CN107805056A - The preparation method and ceramic composite of ceramic composite, light supply apparatus - Google Patents
The preparation method and ceramic composite of ceramic composite, light supply apparatus Download PDFInfo
- Publication number
- CN107805056A CN107805056A CN201610812030.1A CN201610812030A CN107805056A CN 107805056 A CN107805056 A CN 107805056A CN 201610812030 A CN201610812030 A CN 201610812030A CN 107805056 A CN107805056 A CN 107805056A
- Authority
- CN
- China
- Prior art keywords
- sintering aid
- ceramic composite
- green body
- ceramic
- sintering
- 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
- 239000000919 ceramic Substances 0.000 title claims abstract description 203
- 239000002131 composite material Substances 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 202
- 239000002994 raw material Substances 0.000 claims abstract description 75
- 238000002156 mixing Methods 0.000 claims abstract description 61
- 238000005470 impregnation Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000012266 salt solution Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 15
- 238000007598 dipping method Methods 0.000 claims abstract description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012298 atmosphere Substances 0.000 claims abstract description 10
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 7
- 239000002223 garnet Substances 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 128
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 47
- 239000000395 magnesium oxide Substances 0.000 claims description 42
- 238000000498 ball milling Methods 0.000 claims description 38
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 35
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 34
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 32
- 238000001354 calcination Methods 0.000 claims description 30
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 26
- 150000003839 salts Chemical class 0.000 claims description 25
- 239000011812 mixed powder Substances 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 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 10
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 230000005284 excitation Effects 0.000 claims description 8
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 claims description 4
- 238000000926 separation method 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
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 3
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 3
- 239000002736 nonionic surfactant Substances 0.000 claims description 3
- 239000012716 precipitator Substances 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 6
- 229910017083 AlN Inorganic materials 0.000 abstract 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 230000008569 process Effects 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000005303 weighing Methods 0.000 description 13
- 239000002202 Polyethylene glycol Substances 0.000 description 12
- 239000007791 liquid phase Substances 0.000 description 12
- 229920001223 polyethylene glycol Polymers 0.000 description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 238000011049 filling Methods 0.000 description 7
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 239000002270 dispersing agent Substances 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- 239000011858 nanopowder Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 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
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
- 229910002027 silica gel Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000012700 ceramic precursor Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GURPBNBIWUKDMN-UHFFFAOYSA-H S(=O)([O-])[O-].[Y+3].S(=O)([O-])[O-].S(=O)([O-])[O-].[Y+3] Chemical compound S(=O)([O-])[O-].[Y+3].S(=O)([O-])[O-].S(=O)([O-])[O-].[Y+3] GURPBNBIWUKDMN-UHFFFAOYSA-H 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- CNGGOAOYPQGTLH-UHFFFAOYSA-N [O-2].[O-2].[Mg+2].[Al+3] Chemical compound [O-2].[O-2].[Mg+2].[Al+3] CNGGOAOYPQGTLH-UHFFFAOYSA-N 0.000 description 1
- 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 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical group [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- JESHZQPNPCJVNG-UHFFFAOYSA-L magnesium;sulfite Chemical compound [Mg+2].[O-]S([O-])=O JESHZQPNPCJVNG-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000007966 viscous suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910000347 yttrium sulfate Inorganic materials 0.000 description 1
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 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
- C04B35/10—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 aluminium oxide
-
- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
-
- 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
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
-
- 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
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5445—Particle size related information expressed by the size of the particles or aggregates thereof submicron sized, i.e. from 0,1 to 1 micron
-
- 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
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- 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
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6582—Hydrogen containing atmosphere
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)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention protects a kind of preparation method of ceramic composite, comprises the following steps：Batch mixing：Ceramic raw material is mixed with fluorescent material, and it is pre-stamped under default pressure, ceramic composite green compact are obtained, ceramic raw material includes one kind in aluminum oxide or aluminium nitride, and fluorescent material is the fluorescent material of rare earth doped garnet structure；Base substrate impregnates：Ceramic composite green compact are impregnated into 10~120min in the soluble salt solutions of the second sintering aid, then the ceramic composite green compact after dipping are dried, and more than the decomposition temperature of the soluble-salt in the second sintering aid calcined so that the second sintering aid is attached in ceramic composite green compact；Sintering：Ceramic composite green compact after base substrate impregnation steps are sintered under protective atmosphere or under vacuum, obtain ceramic composite.This method improves the addition manner of sintering aid, reduces the cost for obtaining ceramic composite.
Description
Technical Field
The invention relates to the field of fluorescent ceramics, in particular to a preparation method of a ceramic composite material, a related ceramic composite material and a light source device.
Background
The technology of obtaining visible light by exciting a fluorescent material with blue laser is continuously paid attention to along with the development of laser display technology, and the current research trend is mainly to develop a novel fluorescent material (wavelength conversion material) aiming at the characteristics of laser excited fluorescent powder, and the main requirements are that the luminous brightness is high, the fluorescent material can bear high-power laser irradiation, the optical conversion efficiency is high, the heat conduction performance is high, and the like.
With the improvement of technical requirements, the traditional silica gel packaging fluorescent powder technology and glass packaging fluorescent powder technology cannot meet the requirements of high-end products. The bearing temperature of the silica gel is usually not more than 200-250 ℃, the silica gel is easy to age in a high-temperature environment after long-time work, and the service life is short; moreover, the thermal conductivity of the materials of the silica gel package and the glass package is low, and the materials cannot bear the irradiation of high-power or even ultrahigh-power laser.
Because the ceramic has excellent heat-conducting property and high-temperature resistance, the ceramic becomes the key point of the next generation of laser excitation luminescent materials. Generally, the formation conditions of ceramics are harsh, and hot-pressing sintering or other high-pressure sintering methods are required to obtain ceramics with high performance parameters, but these methods have low production efficiency and high cost, and are difficult to produce in batch.
Disclosure of Invention
Aiming at the defects of low production efficiency and high manufacturing cost of the fluorescent ceramic in the prior art, the invention provides a low-cost and high-efficiency preparation method of the fluorescent ceramic, which comprises the following steps:
mixing materials: mixing a ceramic raw material and fluorescent powder, and pre-pressing under a preset pressure to obtain a ceramic composite green body, wherein the ceramic raw material comprises one of aluminum oxide or aluminum nitride, and the fluorescent powder is a rare earth element doped garnet structure fluorescent powder;
and (3) blank impregnation: dipping the ceramic composite material green body in a soluble salt solution of a second sintering aid, drying the dipped ceramic composite material green body, and calcining the ceramic composite material green body above the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached to the ceramic composite material green body;
and (3) sintering: and sintering the ceramic composite material green body subjected to the green body impregnation step in a protective atmosphere or in vacuum to obtain the ceramic composite material.
Preferably, the average particle size of the ceramic raw material is 0.05-1 μm, and the average particle size of the phosphor is 10-30 μm.
Preferably, the preset pressure is 5-200 MPa, and the concentration of the soluble salt solution of the second sintering aid is 1-5 mol/L.
Preferably, the second sintering aid is magnesium oxide, and the soluble salt solution of the second sintering aid is a magnesium nitrate solution; or the second sintering aid is yttrium oxide, and the soluble salt solution of the second sintering aid is yttrium nitrate solution; or the second sintering aid is a mixed aid of magnesium oxide and yttrium oxide, and the soluble salt solution of the second sintering aid is a mixed solution of magnesium nitrate and yttrium nitrate.
Preferably, multiple green body impregnation steps are performed prior to the sintering step.
Preferably, the method comprises a first green body impregnation and a second green body impregnation; the first green body dipping comprises dipping the ceramic composite green body in a soluble salt solution of a second sintering aid, then drying the dipped ceramic composite green body, and calcining above the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached in the ceramic composite green body; the second green body impregnation comprises the steps of impregnating the ceramic composite material green body in a soluble salt solution of a third sintering aid, drying the impregnated ceramic composite material green body, and calcining the ceramic composite material green body above the decomposition temperature of the soluble salt of the third sintering aid to enable the third sintering aid to be attached to the ceramic composite material green body; the sequence of the first green body impregnation and the second green body impregnation can be interchanged; the second sintering aid and the third sintering aid are different sintering aids.
Preferably, the second sintering aid is magnesium oxide, and the third sintering aid is yttrium oxide; or the second sintering aid is yttrium oxide, and the third sintering aid is magnesium oxide; or the second sintering aid is a mixed aid of magnesium oxide and yttrium oxide, and the third sintering aid is yttrium oxide or magnesium oxide; or the second sintering aid and the third sintering aid are respectively mixed aids of magnesium oxide and yttrium oxide with different component proportions.
Preferably, in the mixing step, the step of mixing the ceramic raw material and the phosphor powder includes mixing the ceramic raw material, the phosphor powder and a grinding solvent and ball-milling.
Preferably, in the mixing step, the step of mixing the ceramic raw material with the phosphor includes: mixing the ceramic raw material, the first sintering aid and the fluorescent powder.
Preferably, the first sintering aid comprises at least one of magnesium oxide, aluminum oxide, yttrium oxide, calcium fluoride, and magnesium fluoride.
Preferably, the step of mixing the ceramic raw material, the first sintering aid and the phosphor comprises: mixing and ball-milling a ceramic raw material, a first sintering aid and a grinding solvent, drying and calcining to obtain mixed powder, and mixing the mixed powder with the fluorescent powder; or, the step of mixing the ceramic raw material, the first sintering aid and the phosphor powder comprises: dispersing a ceramic raw material in a non-ionic surfactant aqueous solution, preparing a soluble salt solution of a first sintering aid, mixing the two solutions, adding a precipitator aqueous solution to obtain a suspension, carrying out solid-liquid separation on the suspension, calcining solid components in the suspension at a temperature higher than the decomposition temperature of the soluble salt of the first sintering aid to obtain mixed powder, and mixing the mixed powder with the fluorescent powder.
Preferably, the precipitant is soluble ammonium bicarbonate, hydrogen peroxide or ammonia water solution.
Preferably, the phosphor is a cerium doped yttrium aluminum garnet phosphor.
The invention also provides a ceramic composite material prepared by the preparation method, the ceramic composite material comprises a ceramic body used as a substrate and fluorescent powder used as a luminescence center, the luminescence center is packaged in the substrate, and the ceramic body is alumina ceramic or aluminum nitride ceramic.
The invention also provides a light source device, which comprises an excitation light source and the ceramic composite material, wherein the ceramic composite material is positioned on an emergent light path of the excitation light source.
Compared with the prior art, the invention has the following beneficial effects: the ceramic composite material green body obtained after mixing is soaked in the green body in the soluble salt solution of the sintering aid, so that the soluble salt of the sintering aid remains in the internal gap of the ceramic composite material green body, and the content of the sintering aid in the gap is increased through calcination, so that the liquid phase near the gap in the sintering process is promoted, the particles around the gap can be promoted to transfer substances under the condition of unnecessary hot-pressing sintering, the pores can be eliminated, and the relative density of the green body after sintering is improved. Compared with the hot-pressing sintering method, the method of the invention can be carried out in a common sintering furnace, thereby greatly reducing the production cost.
Drawings
FIG. 1 is a schematic structural view of an ideal green ceramic composite;
FIG. 2 is a schematic structural view of an actual green ceramic composite;
FIG. 3 is a schematic structural view of a green ceramic composite impregnated with a green body;
FIG. 4 is a flow chart of a manufacturing process of the present invention.
Detailed Description
The sintering densification process of the ceramic is mainly promoted by the formation of liquid phase in the ceramic body during the sintering process. In the preparation of the luminescent ceramic, a liquid phase is formed in hot-pressing sintering mainly by adding a sintering aid, so that the sintering temperature is reduced, and the density of the material is improved. However, the hot-pressing sintering requires a special sintering furnace, which is high in cost and not beneficial to mass production.
In the normal pressure or vacuum sintering, the raw material powder is mixed in advance, pressed into a green compact in advance by using a mold, and then placed into a furnace for sintering. In general, ceramic powder and a sintering aid are mixed as uniformly as possible, and then filled into a mold for pre-pressing. However, due to the problems of powder fluidity and filling property, the powder has different piling degrees in the process of filling the powder into a die and pressing and forming under stress, and the shape of each part of an ideal green body is relatively uniform, as shown in fig. 1, which is a structural schematic diagram of the ideal ceramic composite material green body, wherein the ceramic raw material Al is a ceramic raw material2O3The particles are distributed around the phosphor particles, and the sintering aid MgO is uniformly distributed between them. However, in the actual green body, the internal structure thereof will beFig. 2 is a schematic view of the actual green ceramic composite material, because the powder is pressed and moved in the mold, and the particles are affected by the pressure unevenness, the inter-particle friction unevenness and the particle fluidity unevenness, and the voids are formed between the particles as shown in fig. 2. Due to the existence of these voids, the green body cannot fill the voids by sufficient mass transfer during atmospheric or vacuum sintering, and the voids eventually become closed pores or interconnected pores, affecting the properties of the material.
According to the preparation method provided by the invention, the pre-pressed ceramic composite material green body is immersed into the soluble salt solution of the sintering aid, so that large gaps in the green body are filled with the soluble salt solution of the sintering aid, and then the green body is taken out and dried, so that the content of the sintering aid around the gaps is increased. The internal structure of the green body after the processes of dipping, drying, calcining and precipitating the sintering aid is changed from the structure shown in figure 2 to the structure shown in figure 3, and figure 3 is a structural schematic diagram of the green body of the ceramic composite material dipped by the green body, so that the sintering aid amount in the gaps is increased, the liquid phase near the gaps is more remarkable in the sintering process, the substance transfer of particles around the gaps can be promoted, the pores can be eliminated, and the relative density of the sintered ceramic composite material is improved.
The ceramic composite material provided by the invention is a composite material with a light-emitting function, and comprises a ceramic body serving as a substrate and fluorescent powder serving as a light-emitting center, wherein the light-emitting center is encapsulated in the substrate. The fluorescent powder is yttrium aluminum garnet fluorescent powder doped with rare earth elements, and comprises various fluorescent powders sold in the market; the ceramic body matrix is prepared from ceramic raw materials, wherein the ceramic raw materials comprise one of alumina or aluminum nitride, and the ceramic body matrix is characterized by lower refractive index, good heat conduction effect and good light transmittance.
The preparation method of the invention comprises the steps of mixing the fluorescent powder into the ceramic raw material by mixing materials, then forming continuous ceramic after sintering the ceramic raw material, and encapsulating the fluorescent powder in the ceramic. In the preparation process, the fluorescent powder does not participate in the reaction to change, so that the original luminescence property can be maintained. Because the melting points of the fluorescent powder and the ceramic raw material are close, in the preparation process, when the ceramic raw material enters a liquid phase, the original structure of the fluorescent powder is easy to damage, and the luminous efficiency of the obtained ceramic composite material is low. By selecting the combination of the ceramic raw material powder with smaller particle size and the fluorescent powder with large particle size, the temperature of the ceramic raw material entering a liquid phase can be reduced to a certain extent, and the stability of the fluorescent powder in the preparation process is ensured. In order to further reduce the temperature of the ceramic raw material powder entering the liquid phase, the preparation method of the invention additionally adds the sintering aid, the sintering aid firstly enters the liquid phase in the heat treatment process, and promotes the ceramic raw material to enter the liquid phase at a lower temperature, thereby playing a role of promoting sintering, not only improving the heat conduction and light transmission performance of the sintered body, but also ensuring that the fluorescent powder is not influenced by overhigh temperature in the heat treatment process as much as possible, so as to keep the physical structure and the surface appearance stable, and further ensure that the prepared fluorescent ceramic has good luminous efficiency. The high fluidity of the sintering aid at high temperature is also beneficial to purifying impurities in grain boundaries, reducing the scattering of light when the light passes through the grain boundaries and improving the light transmittance of ceramics.
The concept of the present invention is based on the problem of how to incorporate a sintering aid into a green ceramic composite material in which ceramic raw materials are mixed with phosphor powder, proposing a method step for green body impregnation.
As shown in the flow chart of the manufacturing method of the present invention of fig. 4, in the present invention, the manufacturing method of the ceramic composite material includes the steps of:
mixing materials: mixing a ceramic raw material and fluorescent powder, and pre-pressing under a preset pressure to obtain a ceramic composite green body, wherein the ceramic raw material comprises one of aluminum oxide or aluminum nitride, and the fluorescent powder is rare earth element doped fluorescent powder with a garnet structure;
and (3) blank impregnation: dipping the ceramic composite material green body in a soluble salt solution of a second sintering aid for 10-120 min, then drying the dipped ceramic composite material green body, and calcining at a temperature higher than the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached to the ceramic composite material green body;
and (3) sintering: and sintering the ceramic composite material green body subjected to the green body impregnation step in a protective atmosphere or in vacuum to obtain the ceramic composite material.
The rare earth element doped garnet structure phosphor is a rare earth element substituted garnet structure crystal (A)3B2(XO4)3Where A, B, X denotes a cation). Such as Ce: Y3Al5O12、Ce:Lu3Al5O12、Ce:Gd3Al5O12、Ce:Tb3Al5O12、Ce:Y3Ga5O12、Ce:Lu3Ga5O12、Ce:Gd3Ga5O12、Ce:Tb3Ga5O12Or Eu: Y3Al5O12And the like. Preferably, the phosphor is a cerium doped yttrium aluminum garnet phosphor.
The average particle size of the ceramic raw material is 0.05-1 mu m, the average particle size of the fluorescent powder is 10-30 mu m, the particle sizes are set so that the ceramic raw material enters a liquid phase and is sintered to obtain ceramic in the sintering process, the fluorescent powder does not participate in reaction, and the original appearance and the luminescence performance are kept.
The preset pressure is 5-200 MPa, and the powder can be made into a flaky ceramic composite material green body through pre-pressing and is not easy to damage in the subsequent steps. The concentration of the soluble salt solution of the second sintering aid is 1-5 mol/L, and under the high concentration, the soluble salt of the second sintering aid which is impregnated into the ceramic composite green body can be as much as possible, so that the times of the green body impregnation step are reduced.
The method for preparing the ceramic composite material of the present invention is described in detail below.
< mixing >
In the embodiment of the present invention, the mixing step can be roughly divided into two schemes, one scheme is to mix only the ceramic raw material and the phosphor, and the other scheme is to mix the ceramic raw material, the phosphor and the first sintering aid.
In the first technical scheme, the step of mixing the ceramic raw material and the fluorescent powder comprises the step of mixing the ceramic raw material, the fluorescent powder and a grinding solvent and carrying out ball milling.
Firstly weighing a certain amount of ceramic raw material powder, filling the ceramic raw material powder into a ball milling tank, adding a proper amount of grinding solvent (such as ethanol), thickening agent and dispersing agent, then carrying out ball milling to obtain thick suspension-shaped slurry, adding fluorescent powder, and continuing ball milling to obtain the ceramic raw material-fluorescent powder slurry. In the embodiment, a two-step ball milling method is adopted, so that ceramic raw material powder which is small in particle size and not easy to disperse uniformly can be fully dispersed firstly, and then the fluorescent powder is added for ball milling, so that the problem that the fluorescent powder is subjected to ball milling for too long time is avoided, and the damage of the ball milling process to the fluorescent powder is reduced. Of course, the two may be directly mixed and ball-milled to reduce the number of steps.
And secondly, drying the obtained ceramic raw material-fluorescent powder slurry to obtain dry powder, and then calcining the dry powder to decompose and volatilize organic components in the dry powder. Because the ceramic raw material and the fluorescent powder have high melting point and good thermal stability, the structure of the ceramic raw material and the fluorescent powder cannot be influenced by the temperature for removing organic matters; at this temperature, the ceramic raw material and the phosphor are not oxidized, and thus the calcination can be performed in an oxygen atmosphere (e.g., air). The high-purity ceramic raw material, namely fluorescent powder, is obtained after calcination, and is granulated to increase the fluidity of the powder in the heat treatment process, so that the compression molding before heat treatment is facilitated, and the prepared fluorescent ceramic is compact and uniform.
Then, a proper amount of the ceramic raw material-fluorescent powder is weighed, loaded into a mold (such as a graphite mold and a steel mold), and pre-pressed and molded under 5-200 MPa to obtain a ceramic composite green body.
In the material mixing step of the second technical scheme, the step of mixing the ceramic raw material with the phosphor powder includes mixing the ceramic raw material with the first sintering aid to obtain mixed powder, and then mixing the mixed powder with the phosphor powder, that is, mixing the ceramic raw material, the first sintering aid and the phosphor powder.
As outlined in the green body impregnation, the purpose of the green body impregnation is to fill a sintering aid in the voids of the green ceramic composite material obtained after pressing, so as to promote mass transfer of particles around the voids during sintering, eliminate pores, and increase the relative density of the sintered ceramic composite material. But for the densely compacted part of the green body, the sintering aid at the location of the voids has a limited effect.
Therefore, in the second technical scheme of mixing, before the blank body is impregnated in advance, the first sintering aid is doped into the ceramic composite material in the step of mixing, and compared with the method of only adding the sintering aid in the step of impregnating the blank body, the first sintering aid can be dispersed in the green body of the ceramic composite material in advance by the technical scheme, and the impregnation frequency of the subsequent blank body can be reduced.
In a second technical scheme of mixing materials, the step of mixing the ceramic raw material and the first sintering aid to obtain mixed powder comprises the steps of mixing the ceramic raw material, the first sintering aid and a grinding solvent, carrying out ball milling, drying and calcining to obtain the mixed powder. Specifically, a certain amount of ceramic raw materials and a first sintering aid are weighed and filled into a ball milling tank, a grinding solvent (such as ethanol), a thickening agent and a dispersing agent are added, first ball milling is carried out to obtain viscous suspension-shaped slurry, then drying and calcining are carried out, and the grinding solvent, the thickening agent and the dispersing agent are removed, so that pure ceramic raw material-first sintering aid mixed powder is obtained. Of course, the mixing is not limited to ball milling. The first sintering aid optionally includes at least one of magnesium oxide, aluminum oxide, yttrium oxide, calcium fluoride, and magnesium fluoride.
In the second embodiment of the mixed material, for example, a ceramic raw material is dispersed in an aqueous solution of a nonionic surfactant, a soluble salt solution of a first sintering aid is prepared, the two solutions are mixed, an aqueous solution of a precipitant is added to obtain a suspension, the suspension is subjected to solid-liquid separation, and the solid content is calcined at a temperature equal to or higher than the decomposition temperature of the soluble salt of the first sintering aid to obtain a mixed powder.
Specifically, 1-3% of PEG (polyethylene glycol) aqueous solution by mass is prepared, ceramic raw material powder is mixed with the PEG aqueous solution, and ultrasonic treatment is carried out for 1-3 hours, so that the powder is dispersed in the solution. Then preparing a soluble salt solution (such as a magnesium nitrate solution) of a first sintering aid (such as MgO), wherein the concentration of the soluble salt solution is 0.01-1 mol/L, mixing the PEG aqueous solution of the ceramic raw material powder and the soluble salt solution of the first sintering aid, and placing the mixture on a magnetic stirrer to be continuously stirred to obtain a mixed solution. Ammonium bicarbonate is used as a precipitant to prepare 0.01-0.1 mol/L aqueous solution, and the continuously stirred mixed solution is slowly dropped until the pH value of the mixed solution is controlled to be about 8-10, preferably 9-9.5. Keeping pH value, and stirring for 1-5 hr, preferably 2-3 hr to obtain coprecipitated composite powder suspension. And (3) performing centrifugal solid-liquid separation on the suspension, washing and drying the obtained solid component for multiple times, and calcining the obtained powder at a temperature higher than the decomposition temperature of soluble salt (namely magnesium nitrate) of the first sintering aid to obtain mixed powder of the ceramic raw material and the first sintering aid.
The first sintering aid can be magnesium oxide, yttrium oxide and aluminum oxide, soluble salts corresponding to the magnesium oxide include any soluble salts which can be decomposed at high temperature to obtain magnesium oxide, such as magnesium nitrate, magnesium sulfate and magnesium sulfite, soluble salts corresponding to the yttrium oxide include any soluble salts which can be decomposed at high temperature to obtain yttrium oxide, such as yttrium nitrate, yttrium sulfate and yttrium sulfite, and soluble salts corresponding to the aluminum oxide include any soluble salts which can be decomposed at high temperature to obtain aluminum oxide, such as aluminum nitrate and aluminum sulfate.
Besides ammonium bicarbonate, the precipitant can also be other reagents for adjusting the pH value, such as bicarbonate, hydrogen peroxide, ammonia water and the like.
In the second technical scheme of mixing materials, after mixed powder of ceramic raw materials and the first sintering aid is obtained, the mixed powder and fluorescent powder are mixed in a ball milling tank, a proper amount of ethanol is added to serve as a grinding solvent, and zirconia balls with ultra-low grinding loss rate are used for ball milling for 1-120 min. And after the ball milling is finished, removing impurities such as a grinding solvent and the like, sieving and granulating to obtain mixed powder of the ceramic raw material, the first sintering aid and the fluorescent powder, and pre-pressing at 5-200 MPa to obtain a ceramic composite green body.
< impregnation of green body >
The step of dipping the green body comprises the steps of firstly preparing a soluble salt solution (such as a magnesium nitrate solution) of a second sintering aid (such as magnesium oxide), then dipping the ceramic composite material green body into the solution, enabling the liquid level of the solution to be over the top of the green body, and dipping the green body in the solution for 10-120 min, so that the solution can fully enter the inner space of the green body. And then taking out the dipped ceramic composite material green body, drying, and calcining at a temperature (200-500 ℃) higher than the decomposition temperature of a soluble salt (magnesium nitrate) of the second sintering aid, so that the soluble salt (magnesium nitrate) of the second sintering aid in the internal gap of the green body is converted into an insoluble second sintering aid (magnesium oxide) and attached to the ceramic composite material green body.
The concentration of the soluble salt solution of the second sintering aid is preferably 1-5 mol/L, and under the high concentration, the soluble salt of the second sintering aid which is impregnated into the ceramic composite green body can be as much as possible, so that the impregnation efficiency of the green body is improved.
The second sintering aid can be a single sintering aid of magnesium oxide and yttrium oxide, or a mixed aid of magnesium oxide and yttrium oxide, and corresponding nitrate, sulfate and sulfite are soluble salts used for impregnation. The second sintering aid may be the same as or different from the first sintering aid in the mixing step.
In the present invention, it is desirable that the effect of filling the voids with the second sintering aid is achieved by one-time green body impregnation, but in practice, the sintering aid cannot be completely enriched in the voids, and thus, a plurality of green body impregnation steps are required to achieve the intended effect. The multiple times of blank impregnation can be carried out in soluble salt solution of the same sintering aid or soluble salt solution of different sintering aids.
In certain embodiments of the present invention, a first green body impregnation and a second green body impregnation are included. The first green body dipping comprises dipping the ceramic composite green body in a soluble salt solution of a second sintering aid, then drying the dipped ceramic composite green body, and calcining above the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached in the ceramic composite green body; the second green body impregnation comprises the steps of impregnating the ceramic composite green body in a soluble salt solution of a third sintering aid, drying the impregnated ceramic composite green body, and calcining the ceramic composite green body above the decomposition temperature of the soluble salt of the third sintering aid to enable the third sintering aid to be attached to the ceramic composite green body. The first green body impregnation and the second green body impregnation are only arranged for distinguishing two different sintering aids, namely a second sintering aid and a third sintering aid, which are respectively adopted, so that the sequence of the first green body impregnation and the second green body impregnation can be randomly interchanged.
In the embodiment of the present invention, preferably, the second sintering aid is yttrium oxide, and the third sintering aid is magnesium oxide; in a more complicated scheme, the second auxiliary agent can be a mixed auxiliary agent of yttrium oxide and magnesium oxide, and the third sintering auxiliary agent is one of yttrium oxide or magnesium oxide; the second sintering aid can also be yttrium oxide or magnesium oxide, and the third sintering aid is a mixed aid of magnesium oxide and yttrium oxide; the second sintering aid and the third sintering aid can also be mixed aids of magnesium oxide and yttrium oxide with different component proportions.
< sintering >
In the sintering step, the ceramic composite material green body after the green body impregnation is placed into a sintering furnace, sintering is carried out in vacuum or protective atmosphere (such as nitrogen and nitrogen-hydrogen mixed gas), the sintering temperature is 1450-1700 ℃, the heat preservation time is 1-10 hours, and cooling is carried out after sintering is finished, so that the ceramic composite material is obtained. In the invention, as the blank body impregnation method is adopted, the sintering aid is filled in the gaps in the blank body, the sintering aid firstly enters the liquid phase in the sintering process, and the ceramic raw material is promoted to enter the liquid phase at a lower temperature, so that the sintering promoting effect is achieved, the heat conduction and light transmission performance of the sintered body are improved, the influence of overhigh temperature on the fluorescent powder in the sintering process is ensured as much as possible, the physical structure and the surface appearance are kept stable, and the prepared ceramic composite material has good luminous efficiency.
The embodiments of the present invention will be described in detail below with reference to the drawings and the embodiments.
Example one
Mixing materials:
the method comprises the steps of selecting high-purity superfine alumina nano powder with the particle size of 0.05-1 mu m, preferably 0.06-0.2 mu m as a raw material, preparing 1-3% PEG (polyethylene glycol) aqueous solution by mass fraction, mixing a proper amount of the alumina nano powder with the PEG aqueous solution, and carrying out ultrasonic treatment on the PEG aqueous solution of the alumina for 1-3 hours for later use.
Weighing a certain amount of Mg (NO) according to the weight ratio of magnesium oxide to aluminum oxide of (0.01-2) to 1003)2·6H2O, reacting these Mg (NO)3)2·6H2And (3) dividing the O into two parts, and respectively preparing a nitrate solution and a nitrate solution with different concentrations, wherein the concentration of the solution a is 0.01-1 mol/L, and the concentration of the solution b is 1-5 mol/L.
Mixing the PEG aqueous solution of the alumina with the solution a to obtain a mixed solution, and continuously stirring the mixed solution on a magnetic stirrer at the temperature of 20-80 ℃, preferably 40-60 ℃ and the rotating speed of 100-300 r/min.
Ammonium bicarbonate is used as a precipitant to prepare an aqueous solution of about 0.01-0.1 mol/L, and the continuously stirred mixed suspension is slowly dropped until the pH value of the mixed suspension is controlled to be about 8-10, preferably 9-9.5. The proper pH value is very important for the dispersion and deflocculation of the alumina superfine powder particles, and the coprecipitation composite powder suspension is obtained after the proper pH value is kept and the stirring is continued for 1 to 5 hours, preferably 2 to 3 hours.
And (3) centrifugally separating the suspension, washing the obtained powder for 2-8 times, and then drying in vacuum at 50-150 ℃ for 1-10 hours.
Calcining the obtained dry powder at 200-500 ℃ to remove impurities, preserving heat for 1-5h, and then performing air cooling along with the furnace to obtain the alumina-magnesia mixed powder.
Weighing a certain amount of aluminum oxide-magnesium oxide mixed powder and a certain amount of fluorescent powder Ce: YAG, putting the two powders into a polytetrafluoroethylene ball milling tank, adding a proper amount of ethanol as a grinding solvent, and carrying out ball milling by using zirconia balls with ultra-low attrition rate for 1-120min, preferably 30-50 min. The short ball milling time is because the YAG fluorescent powder has larger particles and is easy to disperse, and if the ball milling time is too long, the surface morphology of the crystal grains of the YAG fluorescent powder is easy to damage, and the luminescence performance is influenced.
After ball milling, drying under vacuum at constant temperature to obtain dry powder, and then sieving with 80-mesh, 150-mesh and 200-mesh sieves for granulation to obtain high-fluidity raw material powder. Weighing a proper amount of raw material powder, putting the raw material powder into a steel die, performing pre-pressing under the pressure of 5-200 MPa, and demolding to obtain a green body.
And (3) blank impregnation:
the green body was dipped into solution b at a level that was just above the top of the green body sample. The soaking time is 10 min-120 min, then the soaked green body is taken out, dried at 80 ℃, and calcined at 200-500 ℃ to convert the soluble magnesium nitrate mainly attached to the internal gaps of the green body into water-insoluble magnesium oxide. The infiltration process is repeated a number of times, but each time calcination is necessary to convert the magnesium nitrate.
And (3) sintering:
placing the green body sample subjected to the infiltration process into a sintering furnace, and performing vacuum treatment orSintering in nitrogen/nitrogen-hydrogen atmosphere at 1450-1700 ℃ for 1-10h to obtain the luminescent ceramic composite YAG-Al2O3-MgO。
Example two
Mixing materials:
the method comprises the steps of selecting high-purity superfine alumina nano powder with the particle size of 0.06-0.2 mu m as a raw material, preparing 1-3% PEG (polyethylene glycol) aqueous solution, mixing a proper amount of alumina nano powder with the PEG aqueous solution, and carrying out ultrasonic treatment on the solution for 1-3 hours for later use.
By reacting MgO with Al2O3The weight ratio of (0.01-2) to 100, weighing a certain amount of Mg (NO)3)2·6H2And O, preparing a magnesium nitrate salt solution with the concentration of 0.01-1 mol/L, and marking as a solution a.
Mixing Al2O3Mixing the solution and the solution a to obtain a mixed suspension, and continuously stirring the mixed suspension on a magnetic stirrer at the temperature of 40-60 ℃ and the rotating speed of 170-250 r/min.
Ammonium bicarbonate is used as a precipitator to prepare an aqueous solution of about 0.01-0.1 mol/L, the continuously stirred mixed suspension is slowly dripped until the pH value of the mixed suspension is controlled to be about 9-9.5, and the mixed suspension is continuously stirred for 2-3 hours after the pH value is maintained, so that the coprecipitated composite powder suspension is obtained.
And (3) centrifugally separating the suspension, washing the obtained solid for 2-8 times, and then drying in vacuum at 50-150 ℃ for 1-10 hours to obtain dry powder.
Calcining the obtained dry powder at 200-500 ℃ to remove impurities, preserving heat for 1-5h, and then performing furnace air cooling to obtain Al2O3-MgO mixed powder.
Weighing a certain amount of Al2O3MgO mixed powder and a certain amount of fluorescent powder, and the two powders are filled into poly-tetra-polyAdding a proper amount of ethanol as a grinding solvent into a vinyl fluoride ball milling tank, and carrying out ball milling by using zirconia balls with ultralow loss rate for 30-50 min.
After ball milling, drying under vacuum at constant temperature to obtain dry powder, and then sieving with 80-mesh, 150-mesh and 200-mesh sieves for granulation to obtain high-fluidity raw material powder. Weighing a proper amount of raw material powder, putting the raw material powder into a steel die, performing pre-pressing under the pressure of 5-200 MPa, and demolding to obtain a green body.
And (3) blank impregnation:
weighing a certain amount of Y (NO)3)3·6H2And O, preparing yttrium nitrate salt solution with the concentration of 1-5 mol/L, and marking as solution b.
The green body is dipped into a solution b, yttrium nitrate solution, at a level that is just above the top of the green body sample. The soaking time is 60-90 min, then the soaked green body is taken out, dried at 80 ℃, and calcined at 200-500 ℃ to convert soluble yttrium nitrate mainly attached to the internal gaps of the green body into water-insoluble yttrium oxide. The infiltration process can be repeated as many times as desired, but each time calcination is necessary to convert the magnesium nitrate.
And (3) sintering:
and (3) putting the green body sample subjected to the dipping process into a sintering furnace, sintering in vacuum or nitrogen-hydrogen mixed gas atmosphere at the sintering temperature of 1450-1700 ℃, keeping the temperature for 1-10h, and obtaining the luminescent ceramic composite material after sintering.
EXAMPLE III
Mixing materials:
weighing aluminum nitride with the particle size of 0.5-1 mu m, filling the aluminum nitride into a ball milling tank, adding a proper amount of ethanol grinding solvent, adding a grinding body, and carrying out ball milling. And when the slurry in the ball milling tank is in a viscous suspension state, adding Ce: YAG fluorescent powder particles with the particle size of 15-25 mu m, continuing ball milling until the fluorescent powder is uniformly distributed, and finishing ball milling.
And then taking out the slurry, drying at constant temperature in vacuum to obtain dry powder, calcining the dry powder in a muffle furnace, and removing organic components in the dry powder to obtain high-purity aluminum nitride-fluorescent powder. Then sieving and granulating the powder to obtain the high-fluidity aluminum nitride-fluorescent powder. Weighing a proper amount of aluminum nitride-fluorescent powder, filling the aluminum nitride-fluorescent powder into a die, and performing compression molding under the pressure of 50MPa to obtain a ceramic composite green body.
And (3) blank impregnation:
weighing a certain amount of Mg (NO)3)2·6H2O and Y (NO)3)3·6H2And O, respectively preparing a magnesium nitrate salt solution with the concentration of 1-5 mol/L, namely a solution a and an yttrium nitrate salt solution with the concentration of 1-5 mol/L, namely a solution b.
And (3) soaking the green body into the solution a for 60-90 min, taking out the soaked green body, drying at 80 ℃, and calcining at 200-500 ℃ to convert soluble magnesium nitrate mainly attached to the inner gaps of the green body into water-insoluble magnesium oxide.
And then soaking the green body into the solution b for 60-90 min, taking out the soaked green body, drying at 80 ℃, and calcining at 200-500 ℃ to convert soluble yttrium nitrate mainly attached to the internal gaps of the green body into water-insoluble yttrium oxide.
And (3) sintering:
and (3) putting the green body sample subjected to the dipping process into a sintering furnace, sintering in a vacuum atmosphere at the sintering temperature of 1450-1700 ℃, and keeping the temperature for 1-10 hours to obtain the luminescent ceramic composite material after sintering.
Example four
Mixing materials:
the raw materials are high-purity superfine alumina nano powder with the grain diameter of 0.08-0.2 mu m, high-purity superfine nano yttrium oxide powder with the grain diameter of 0.05-0.1 mu m, high-purity superfine nano magnesium oxide powder with the grain diameter of 0.05-0.1 mu m and Ce: YAG fluorescent powder with the grain diameter of 15-20 mu m.
A certain amount of alumina powder (30 wt%), yttria powder (0.5 wt%), magnesia powder (0.5 wt%) and Ce: YAG phosphor powder (69 wt%) were weighed. Putting alumina powder, yttrium oxide powder and magnesium oxide powder into a polytetrafluoroethylene ball milling tank, adding a proper amount of ethanol as a grinding solvent, adding a proper amount of ceramic dispersant as a dispersant, and carrying out primary ball milling by using zirconia balls with ultralow attrition loss rate for 24 hours.
And after the first ball milling is finished, adding the Ce: YAG fluorescent powder into a ball milling tank, and carrying out second ball milling for 40 min.
And after the ball milling is finished for two times, drying at constant temperature in vacuum to obtain dry powder.
The dry powder was calcined in a muffle furnace at 600 ℃ to remove the organic components from the powder for 2 hours. And sieving and granulating the calcined powder to obtain the high-fluidity fluorescent ceramic precursor powder. Weighing a proper amount of fluorescent ceramic precursor powder, filling the fluorescent ceramic precursor powder into a mold, and pre-pressing under the pressure of 15MPa to obtain a ceramic composite green body.
And (3) blank impregnation:
weighing a certain amount of Mg (NO)3)2·6H2O and Y (NO)3)3·6H2O, preparing a magnesium nitrate and yttrium nitrate mixed solution with nitrate concentration of 1-5 mol/L.
And (3) soaking the green body into the mixed solution for 60-90 min, taking out the soaked green body, drying at 80 ℃, and calcining at 200-500 ℃ to convert magnesium nitrate and yttrium nitrate which are mainly attached to the inner gaps of the green body into magnesium oxide and yttrium oxide which are not soluble in water.
The green body impregnation step was repeated three times.
And (3) sintering:
and (3) putting the green body sample subjected to the dipping process into a sintering furnace, sintering in a nitrogen-hydrogen mixed gas atmosphere at the sintering temperature of 1450-1700 ℃, keeping the temperature for 1-10h, and obtaining the luminescent ceramic composite material after sintering.
The invention also claims a ceramic composite material prepared by the preparation method, the ceramic composite material comprises a ceramic body used as a matrix and fluorescent powder used as a luminescence center, the luminescence center is encapsulated in the matrix, and the ceramic body is alumina ceramic or aluminum nitride ceramic. Further, the fluorescent powder is cerium-doped yttrium aluminum garnet fluorescent powder.
The invention also relates to a light-emitting device which is a wavelength conversion color wheel, wherein the ceramic composite material is arranged on the wavelength conversion color wheel.
The invention also relates to a light source device, which comprises an excitation light source and the ceramic composite material, wherein the ceramic composite material is arranged on an emergent light path of the excitation light source and is used for absorbing the excitation light and emitting excited light. The light source device can be applied to lighting sources such as automobile headlights, stage lamps and the like, and can also be used as a light source of a projector for image display.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (15)
1. The preparation method of the ceramic composite material is characterized by comprising the following steps:
mixing materials: mixing a ceramic raw material and fluorescent powder, and pre-pressing under a preset pressure to obtain a ceramic composite green body, wherein the ceramic raw material comprises one of aluminum oxide or aluminum nitride, and the fluorescent powder is rare earth element doped fluorescent powder with a garnet structure;
and (3) blank impregnation: dipping the ceramic composite material green body in a soluble salt solution of a second sintering aid for 10-120 min, then drying the dipped ceramic composite material green body, and calcining at a temperature higher than the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached to the ceramic composite material green body;
and (3) sintering: and sintering the ceramic composite material green body subjected to the green body impregnation step in a protective atmosphere or in vacuum.
2. The method according to claim 1, wherein the ceramic raw material has an average particle size of 0.05 to 1 μm, and the phosphor has an average particle size of 10 to 30 μm.
3. The preparation method according to claim 1, wherein the preset pressure is 5 to 200MPa, and the concentration of the soluble salt solution of the second sintering aid is 1 to 5 mol/L.
4. The preparation method according to claim 1, wherein the second sintering aid is magnesium oxide, and the soluble salt solution of the second sintering aid is a magnesium nitrate solution; or
The second sintering aid is yttrium oxide, and the soluble salt solution of the second sintering aid is yttrium nitrate solution; or
The second sintering aid is a mixed aid of magnesium oxide and yttrium oxide, and the soluble salt solution of the second sintering aid is a mixed solution of magnesium nitrate and yttrium nitrate.
5. The production method according to claim 1, wherein the green body impregnation step is performed a plurality of times before the sintering step.
6. The preparation method according to claim 5, characterized by comprising a first green body impregnation and a second green body impregnation;
the first green body impregnation comprises the steps of impregnating the ceramic composite material green body in a soluble salt solution of a second sintering aid, drying the impregnated ceramic composite material green body, and calcining the ceramic composite material green body above the decomposition temperature of the soluble salt of the second sintering aid to enable the second sintering aid to be attached to the ceramic composite material green body;
the second green body impregnation comprises the steps of impregnating the ceramic composite green body in a soluble salt solution of a third sintering aid, drying the impregnated ceramic composite green body, and calcining the ceramic composite green body above the decomposition temperature of the soluble salt of the third sintering aid to enable the third sintering aid to be attached to the ceramic composite green body;
the second sintering aid and the third sintering aid are different sintering aids.
7. The production method according to claim 6, wherein the second sintering aid is magnesium oxide, and the third sintering aid is yttrium oxide; or
The second sintering aid is yttrium oxide, and the third sintering aid is magnesium oxide; or
The second sintering aid is a mixed aid of magnesium oxide and yttrium oxide, and the third sintering aid is yttrium oxide or magnesium oxide; or
The second sintering aid and the third sintering aid are respectively mixed aids of magnesium oxide and yttrium oxide with different component proportions.
8. The method according to any one of claims 1 to 7, wherein in the mixing step, the step of mixing the ceramic raw material with the phosphor comprises mixing the ceramic raw material, the phosphor and a grinding solvent and ball-milling.
9. The production method according to any one of claims 1 to 7, wherein in the mixing step, the step of mixing the ceramic raw material with the phosphor includes: and mixing the ceramic raw material, the first sintering aid and the fluorescent powder.
10. The method of claim 9, wherein the first sintering aid comprises at least one of magnesium oxide, aluminum oxide, yttrium oxide, calcium fluoride, and magnesium fluoride.
11. The method of claim 9, wherein the step of mixing the ceramic raw material, the first sintering aid, and the phosphor comprises: mixing the ceramic raw material, the first sintering aid and a grinding solvent, performing ball milling, drying and calcining to obtain mixed powder, and mixing the mixed powder with the fluorescent powder; or,
the step of mixing the ceramic raw material, the first sintering aid and the phosphor powder comprises: dispersing the ceramic raw material in a non-ionic surfactant aqueous solution, preparing a soluble salt solution of the first sintering aid, mixing the two solutions, adding a precipitator aqueous solution to obtain a suspension, carrying out solid-liquid separation on the suspension, calcining solid components in the suspension at a temperature higher than the decomposition temperature of the soluble salt of the first sintering aid to obtain mixed powder, and mixing the mixed powder with the fluorescent powder.
12. The preparation method according to claim 11, wherein the precipitant is soluble ammonium bicarbonate, hydrogen peroxide or an aqueous ammonia solution.
13. The method of claim 1, wherein the phosphor is cerium-doped yttrium aluminum garnet phosphor.
14. A ceramic composite material prepared by the preparation method of any one of claims 1 to 13, the ceramic composite material comprising a ceramic body as a matrix and a phosphor as a luminescence center, the luminescence center being encapsulated within the matrix, the ceramic body being an alumina ceramic or an aluminum nitride ceramic.
15. A light source apparatus comprising an excitation light source and the ceramic composite material according to claim 14, the ceramic composite material being located on an exit light path of the excitation light source.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610812030.1A CN107805056A (en) | 2016-09-09 | 2016-09-09 | The preparation method and ceramic composite of ceramic composite, light supply apparatus |
| PCT/CN2017/086863 WO2018045782A1 (en) | 2016-09-09 | 2017-06-01 | Preparation method for ceramic composite material, ceramic composite material, and light source apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610812030.1A CN107805056A (en) | 2016-09-09 | 2016-09-09 | The preparation method and ceramic composite of ceramic composite, light supply apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107805056A true CN107805056A (en) | 2018-03-16 |
Family
ID=61561233
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610812030.1A Pending CN107805056A (en) | 2016-09-09 | 2016-09-09 | The preparation method and ceramic composite of ceramic composite, light supply apparatus |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN107805056A (en) |
| WO (1) | WO2018045782A1 (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095923A (en) * | 2017-06-20 | 2018-12-28 | 深圳市光峰光电技术有限公司 | A kind of preparation method and luminescent ceramic composite of luminescent ceramic composite |
| WO2019179119A1 (en) * | 2018-03-21 | 2019-09-26 | 深圳光峰科技股份有限公司 | Light-emitting ceramic and preparation method therefor |
| CN110342908A (en) * | 2018-04-05 | 2019-10-18 | 日亚化学工业株式会社 | The manufacturing method of ceramic composite, projector light source and ceramic composite |
| WO2019200934A1 (en) * | 2018-04-19 | 2019-10-24 | 深圳光峰科技股份有限公司 | Multiphase fluorescent ceramic and preparation method therefor |
| CN110386820A (en) * | 2018-04-19 | 2019-10-29 | 深圳光峰科技股份有限公司 | A kind of fluorescence ceramics and preparation method thereof of aluminum oxynitride matrix |
| CN110386818A (en) * | 2018-04-23 | 2019-10-29 | 中国科学院上海光学精密机械研究所 | Mix zirconium terbium aluminium garnet magnetic rotation crystalline ceramics and preparation method thereof |
| CN111039660A (en) * | 2018-10-11 | 2020-04-21 | 深圳光峰科技股份有限公司 | Fluorescent ceramic, preparation method thereof, light source device and projection device |
| CN111732434A (en) * | 2020-07-07 | 2020-10-02 | 韶关学院 | Ceramic preparation method using in-situ generated oxide as sintering aid |
| CN114394822A (en) * | 2022-01-30 | 2022-04-26 | 中国科学院宁波材料技术与工程研究所 | Face-centered structure composite ceramic, preparation method thereof and laser white light source device |
| CN114538931A (en) * | 2022-03-11 | 2022-05-27 | 北京理工大学 | High-performance AlON transparent ceramic and low-temperature rapid preparation method thereof |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110759721A (en) * | 2019-10-31 | 2020-02-07 | 醴陵振美艺术陶瓷有限公司 | Banquet porcelain and preparation method thereof |
| CN112094110A (en) * | 2020-10-15 | 2020-12-18 | 贵州赛义光电科技有限公司 | Al (aluminum)2O3-YAG:Ce3+Preparation method of complex phase fluorescent ceramic |
| CN114832828B (en) * | 2022-06-06 | 2023-10-24 | 青岛科技大学 | Metal salt ceramic composite material and preparation method and application thereof |
| CN115180948B (en) * | 2022-07-12 | 2023-08-18 | 江苏师范大学 | High-light-efficiency complex-phase fluorescent ceramic for laser illumination and preparation method thereof |
| CN117623797A (en) * | 2022-08-19 | 2024-03-01 | 比亚迪股份有限公司 | Conductive ceramic and preparation method and application thereof |
| CN115432957B (en) * | 2022-08-30 | 2023-09-08 | 重庆大学 | Method for preparing ZnO-PTFE super-hydrophobic composite ceramic by cold sintering |
| CN116161972A (en) * | 2023-03-14 | 2023-05-26 | 广州瑞鑫通科技有限公司 | Preparation method of alumina ceramic sintering aid |
| CN116535196A (en) * | 2023-05-23 | 2023-08-04 | 长沙华脉新材料有限公司 | Preparation method and application of alumina ceramic |
| CN117185789B (en) * | 2023-08-30 | 2024-07-16 | 湖南宥臻新材料科技有限公司 | High-light-efficiency alumina-based ceramic material and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134692A (en) * | 1993-11-12 | 1996-10-30 | 美国3M公司 | Abrasive grain and method for making the same |
| US5587346A (en) * | 1995-06-16 | 1996-12-24 | Osram Sylvania, Inc. | Translucent polycrystalline alumina |
| CN1263877A (en) * | 1999-01-29 | 2000-08-23 | 住友化学工业株式会社 | Semi-transparent alumina sintered substance and its production |
| JP2005340240A (en) * | 2004-05-24 | 2005-12-08 | Cimeo Precision Co Ltd | Transmitting light color converting member and manufacturing method thereof |
| CN101697367A (en) * | 2009-09-30 | 2010-04-21 | 烁光特晶科技有限公司 | Method for preparing LED by using transparent ceramics |
| CN102093037A (en) * | 2010-12-03 | 2011-06-15 | 清华大学 | Method for preparing semitransparent alumina ceramic by introducing sintering auxiliary agent through impregnated blank |
| CN102757237A (en) * | 2012-06-28 | 2012-10-31 | 航天材料及工艺研究所 | Method for adding ceramic material sintering aid |
| CN103304242A (en) * | 2013-06-13 | 2013-09-18 | 景德镇陶瓷学院 | Method for adding ceramic sintering auxiliary |
| CN104291796A (en) * | 2014-09-23 | 2015-01-21 | 上海三思电子工程有限公司 | Preparation method of transparent fluorescent ceramic for LEDs (light-emitting diodes) |
| CN104818023A (en) * | 2015-03-19 | 2015-08-05 | 合肥工业大学 | Rare earth luminescent material preparation method containing crystal defect repair technology and product thereof |
| CN108997998A (en) * | 2017-06-06 | 2018-12-14 | 深圳市光峰光电技术有限公司 | Fluorescent powder grain of monodispersed core-shell structural and preparation method thereof |
-
2016
- 2016-09-09 CN CN201610812030.1A patent/CN107805056A/en active Pending
-
2017
- 2017-06-01 WO PCT/CN2017/086863 patent/WO2018045782A1/en active Application Filing
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1134692A (en) * | 1993-11-12 | 1996-10-30 | 美国3M公司 | Abrasive grain and method for making the same |
| US5587346A (en) * | 1995-06-16 | 1996-12-24 | Osram Sylvania, Inc. | Translucent polycrystalline alumina |
| CN1263877A (en) * | 1999-01-29 | 2000-08-23 | 住友化学工业株式会社 | Semi-transparent alumina sintered substance and its production |
| JP2005340240A (en) * | 2004-05-24 | 2005-12-08 | Cimeo Precision Co Ltd | Transmitting light color converting member and manufacturing method thereof |
| CN101697367A (en) * | 2009-09-30 | 2010-04-21 | 烁光特晶科技有限公司 | Method for preparing LED by using transparent ceramics |
| CN102093037A (en) * | 2010-12-03 | 2011-06-15 | 清华大学 | Method for preparing semitransparent alumina ceramic by introducing sintering auxiliary agent through impregnated blank |
| CN102757237A (en) * | 2012-06-28 | 2012-10-31 | 航天材料及工艺研究所 | Method for adding ceramic material sintering aid |
| CN103304242A (en) * | 2013-06-13 | 2013-09-18 | 景德镇陶瓷学院 | Method for adding ceramic sintering auxiliary |
| CN104291796A (en) * | 2014-09-23 | 2015-01-21 | 上海三思电子工程有限公司 | Preparation method of transparent fluorescent ceramic for LEDs (light-emitting diodes) |
| CN104818023A (en) * | 2015-03-19 | 2015-08-05 | 合肥工业大学 | Rare earth luminescent material preparation method containing crystal defect repair technology and product thereof |
| CN108997998A (en) * | 2017-06-06 | 2018-12-14 | 深圳市光峰光电技术有限公司 | Fluorescent powder grain of monodispersed core-shell structural and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王桂茹: "《催化剂与催化作用》", 31 August 2000, 大连理工大学出版社 * |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109095923A (en) * | 2017-06-20 | 2018-12-28 | 深圳市光峰光电技术有限公司 | A kind of preparation method and luminescent ceramic composite of luminescent ceramic composite |
| WO2019179119A1 (en) * | 2018-03-21 | 2019-09-26 | 深圳光峰科技股份有限公司 | Light-emitting ceramic and preparation method therefor |
| CN110294628A (en) * | 2018-03-21 | 2019-10-01 | 深圳光峰科技股份有限公司 | Luminescent ceramic and preparation method thereof |
| CN110342908A (en) * | 2018-04-05 | 2019-10-18 | 日亚化学工业株式会社 | The manufacturing method of ceramic composite, projector light source and ceramic composite |
| CN110386822B (en) * | 2018-04-19 | 2021-02-26 | 深圳光峰科技股份有限公司 | Complex phase fluorescent ceramic and preparation method thereof |
| WO2019200934A1 (en) * | 2018-04-19 | 2019-10-24 | 深圳光峰科技股份有限公司 | Multiphase fluorescent ceramic and preparation method therefor |
| CN110386820A (en) * | 2018-04-19 | 2019-10-29 | 深圳光峰科技股份有限公司 | A kind of fluorescence ceramics and preparation method thereof of aluminum oxynitride matrix |
| CN110386822A (en) * | 2018-04-19 | 2019-10-29 | 深圳光峰科技股份有限公司 | A kind of complex phase fluorescence ceramics and preparation method thereof |
| CN110386820B (en) * | 2018-04-19 | 2021-02-26 | 深圳光峰科技股份有限公司 | Aluminum oxynitride matrix fluorescent ceramic and preparation method thereof |
| CN110386818A (en) * | 2018-04-23 | 2019-10-29 | 中国科学院上海光学精密机械研究所 | Mix zirconium terbium aluminium garnet magnetic rotation crystalline ceramics and preparation method thereof |
| CN111039660A (en) * | 2018-10-11 | 2020-04-21 | 深圳光峰科技股份有限公司 | Fluorescent ceramic, preparation method thereof, light source device and projection device |
| CN111039660B (en) * | 2018-10-11 | 2021-10-26 | 深圳光峰科技股份有限公司 | Fluorescent ceramic, preparation method thereof, light source device and projection device |
| CN111732434A (en) * | 2020-07-07 | 2020-10-02 | 韶关学院 | Ceramic preparation method using in-situ generated oxide as sintering aid |
| CN114394822A (en) * | 2022-01-30 | 2022-04-26 | 中国科学院宁波材料技术与工程研究所 | Face-centered structure composite ceramic, preparation method thereof and laser white light source device |
| CN114538931A (en) * | 2022-03-11 | 2022-05-27 | 北京理工大学 | High-performance AlON transparent ceramic and low-temperature rapid preparation method thereof |
| CN114538931B (en) * | 2022-03-11 | 2022-11-29 | 北京理工大学 | High-performance AlON transparent ceramic and low-temperature rapid preparation method thereof |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
| CN114656277B (en) * | 2022-03-17 | 2022-12-27 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2018045782A1 (en) | 2018-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107805056A (en) | The preparation method and ceramic composite of ceramic composite, light supply apparatus | |
| CN107285746B (en) | Preparation method of alumina matrix fluorescent ceramic and related fluorescent ceramic | |
| CN107285745B (en) | Preparation method of alumina matrix fluorescent ceramic and related fluorescent ceramic | |
| CN107200588B (en) | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic | |
| CN109467453B (en) | Fluorescent ceramic with characteristic microstructure and preparation method and application thereof | |
| CN112441817B (en) | Fluorescent ceramic, preparation method thereof and light source device | |
| EP3553041B1 (en) | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter | |
| US9260340B2 (en) | Luminous nano-glass-ceramics used as white LED source and preparing method of luminous nano-glass-ceramics | |
| CN112939578B (en) | Fluorescent ceramic, preparation method thereof, light-emitting device and projection device | |
| CN110240468B (en) | Fluorescent ceramic and preparation method thereof | |
| CN108947516A (en) | A kind of (Cu, Ce): YAG transparent fluorescent ceramic and the preparation method and application thereof | |
| CN107384398A (en) | A kind of YAG fluorescent powder and preparation method thereof and YAG fluorescence ceramics prepared therefrom | |
| WO2021135883A1 (en) | Preparation method for fluorescent ceramic and fluorescent ceramic | |
| CN107200587B (en) | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic | |
| CN113045205A (en) | Green fluorescent ceramic and preparation method and application thereof | |
| CN113402269A (en) | Preparation method of three-color transparent fluorescent ceramic capable of adjusting white light of different degrees | |
| CN111517804A (en) | Nitride red complex-phase fluorescent ceramic and preparation method thereof | |
| CN107200589B (en) | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic | |
| CN111039660B (en) | Fluorescent ceramic, preparation method thereof, light source device and projection device | |
| CN106380208A (en) | High-thermal-conductivity silicon nitride-aluminum nitride multiphase ceramic substrate of LED and manufacturing method thereof | |
| CN112979162A (en) | Preparation method of glass ceramic fluorescent sheet with Ra being larger than 80 for automobile illumination | |
| CN112239352A (en) | Complex phase fluorescent ceramic material and preparation method thereof | |
| CN116177995B (en) | Preparation method of fluorescent ceramic based on 3D printing composite structure | |
| RU2808387C1 (en) | METHOD FOR PRODUCING LUMINESCENT CERAMICS CONTAINING YAG:Ce PHASE FOR WHITE LIGHT SOURCES | |
| CN117964358A (en) | Preparation method of high-transmittance Ce-YAG transparent ceramic |
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 | ||
| CB02 | Change of applicant information |
Address after: 518000 20-22, 20-22 headquarters building, 63 high tech Zone, Xuefu Road, Nanshan District, Guangdong Province, Guangdong. Applicant after: SHENZHEN GUANGFENG TECHNOLOGY Co.,Ltd. Address before: 518055 Guangdong province Shenzhen Nanshan District Xili town Cha Guang road Shenzhen integrated circuit design application Industrial Park 401 Applicant before: APPOTRONICS Corp.,Ltd. Address after: 518000 20-22, 20-22 headquarters building, 63 high tech Zone, Xuefu Road, Nanshan District, Guangdong Province, Guangdong. Applicant after: APPOTRONICS Corp.,Ltd. Address before: 518000 20-22, 20-22 headquarters building, 63 high tech Zone, Xuefu Road, Nanshan District, Guangdong Province, Guangdong. Applicant before: SHENZHEN GUANGFENG TECHNOLOGY Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180316 |
|
| RJ01 | Rejection of invention patent application after publication |