糖、淀粉、麦芽糖和核糖中的一种或几种;有机胺类为脂肪胺类、醇胺类、酰胺类、脂环胺类、芳香胺类或萘系胺类;糖类和有机胺类的质量比为1:(0.1-50)。
优选的,步骤(2)中,钇盐中的钇元素与铝盐中的铝元素之间的摩尔比为1:(1-4)。
优选的,步骤(2)中,稀土盐中的稀土元素或过渡金属盐中的过渡金属元素与钇盐中的钇元素的摩尔比为1:(10-300)。
优选的,步骤(2)中,钇盐中的钇元素、铝盐中的铝元素、稀土盐中的稀土元素或过渡金属盐中的过渡金属元素总摩尔量与糖类之间的摩尔比为(0.2-3):1。
优选的,步骤(2)中,钇盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种;铝盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种;稀土盐或过渡金属盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种。
优选的,步骤(3)中,加热的方式有为高温碳化、水热碳化、微波碳化中的一种。
优选的,步骤(4)中,热处理的氛围为三种氛围中的一种,三种氛围分别为空气、氧气、先惰性气体再空气或氧气。
优选的,步骤(4)中,得到的YAG纳米粉体粒径为20-5000nm;优选为20-100nm。
本发明通过控制原料配比、反应温度、微波条件、煅烧温度和时长等合成条件能够有效调控材料的大小、纯度。本发明先将糖类和有机胺混合形成均相共融体系,再添加钇盐、铝盐,通过搅拌使金属盐均匀分布在混合液体中。有机胺在加热过程中少部分会被分解,在该过程能够不断产生氨气溶于混合溶液提供弱碱性环境,可以有效防止YAG在生长过程中团聚;另外,微波加热后其中的糖类迅速碳化,提供了碳模板能使金属盐均匀分布碳模板上也能有效防止YAG的团聚,而且煅烧过程中碳模板能够被轻易的除去得到高纯的YAG纳米粉体。该方法一方面简化了工艺流程、缩短了制备周期、降低了生产成本,另一方面还减少了颗粒聚集的情况;所制备出的YAG纳米粉具有形状规则、粒径均一、粉体流动性和填充性好、纯度高等优点,适于工业化生产。
附图说明
图1为实施例一中材料YAG的SEM图;
图2为实施例二中材料YAG:Ce3+-1的XRD谱图;
图3为实施例五中材料YAG:Ce3+-4的SEM图;
图4为实施例二至实施例五中材料YAG:Ce3+的发射荧光谱图;
图5为实施例六中材料YAG:Eu3+的XRD图;
图6为实施例七中材料YAG:Gd3+的XRD图;
图7为实施例八中材料YAG:Pr3+的XRD图。
具体实施方式
以下结合附图和具体实施例对本发明作进一步详细说明。
以下实施例中的实验药品除特别说明外,均通过市购得到并直接使用。
实施例一
一种YAG纳米粉体的制备方法,该方法包括如下步骤:
(1)将葡萄糖(3.0g)(0.0167mol)和尿素(5.0g)(0.0831mol)置于烧杯中,加热至100℃搅拌混合20min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入六水硝酸钇(0.77g)(0.002mol)、九水硝酸铝(1.26g)(0.0033mol),继续在100℃温度下加热搅拌120min,使金属盐完全溶解形成均匀且粘稠的熔融混合物;六水硝酸钇中的钇元素与九水硝酸铝中的铝元素的摩尔比为1:1.65;
(3)将熔融混合物微波加热10min,微波功率550W,使得葡萄糖脱水碳化得到黑褐色蓬松固体,然后将烧杯取出;
(4)将黑褐色蓬松固体放入箱式炉中,在空气氛围下于800℃热处理2h得到YAG纳米粉体,粒径为20nm。
从图1中可以看出,该方法制得的YAG分散良好。
实施例二
一种YAG纳米粉体的制备方法,该方法包括如下步骤:
(1)将葡萄糖(3.0g)(0.0167mol)和尿素(5.0g)(0.0831mol)置于烧杯中,加热至100℃搅拌混合20min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入六水硝酸钇(0.77g)(0.002mol)、九水硝酸铝(1.26g)(0.0033mol)、六水硝酸铈(0.01g)(0.000023mol),继续在100℃温度下加热搅拌120min,使金属盐完全溶解形成均匀且粘稠的熔融混合物;六水硝酸钇中的钇元素与九水硝酸铝中的铝元素的摩尔比为1:1.65;六水硝酸铈中的铈元素和六水硝酸钇中的钇元素的摩尔比为1:86.96;葡萄糖与六水硝酸钇中的钇元素、九水硝酸铝中的铝元素、六水硝酸铈中的铈元素总摩尔之比为1:0.32;
(3)将熔融混合物微波加热4min,微波功率700W,使得葡萄糖脱水碳化得到黑褐色蓬松固体,然后将烧杯取出;
(4)将黑褐色蓬松固体放入箱式炉中,在空气氛围下于800℃热处理2h得到稀土掺杂YAG纳米粉体YAG:Ce3+-1,粒径为20nm。
从图2中可以看出,该方法制得的产物与标准PDF卡片对应,说明制备的产物为YAG:Ce3+,峰行窄而尖锐则说明制得的YAG:Ce3+晶型良好,没有杂峰则说明制得的YAG:Ce3+纯度较高。
实施例三至实施例五分别与实施例二的区别仅仅在于煅烧温度分别为900℃、1000℃、1100℃,其他步骤均与实施例保持一致。通过实施例三至实施例五分别制备得到稀土掺杂YAG纳米粉体YAG:Ce3+-2、YAG:Ce3+-3、YAG:Ce3+-4。
从图3中可以看出,实施例五制得的YAG:Ce3+-4颗粒较小,粒径较为均一,分散性较好。
从图4中可以看出,本发明制得的YAG:Ce3+有较好的荧光性能,且可以通过调整煅烧温度得到不同荧光强度的纳米粉体;随着煅烧温度的升高,纳米粉体的荧光性能增强。
实施例六
一种YAG纳米粉体的制备方法,该方法包括如下步骤:
(1)将蔗糖(1.0g)(0.0029mol)和乙二胺(10.0g)(0.166mol)置于烧杯中,加热至180℃搅拌混合120min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入六水氯化钇(1.22g)(0.004mol)、异丙醇铝(1.01g)(0.004mol)、六水硝酸铕(0.18g)(0.0004mol),继续在180℃温度下加热搅拌80min,使金属盐完全溶解形成均匀且粘稠的熔融混合物;六水氯化钇中的钇元素与异丙醇铝中的铝元素的摩尔比为1:1;六水硝酸铕中的铕元素和六水氯化钇中的钇元素的摩尔比为1:10;蔗糖与六水氯化钇中的钇元素、异丙醇铝中的铝元素、六水硝酸铕中的铕元素总摩尔之比为1:2.89;
(3)将熔融混合物放于180℃烘箱24h,使得蔗糖脱水碳化得到黑褐色蓬松固体,然后将烧杯取出;
(4)将黑褐色蓬松固体放入箱式炉中,在空气氛围下于850℃热处理15h得到稀土掺杂YAG纳米粉体YAG:Eu3+,粒径为70nm。
从图5中可以看出,本实施例制备出YAG:Eu3+晶型良好且不含杂峰。
实施例七
一种YAG纳米粉体的制备方法,该方法包括如下步骤:
(1)将葡萄糖(50.0g)(0.2775mol)和乙醇胺(5.0g)(0.0831mol)置于烧杯中,加热至25℃搅拌混合25min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入草酸钇(3.55g)(0.00803mol)、无水硫酸铝(11.07g)(0.03212mol)、六水硝酸钆(0.024g)(0.000054mol),继续在25℃温度下加热搅拌120min,使金属盐完全溶解形成均匀且粘稠的熔融混合物;草酸钇中的钇元素与无水硫酸铝中的铝元素的摩尔比为1:4;六水硝酸钆中的钆元素和草酸钇中的钇元素的摩尔比为1:297.41;葡萄糖与草酸钇中的钇元素、无水硫酸铝中的铝元素、六水硝酸钆中的钆元素总摩尔之比为1:0.29;
(3)将熔融混合物转移进水热反应釜,于200℃水热3h,使得葡萄糖脱水碳化得到黑褐色蓬松固体,然后将样品从水热釜中取出;
(4)将黑褐色蓬松固体放入箱式炉中,在氧气氛围下于900℃热处理20h得到稀土掺杂YAG纳米粉体YAG:Gd3+,粒径为120nm。
从图6中可以看出,本实施例制备出的YAG:Gd3+晶型良好且不含杂峰。
实施例八
一种YAG纳米粉体的制备方法,该方法包括如下步骤:
(1)将果糖(1.0g)(0.00555mol)和聚乙烯亚胺(50.0g)(0.167mol)置于烧杯中,加热至108℃搅拌混合2min,熔融得到澄清透明混合液;
(2)向澄清透明混合液中加入八水硫酸钇(0.62g)(0.001mol)、九水硝酸铝(1.81g)(0.0047mol)、六水硝酸镨(0.012g)(0.000027mol),继续在108℃温度下加热搅拌5min,使金属盐完全溶解形成均匀且粘稠的熔融混合物;八水硫酸钇中的钇元素与九水硝酸铝中的铝元素的摩尔比为1:2.35;六水硝酸镨中的镨元素和八水硫酸钇中的钇元素的摩尔比为1:74;果糖与八水硫酸钇中的钇元素、九水硝酸铝中的铝元素、六水硝酸镨中的镨元素总摩尔之比为1:1.21;
(3)将熔融混合物微波加热8min,微波功率100kW,使得果糖脱水碳化得到黑褐色蓬松固体,然后将烧杯取出;
(4)将黑褐色蓬松固体放入箱式炉中,在氮气氛围下于1500℃先热处理20h,再在空气氛围下800℃热处理20h,得到稀土掺杂YAG纳米粉体YAG:Pr3+,粒径为5000nm。
从图7中可以看出,本实施例制备出的YAG:Pr3+晶型良好且不含杂峰。
Claims (5)
1.一种YAG纳米粉体的制备方法,其特征在于,包括如下步骤:
(1)将糖类和有机胺类按照一定比例混合置于容器中,在25-180℃加热条件下搅拌混合2-120min,熔融得到澄清透明混合液;糖类为葡萄糖、蔗糖、果糖、乳糖、淀粉、麦芽糖和核糖中的一种或几种;有机胺类为脂肪胺类、醇胺类、酰胺类、脂环胺类、芳香胺类或萘系胺类;糖类和有机胺类的质量比为1:(0.1-50);
(2)向澄清透明混合液中加入一定比例的钇盐、铝盐和稀土盐或过渡金属盐,继续在25-180℃温度下加热搅拌5-120min,使金属盐完全溶解形成均匀的熔融混合物;钇盐中的钇元素与铝盐中的铝元素之间的摩尔比为1:(1-4);钇盐中的钇元素、铝盐中的铝元素、稀土盐中的稀土元素或过渡金属盐中的过渡金属元素总摩尔量与糖类之间的摩尔比为(0.2-3):1;
(3)将均匀的熔融混合物加热使得糖类脱水碳化得到黑褐色蓬松固体;
(4)将黑褐色蓬松固体于800-1500℃热处理2-40h得到粒径为20-5000nm的YAG纳米粉体。
2.根据权利要求1所述的一种YAG纳米粉体的制备方法,其特征在于,步骤(2)中,稀土盐中的稀土元素或过渡金属盐中的过渡金属元素与钇盐中的钇元素的摩尔比为1:(10-300)。
3.根据权利要求1所述的一种YAG纳米粉体的制备方法,其特征在于,步骤(2)中,钇盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种;铝盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种;稀土盐或过渡金属盐为硝酸盐、硫酸盐、草酸盐、醋酸盐、磷酸盐、次氯酸盐、卤化盐中的一种。
4.根据权利要求1所述的一种YAG纳米粉体的制备方法,其特征在于,步骤(3)中,加热的方式有为高温碳化、水热碳化、微波碳化中的一种。
5.根据权利要求1所述的一种YAG纳米粉体的制备方法,其特征在于,步骤(4)中,热处理的氛围为三种氛围中的一种,三种氛围分别为空气、氧气、先惰性气体再空气或氧气。
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