WO2018103481A1 - 陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 - Google Patents
陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 Download PDFInfo
- Publication number
- WO2018103481A1 WO2018103481A1 PCT/CN2017/109317 CN2017109317W WO2018103481A1 WO 2018103481 A1 WO2018103481 A1 WO 2018103481A1 CN 2017109317 W CN2017109317 W CN 2017109317W WO 2018103481 A1 WO2018103481 A1 WO 2018103481A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- phosphor
- ceramic composite
- alumina
- coated
- particle diameter
- 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.)
- Ceased
Links
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
- C04B35/111—Fine ceramics
- C04B35/115—Translucent or transparent products
-
- 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
- C04B35/62802—Powder coating materials
- C04B35/62805—Oxide ceramics
- C04B35/62813—Alumina or aluminates
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/028—Beta-aluminas
-
- 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
-
- 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
- C04B35/111—Fine ceramics
- C04B35/113—Fine ceramics based on beta-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
- C04B35/01—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
- C04B35/111—Fine ceramics
- C04B35/117—Composites
-
- 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
- C04B35/16—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 silicates other than clay
-
- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
-
- 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
- C04B35/16—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 silicates other than clay
- C04B35/22—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 silicates other than clay rich in calcium oxide, e.g. wollastonite
-
- 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
- C04B35/44—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- 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
- 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
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- 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 materials, e.g. electroluminescent or chemiluminescent
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- 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 materials, e.g. electroluminescent or chemiluminescent
- C09K11/08—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials
- C09K11/77—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent materials, e.g. electroluminescent or chemiluminescent containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7774—Aluminates
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
- H10H20/80—Constructional details
- H10H20/85—Packages
- H10H20/851—Wavelength conversion means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00805—Details of the particulate material
-
- 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
- C04B2235/30—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
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
-
- 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
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium 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
- 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
- C04B2235/3225—Yttrium oxide 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
- C04B2235/30—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
- C04B2235/3229—Cerium 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
- C04B2235/30—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
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
-
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
-
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3454—Calcium silicates, e.g. wollastonite
-
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
-
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—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
- C04B2235/02—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
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- 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
- C04B2235/5463—Particle size distributions
- C04B2235/5472—Bimodal, multi-modal or multi-fraction
-
- 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
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/604—Pressing at temperatures other than sintering temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/782—Grain size distributions
- C04B2235/783—Bimodal, multi-modal or multi-fractional
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Definitions
- the invention relates to the technical field of luminescent materials, in particular to a method for preparing a ceramic composite material, a ceramic composite material and a wavelength converter.
- the phosphor package of the wavelength conversion device is mainly a package of an organic resin, an organic silica gel and an inorganic glass, and the wavelength conversion device of the technical solution has poor thermal conductivity and poor heat resistance.
- a phosphor is sintered together with a permeable inorganic ceramic, and the obtained ceramic composite material has high thermal conductivity performance and heat resistance.
- the main object of the present invention is to provide a method for preparing a ceramic composite material, which aims to obtain a ceramic composite material having high light efficiency, high thermal conductivity and high mechanical properties.
- the method for preparing a ceramic composite material comprises the following steps:
- the mass ratio of Al 2 O 3 to the phosphor 100, the aluminum salt solution and the phosphor are respectively disposed;
- the suspension is titrated with the aluminum salt solution to obtain a phosphor coated with a film of Al 2 O 3 hydrate;
- the phosphor coated with the Al 2 O 3 hydrate film is calcined to obtain an Al 2 O 3 coated phosphor
- the mixed powder is pre-compressed and sintered to obtain the ceramic composite.
- the phosphor comprises Ca 3 Al 2 Si 3 O 12 , Ca 3 Sc 2 Si 3 O 12 , Gd 3 Al 5 O 12 , Gd 3 Ga 5 O 12 , Tb 3 Al 5 O 12 , Tb 3 Ga 5 O 12 , Y 3 Al 5 O 12 , Y 3 Ga 5 O 12 , Lu 3 Al 5 O 12 , Lu 3 Ga 5 O 12 and Y 3 Mg 2 AlSi 2 O 12 doped with Ce 3+ fluorescence At least one of the powders.
- the phosphor has a particle size ranging from 13 ⁇ m to 20 ⁇ m.
- the concentration of the aluminum salt solution is from 0.01 mol/L to 1 mol/L.
- the temperature of the suspension is 40° C. to 70° C.
- the stirring rate is 100 r/min to 300 r/min
- the titration rate is It is 5 mL/min to 50 mL/min.
- the calcination temperature is 300 ° C to 600 ° C, and the calcination time is 2 h to 5 h.
- the pre-pressing process is carried out at a pressure of 5 MPa to 15 MPa.
- the sintering process is performed under an argon atmosphere, the sintering temperature is 1250 ° C to 1550 ° C, the sintering pressure is 30 MPa to 200 MPa, and the holding time is 30 min to 360 min.
- a particle diameter is further added.
- the alumina powder of 0.01 ⁇ m to 0.1 ⁇ m has a molar ratio of the alumina powder of 0.01 ⁇ m to 0.1 ⁇ m to the alumina powder of 0.1 ⁇ m to 1 ⁇ m (0.1 to 1): 100.
- the step of mixing the Al 2 O 3 coated phosphor with the mixed alumina powder comprises:
- the Al 2 O 3 coated phosphor is added to the ball mill jar and ball milling is continued for 30 min to 60 min.
- the present invention also provides a ceramic composite material comprising an alumina matrix, a phosphor uniformly distributed on the alumina matrix, and a scattering center uniformly distributed in the alumina matrix, wherein the alumina matrix is In the alumina ceramic, the scattering center is alumina particles, and the alumina particles have a particle diameter ranging from 1 ⁇ m to 10 ⁇ m, and the phosphor particles have a particle diameter ranging from 13 ⁇ m to 20 ⁇ m.
- the invention also proposes a wavelength converter comprising the ceramic composite as described above material.
- a small amount of fine particle size Al 2 O 3 particles may be coated on the surface of the phosphor particle by a liquid phase precipitation method, and then the product is made to have a medium particle size.
- Al 2 O 3 particles and larger particle size Al 2 O 3 particles are mixed so that a small amount of fine particle size Al 2 O 3 particles (ie, Al 2 O 3 film) coated on the surface of the phosphor particles are sintered. It can take the lead in entering the liquid phase, which improves the sintering performance of the ceramic composite and can effectively improve the bonding force between the phosphor phase and the Al 2 O 3 phase in the ceramic composite.
- dissolution - reprecipitation mechanism can effectively inhibit the median particle diameter of Al 2 O 3 particles abnormal growth during sintering, and to enhance the performance of Al 2 O 3 matrix.
- Larger particle size Al 2 O 3 particles can be used as scattering particles in ceramic composites. Thereby, a ceramic composite material with high light efficiency, high thermal conductivity and high mechanical properties is prepared.
- the invention provides a preparation method of a ceramic composite material, which aims to obtain a ceramic composite material with high luminous efficiency, high thermal conductivity, high mechanical properties and adjustable blue light transmittance, and is applied to a high performance laser light source.
- the preparation method of the ceramic composite material comprises the following steps:
- step S100 an aluminum salt solution and a phosphor are respectively disposed according to a mass ratio of Al 2 O 3 to a phosphor (0.1 to 1): 100. among them,
- the phosphor comprises Ca 3 Al 2 Si 3 O 12 , Ca 3 Sc 2 Si 3 O 12 , Gd 3 Al 5 O 12 , Gd 3 Ga 5 O 12 , Tb 3 Al 5 O 12 , Tb 3 Ga 5 O 12 And Y 3 Al 5 O 12 , Y 3 Ga 5 O 12 , Lu 3 Al 5 O 12 , Lu 3 Ga 5 O 12 and Y 3 Mg 2 AlSi 2 O 12 are doped with at least Ce 3+ phosphor One. Further, the phosphor has a particle diameter ranging from 13 ⁇ m to 20 ⁇ m, preferably 15 ⁇ m to 17 ⁇ m.
- the concentration of the aluminum salt solution is from 0.01 mol/L to 1 mol/L, preferably from 0.2 mol/L to 0.5 mol/L.
- the aluminum salt solution may be selected from an aluminum nitrate solution.
- the mass ratio of Al 2 O 3 to the phosphor is first determined, and a certain amount of phosphor is weighed; then, according to the quality of the phosphor and Al 2 O 3 and The mass ratio of the phosphor is calculated, and the mass of the desired Al 2 O 3 is calculated, and then the number of moles of Al 3+ is obtained by conversion; then the mass of the corresponding aluminum salt is converted according to the number of moles of Al 3+ ;
- the aluminum salt solution of the corresponding quality is configured to obtain an aluminum salt solution, and the steps of separately configuring the aluminum salt solution and the phosphor are completed.
- step S200 the phosphor is dispersed in a buffer solution having a pH of 4.5 to 5.5 to obtain a suspension.
- the buffer solution may be selected from a citric acid-sodium hydroxide solution, and the concentration of citric acid in the citric acid-sodium hydroxide solution may be 0.8 mol/L to 1.2 mol/L.
- step S300 the suspension is titrated with the aluminum salt solution to obtain a phosphor coated with a film of Al 2 O 3 hydrate. among them,
- the temperature of the suspension is 40 ° C to 70 ° C
- the stirring rate is 100 r / min to 300 r / min
- the titration rate is 5 mL / min ⁇ 50 mL / min.
- the temperature is kept constant and stirred for 1 h to 2 h, and the pH value can be adjusted to a range of 6 to 7 by using a sodium hydroxide solution.
- step S400 the phosphor coated with the Al 2 O 3 hydrate film is calcined to obtain an Al 2 O 3 coated phosphor. among them,
- the phosphor powder coated with the Al 2 O 3 hydrate film obtained by the separation was washed with water, dehydrated 3-5 times, and dried at 75 ° C to 85 ° C.
- the calcination temperature is from 300 ° C to 600 ° C, and the calcination time is from 2 h to 5 h.
- the surface of the phosphor is coated with fine particle diameter Al 2 O 3 particles.
- step S500 the alumina powder having a particle diameter of 0.1 ⁇ m to 1 ⁇ m and the alumina powder having a particle diameter of 1 ⁇ m to 10 ⁇ m are arranged in a molar ratio of 100: (0.1 to 5) to obtain a mixed alumina powder. among them,
- the alumina powder having a particle diameter of 0.1 ⁇ m to 1 ⁇ m preferably has a particle diameter ranging from 0.1 ⁇ m to 0.3 ⁇ m.
- the alumina powder having a particle diameter of 1 ⁇ m to 10 ⁇ m (that is, the Al 2 O 3 particles having a larger particle diameter) preferably has a particle diameter ranging from 3 ⁇ m to 5 ⁇ m.
- alumina powder having a particle diameter of 0.01 ⁇ m to 0.1 ⁇ m may be further added, preferably having a particle diameter ranging from 0.02 ⁇ m to 0.05 ⁇ m, and having an oxidation particle diameter of 0.01 ⁇ m to 0.1 ⁇ m.
- the molar ratio of the aluminum powder to the alumina powder having a particle diameter of 0.1 ⁇ m to 1 ⁇ m is (0.1 to 1): 100.
- Step S600 mixing the Al 2 O 3 coated phosphor with the mixed alumina powder to obtain a mixed powder, wherein the Al 2 O 3 coated phosphor accounts for 40% of the weight of the mixed powder. % ⁇ 90%. among them,
- the Al 2 O 3 coated phosphor accounts for 50% to 70% by weight of the total powder.
- the step of mixing the Al 2 O 3 coated phosphor with the mixed alumina powder comprises:
- the Al 2 O 3 coated phosphor is added to the ball mill jar and ball milling is continued for 30 min to 60 min.
- step S700 the mixed powder is pre-compressed and sintered to obtain the ceramic composite material. among them,
- the pre-pressing process is carried out at a pressure of 5 MPa to 15 MPa.
- the sintering process is carried out under an argon atmosphere, the sintering temperature is 1250 ° C ⁇ 1550 ° C, the sintering pressure is 30 MPa ⁇ 200 MPa, and the holding time is 30 min - 360 min. Among them, the sintering pressure is preferably 40 MPa to 100 MPa.
- the mixed powder may be such that during sintering, the particle size of the fine particles and Al 2 O 3 Average particle diameter of Al 2 O 3 particles can be sufficiently sintered into the liquid phase, the larger particles
- the Al 2 O 3 particles of the diameter are only partially involved in sintering, or do not participate in sintering, and the phosphor does not participate in sintering.
- the crystal form and grain size of the phosphor do not change, and the crystal form of the larger particle size Al 2 O 3 particles will change from the other phase to the ⁇ phase, and the size thereof will increase due to the dissolution and re-precipitation mechanism.
- the dissolution re-precipitation mechanism in the technical solution of the present invention is: during the sintering process, the fine particle size Al 2 O 3 particles will first enter the liquid phase and be fully melted, and the medium-sized Al 2 O 3 particles will partially enter the liquid phase. Also, the smaller the particle size, the easier the particles enter the liquid phase. These liquid phases flow in the interstitial spaces and become the primary means of material migration. When these liquid phases flow over the surface of large particles, small crystal grains of Al 2 O 3 are precipitated on the surface (the surface of small particles may also precipitate small crystal grains of Al 2 O 3 , but the precipitation on the surface of large particles may be larger. , to a higher degree), at this time, Al 2 O 3 small crystal precipitation is divided into two types:
- the second is to precipitate on the surface of larger particle size Al 2 O 3 particles.
- the small crystal grains of these Al 2 O 3 fractions (depending on the temperature, the degree will be different) will be combined with the larger particle size Al 2 O 3 particles. (Enggered by larger particle size Al 2 O 3 particles) becomes larger particles while absorbing a large amount of energy.
- the continued growth of larger particle size Al 2 O 3 particles actually weakens the abnormal growth of medium-sized Al 2 O 3 particles and promotes the majority of medium-sized Al 2 O particles. 3
- the fine particle size Al 2 O 3 particles and the medium particle size Al 2 O 3 particles are ceramic continuous substrates with certain light transmission properties, phosphors and larger particle size Al 2 O 3
- the particles become particles dispersed in a continuous matrix of ceramics, which have a scattering effect on light.
- the phosphor has an absorption effect on a short-wavelength blue light such as 445 nm to 460 nm
- the larger particle diameter Al 2 O 3 particles have a scattering and reflection effect on light in a short wavelength to a visible light wavelength range.
- the content of the larger particle size Al 2 O 3 particles the degree of penetration and scattering of the blue light can be changed, and the color temperature of the ceramic composite material can be changed.
- a small amount of fine particle diameter Al 2 O 3 particles ie, an Al 2 O 3 film
- the product is passed through Mixing with medium-sized Al 2 O 3 particles and larger particle size Al 2 O 3 particles allows a small amount of fine particle size Al 2 O 3 particles (ie, Al 2 O 3 ) coated on the surface of the phosphor particles.
- the film can be firstly introduced into the liquid phase during sintering, so that the sintering property of the ceramic composite material can be improved, and the bonding force between the phosphor phase and the Al 2 O 3 phase in the ceramic composite material can be effectively improved.
- the abnormal growth of the medium-sized Al 2 O 3 particles during sintering can be effectively suppressed, and the properties of the Al 2 O 3 matrix can be improved.
- Larger particle size Al 2 O 3 particles can be used as scattering particles in ceramic composites. Thereby, a ceramic composite material with high light efficiency, high thermal conductivity, high mechanical properties and adjustable blue light transmittance is prepared.
- a citric acid-sodium hydroxide solution having a pH of 5.0 and a concentration of 1.0 mol/L was prepared, followed by addition of 2 wt% of PEG 4000, and ultrasonication was carried out. Thereafter, YAG:Ce 3+ phosphor was added, and after ultrasonic dispersion, a magnetic stir bar was added, and the mixture was stirred on a magnetic stirrer to obtain a phosphor suspension.
- the phosphor suspension was heated to 50 ° C, and stirring was continued at a stirring rate of 150 r / min. Thereafter, the aluminum nitrate solution was dropped into the phosphor suspension at a titration rate of 30 mL / min with a dropper. After the completion of the titration, the mixture was kept warm and stirred for 1 hour, and the pH was adjusted to 6.5 with a sodium hydroxide solution to obtain a YAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate.
- the mixture was centrifuged using a YAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate, washed with water, dehydrated three times, and dried at 80 ° C, followed by calcination at 500 ° C for 5 h to obtain Al 2 O. 3 coated YAG: Ce 3+ phosphor.
- a 1 wt% solution of PEG 4000-ethanol was prepared, and then mixed Al 2 O 3 powder was added thereto, ultrasonically dispersed, placed in a polytetrafluoroethylene ball mill jar, and an appropriate amount of high-purity zirconia balls were added and ball-milled for 12 hours. Thereafter, Al 2 O 3 coated YAG:Ce 3+ phosphors, which accounted for 50% of the total powder weight, were added to the ball mill jar and ball milling was continued for 40 min.
- the ball-milled slurry was vacuum dried, pulverized, and sieved to obtain a mixed powder.
- a citric acid-sodium hydroxide solution having a pH of 5.0 and a concentration of 1.0 mol/L was prepared, followed by addition of 3 wt% of PEG 4000, and ultrasonication was carried out. Thereafter, YAG:Ce 3+ phosphor was added, and after ultrasonic dispersion, a magnetic stir bar was added, and the mixture was stirred on a magnetic stirrer to obtain a phosphor suspension.
- the phosphor suspension was heated to 65 ° C, and stirring was continued at a stirring rate of 280 r / min. Thereafter, the aluminum nitrate solution was dropped into the phosphor suspension at a titration rate of 45 mL / min with a dropper. After the completion of the titration, the mixture was kept warm and stirred for 1 hour, and the pH was adjusted to 7.0 with a sodium hydroxide solution to obtain a YAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate.
- the mixture was centrifuged using a YAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate, washed with water, dehydrated 5 times, and dried at 85 ° C, followed by calcination at 320 ° C for 5 h to obtain Al 2 O. 3 coated YAG: Ce 3+ phosphor.
- High-purity ultrafine Al 2 O 3 powder (particle size 0.01-0.1 ⁇ m), high-purity ultrafine Al 2 O 3 powder (particle size 0.1-1 ⁇ m), and high-purity Al 2 O 3 powder (particle size is selected) 1 to 10 ⁇ m), the molar ratio of 1:100:3 is configured to mix Al 2 O 3 powder.
- a 2 wt% solution of PEG 4000-ethanol was prepared, and then mixed Al 2 O 3 powder was added thereto, ultrasonically dispersed, placed in a polytetrafluoroethylene ball mill jar, and an appropriate amount of high-purity zirconia balls were added and ball-milled for 24 hours. Thereafter, 70% of the total powder weight of Al 2 O 3 coated YAG:Ce 3+ phosphor was added to the ball mill jar and ball milling was continued for 60 min.
- the ball-milled slurry was vacuum dried, pulverized, and sieved to obtain a mixed powder.
- a citric acid-sodium hydroxide solution having a pH of 5.0 and a concentration of 1.0 mol/L was prepared, followed by addition of 1 wt% of PEG 4000, and ultrasonication was carried out. Thereafter, LuAG:Ce 3+ phosphor was added, and after ultrasonic dispersion, a magnetic stir bar was added, and the mixture was stirred on a magnetic stirrer to obtain a phosphor suspension.
- the phosphor suspension was heated to 40 ° C, and stirring was continued at a stirring rate of 110 r/min. Thereafter, the aluminum nitrate solution was dropped into the phosphor suspension at a titration rate of 15 mL/min with a pipette. After the completion of the titration, the mixture was kept warm and stirred for 1 hour, and the pH was adjusted to 7.0 with a sodium hydroxide solution to obtain a LuAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate.
- the mixture was centrifuged using a LuAG:Ce 3+ phosphor coated with a film of Al 2 O 3 hydrate, washed with water, dehydrated 4 times, and dried at 80 ° C, followed by calcination at 300 ° C for 5 h to obtain Al 2 O. 3 coated LuAG: Ce 3+ phosphor.
- a high-purity ultrafine Al 2 O 3 powder (having a particle diameter of 0.1 to 1 ⁇ m) and a high-purity Al 2 O 3 powder (having a particle diameter of 1 to 10 ⁇ m) were used, and a molar ratio of 20:1 was used to mix the Al 2 O 3 powder.
- a 3 wt% solution of PEG 4000-ethanol was prepared, and then mixed Al 2 O 3 powder was added thereto, ultrasonically dispersed, placed in a polytetrafluoroethylene ball mill jar, and an appropriate amount of high-purity zirconia balls were added and ball-milled for 8 hours. Thereafter, Al 2 O 3 coated LuAG:Ce 3+ phosphors, which accounted for 45% of the total powder weight, were added to the ball mill jar and ball milling was continued for 30 min.
- the ball-milled slurry was vacuum dried, pulverized, and sieved to obtain a mixed powder.
- the preparation method of the ceramic composite material is carried out by the preparation method described in Examples 1-3, and the ternary system of the alumina particles contributes to the sintering process of the ceramic composite material, wherein the small particle alumina can help
- the role of the solvent, and the large-particle alumina not only serves to improve the filling efficiency at the time of powder filling, but also improves liquid phase sintering and prevents abnormal growth of crystal grains during sintering.
- large-grained alumina also has a scattering effect on light, which can be changed by adjusting the content of large-particle alumina.
- the ceramic composite can adjust the color temperature of the ceramic composite for the transmission and reflection properties of the excited blue light.
- the ternary system is sintered, it is also beneficial to improve the degree of bonding between the phosphor particles and the alumina matrix, and improve the mechanical properties of the ceramic composite.
- the invention also provides a ceramic composite material comprising an alumina matrix, a phosphor uniformly distributed on the alumina matrix, and a scattering center uniformly distributed in the alumina matrix, wherein the alumina matrix is continuous
- the ceramic is characterized in that the scattering center is alumina particles, and the alumina particles have a particle diameter ranging from 1 ⁇ m to 10 ⁇ m, and the phosphor particles have a particle diameter ranging from 13 ⁇ m to 20 ⁇ m.
- the ceramic composite material has high temperature resistance, good thermal conductivity and excellent mechanical properties.
- the invention also proposes a wavelength converter comprising a ceramic composite as previously described. Since all the technical solutions of all the foregoing embodiments are adopted in the present wavelength converter, at least all the beneficial effects brought by the technical solutions of the foregoing embodiments are not repeated herein.
- the wavelength converter can be used in fixed installation environments as well as in motion devices (eg, wavelength conversion color wheel).
- the wavelength converter can be applied to the field of illumination, such as various lamps - street lamps, searchlights, stage lights, car headlights; the wavelength converter can also be applied to display systems, such as projectors, televisions, etc. Its use needs.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- General Chemical & Material Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Luminescent Compositions (AREA)
Abstract
一种陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器,其中,制备方法包括步骤:按Al 2O 3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;将荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;用铝盐溶液对悬浮液进行滴定,得到包覆有Al 2O 3水合物薄膜的荧光粉;将包覆有Al 2O 3水合物薄膜的荧光粉进行煅烧,得到Al 2O 3包覆的荧光粉;将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;将Al 2O 3包覆的荧光粉与混合氧化铝粉末进行混合,得到混合粉末,其中,Al 2O 3包覆的荧光粉占混合粉末重量的40%~90%;对混合粉末进行预压制、烧结,得到陶瓷复合材料。
Description
本发明涉及发光材料技术领域,特别涉及一种陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器。
在照明显示领域,波长转换装置的荧光粉封装主要是有机树脂、有机硅胶和无机玻璃的封装,该类技术方案的波长转换装置导热差、耐热差。为解决这一问题,有技术将荧光粉与可透光的无机陶瓷烧结在一起,获得的陶瓷复合材料具有很高的热导率性能和耐热性能。
目前,对于荧光粉封装于Al2O3的陶瓷复合材料而言,普遍存在着荧光粉相与Al2O3相之间结合力较弱的问题,导致其机械性能不高。并且,陶瓷复合材料大多还存在光效偏低,加工过程中易出现荧光粉颗粒拔出、表面难抛光等问题,从而影响陶瓷复合材料的性能。
发明内容
本发明的主要目的是提供一种陶瓷复合材料的制备方法,旨在制得高光效、高热导率、高机械性能的陶瓷复合材料。
为实现上述目的,本发明提出的陶瓷复合材料的制备方法包括以下步骤:
按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;
将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;
用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉;
将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉;
将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;
将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%;
对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。
可选地,所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。
可选地,所述荧光粉的粒径范围是13μm~20μm。
可选地,所述铝盐溶液的浓度为0.01mol/L~1mol/L。
可选地,在所述用所述铝盐溶液对所述悬浮液进行滴定的步骤中,所述悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
可选地,所述煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
可选地,所述预压制过程在5MPa~15MPa压强下进行。
可选地,所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。
可选地,在所述将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好的步骤中,还加入粒径为0.01μm~0.1μm的氧化铝粉末,所述0.01μm~0.1μm的氧化铝粉末与所述0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
可选地,所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:
将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;
将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
本发明还提出一种陶瓷复合材料,该陶瓷复合材料包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,所述氧化铝基质为氧化铝陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,荧光粉的粒径范围是13μm~20μm。
本发明还提出一种波长转换器,该波长转换器包括如上所述的陶瓷复合
材料。
本发明的技术方案,通过液相沉淀法,可先将微量细小粒径的Al2O3颗粒(即Al2O3薄膜)包覆于荧光粉颗粒表面,之后通过将产物与中等粒径的Al2O3颗粒、较大粒径的Al2O3颗粒进行混合,可使得包覆于荧光粉颗粒表面的微量细小粒径的Al2O3颗粒(即Al2O3薄膜)在烧结中能够率先进入液相,使得陶瓷复合材料的烧结性能得以改善,并可有效提高陶瓷复合材料中荧光粉相与Al2O3相之间的结合力。同时,通过溶解-再析出机制,可有效抑制中等粒径的Al2O3颗粒在烧结过程中的异常长大,提升Al2O3基体的各项性能。而较大粒径的Al2O3颗粒,则可作为陶瓷复合材料中的散射粒子。从而,制备得到高光效、高热导率、高机械性能的陶瓷复合材料。
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
另外,各个实施例之间的技术方案可以相互结合,但是必须是以本领域普通技术人员能够实现为基础,当技术方案的结合出现相互矛盾或无法实现时应当认为这种技术方案的结合不存在,也不在本发明要求的保护范围之内。
本发明提出一种陶瓷复合材料的制备方法,旨在制得高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料,以应用于高性能激光光源。
该陶瓷复合材料的制备方法,包括以下步骤:
步骤S100,按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉。其中,
所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。并且,所述荧光粉的粒径范围为13μm~20μm,优选为15μm~17μm。
所述铝盐溶液的浓度为0.01mol/L~1mol/L,优选为0.2mol/L~0.5mol/L。
所述铝盐溶液可选用硝酸铝溶液。
应当理解的,在实际配置铝盐溶液与荧光粉时,首先确定Al2O3与荧光粉的质量比,并称取一定质量的荧光粉;之后,根据荧光粉的质量以及Al2O3与荧光粉的质量比,计算得到所需Al2O3的质量,再经换算即可得到Al3+的摩尔数;继而根据Al3+的摩尔数换算出对应的铝盐的质量;最后,称取对应质量的铝盐进行配置,即可得到铝盐溶液,完成分别配置铝盐溶液与荧光粉的步骤。
步骤S200,将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液。其中,所述缓冲溶液可选用柠檬酸-氢氧化钠溶液,且所述柠檬酸-氢氧化钠溶液中柠檬酸的浓度可为0.8mol/L~1.2mol/L。
并且,将荧光粉分散于缓冲溶液之前,预先向缓冲溶液中加入1wt%~3wt%的PEG4000。
步骤S300,用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉。其中,
滴定过程中,悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
滴定完毕后,持续保温和搅拌1h~2h,并可选用氢氧化钠溶液将pH值调整到6~7的范围。
步骤S400,将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉。其中,
煅烧步骤前,包括:
将包覆有Al2O3水合物薄膜的荧光粉进行离心分离;
将分离所得的包覆有Al2O3水合物薄膜的荧光粉进行水洗、脱水3-5次,并在75℃~85℃下烘干。
在煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
需要说明的是,此时,荧光粉表面包覆的为细小粒径的Al2O3颗粒。
步骤S500,将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末。其中,
粒径为0.1μm~1μm的氧化铝粉末(即中等粒径的Al2O3颗粒)优选粒径范围是0.1μm~0.3μm。
粒径为1μm~10μm的氧化铝粉末(即较大粒径的Al2O3颗粒)优选粒径范围是3μm~5μm。
进一步地,在混合氧化铝粉末中,还可加入粒径为0.01μm~0.1μm的氧化铝粉末,其优选粒径范围是0.02μm~0.05μm,并且,粒径为0.01μm~0.1μm的氧化铝粉末与粒径为0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
步骤S600,将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%。其中,
优选地,Al2O3包覆的荧光粉占总粉末重量的50%~70%。
所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:
将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;
将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
步骤S700,对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。其中,
所述预压制过程在5MPa~15MPa压强下进行。
所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。其中,烧结压力优选为40MPa~100MPa。
需要说明的是,适当的控制烧结温度,可使得混合粉末在烧结过程中,细小粒径的Al2O3颗粒和中等粒径的Al2O3颗粒能够充分进入液相进行烧结,较大粒径的Al2O3颗粒则只有部分参与烧结,或不参与烧结,而荧光粉则不参与烧结。其中,荧光粉的晶型及晶粒尺寸不发生改变,较大粒径的Al2O3颗粒的
晶型会由其他相转变为α相,而其尺寸会因为溶解再析出机制而增大。
本发明技术方案中的溶解再析出机制为:烧结过程中,细小粒径的Al2O3颗粒会率先进入液相,并充分熔化,中等粒径的Al2O3颗粒会部分进入液相,并且,粒径越小的颗粒越容易进入液相。这些液相会在颗粒间隙中流动,成为物质迁移的主要方式。当这些液相流过大颗粒表面时,会在其表面析出Al2O3小晶粒(小颗粒表面也可析出Al2O3小晶粒的可能,只是在大颗粒表面析出的可能更大,程度更高),此时,Al2O3小晶粒析出分两种类型:
一是在荧光粉颗粒表面析出,但是由于荧光粉并不参与烧结,这些析出的Al2O3小晶粒会和周围的Al2O3晶粒通过烧结颈连接-融合-长大,成为与荧光粉颗粒紧密相连的氧化铝相;
二是在较大粒径的Al2O3颗粒表面析出,这些Al2O3小晶粒的部分(根据温度的不同,程度会不同)会与较大粒径的Al2O3颗粒相结合(被较大粒径的Al2O3颗粒吞并)变成更大的颗粒,同时吸收大量的能量。而较大粒径的Al2O3颗粒的继续长大,实际上就削弱了中等粒径的Al2O3颗粒的异常长大现象,促使占绝大部分比例的中等粒径的Al2O3颗粒长大的均匀性,从而使得光学和机械性能得以有效提高。
烧结后的陶瓷中,细小粒径的Al2O3颗粒和中等粒径的Al2O3颗粒为陶瓷的连续基质,具有一定的透光性能,荧光粉和较大粒径的Al2O3颗粒则成为分散于陶瓷的连续基质中的颗粒,对光具有散射作用。其中,荧光粉具有对如445nm~460nm的短波长的蓝光的吸收作用,较大粒径的Al2O3颗粒则对短波长至可见光波长范围内的光具有散射和反射作用。并且,通过调整较大粒径的Al2O3颗粒的含量,可改变蓝光的穿透和散射程度,进而可改变陶瓷复合材料的色温。
因此,可以理解的,本发明技术方案,通过液相沉淀法,可先将微量细小粒径的Al2O3颗粒(即Al2O3薄膜)包覆于荧光粉颗粒表面,之后通过将产物与中等粒径的Al2O3颗粒、较大粒径的Al2O3颗粒进行混合,可使得包覆于荧光粉颗粒表面的微量细小粒径的Al2O3颗粒(即Al2O3薄膜)在烧结中能够率先进入液相,使得陶瓷复合材料的烧结性能得以改善,并可有效提高陶瓷复合材料中荧光粉相与Al2O3相之间的结合力。同时,通过溶解-再析出机制,可有效抑制中等粒径的Al2O3颗粒在烧结过程中的异常长大,提升Al2O3基体的各项性
能。而较大粒径的Al2O3颗粒,则可作为陶瓷复合材料中的散射粒子。从而,制备得到高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料。
以下通过具体实施例对本发明技术方案进行具体说明。
实施例1:
称取适量的粒径为13μm~20μm的YAG:Ce3+荧光粉。
按照Al2O3与YAG:Ce3+荧光粉质量比1:100的比例,称取相应量的Al(NO3)3·9H2O配制成1mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入2wt%的PEG4000,并进行超声溶解。之后,加入YAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至50℃,在搅拌速率为150r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为30mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到6.5,得到包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉进行离心分离,水洗、脱水3次,并在80℃下烘干,之后在500℃条件下煅烧5h,得到Al2O3包覆的YAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.1~1μm)与高纯度Al2O3粉末(粒径为1~10μm),按摩尔比100:1配置成混合Al2O3粉末。
配制1wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨12h。之后,将占总粉末重量50%的Al2O3包覆的YAG:Ce3+荧光粉加入该球磨罐中,继续球磨40min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在10MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1250℃,烧结压力为100MPa时,保温60min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料YAG:Ce3+-Al2O3。
实施例2:
称取适量的粒径为13μm~20μm的YAG:Ce3+荧光粉。
按照Al2O3与YAG:Ce3+荧光粉质量比1:1000的比例,称取相应量的Al(NO3)3·9H2O配制成0.5mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入3wt%的PEG4000,并进行超声溶解。之后,加入YAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至65℃,在搅拌速率为280r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为45mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到7.0,得到包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的YAG:Ce3+荧光粉进行离心分离,水洗、脱水5次,并在85℃下烘干,之后在320℃条件下煅烧5h,得到Al2O3包覆的YAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.01~0.1μm)、高纯度超细Al2O3粉末(粒径为0.1~1μm)、及高纯度Al2O3粉末(粒径为1~10μm),按摩尔比1:100:3配置成混合Al2O3粉末。
配制2wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨24h。之后,将占总粉末重量70%的Al2O3包覆的YAG:Ce3+荧光粉加入该球磨罐中,继续球磨60min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在15MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1500℃,烧结压力为60MPa时,保温300min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料YAG:Ce3+-Al2O3。
实施例3:
称取适量的粒径为13μm~20μm的LuAG:Ce3+荧光粉。
按照Al2O3与LuAG:Ce3+荧光粉质量比1:500的比例,称取相应量的Al(NO3)3·9H2O配制成0.3mol/L的硝酸铝溶液。
配制pH值为5.0、浓度为1.0mol/L的柠檬酸-氢氧化钠溶液,继而加入1wt%的PEG4000,并进行超声溶解。之后,加入LuAG:Ce3+荧光粉,超声分散后,加入磁力搅拌子,并置于磁力搅拌器上搅拌均匀,得到荧光粉悬浮液。
将荧光粉悬浮液加热至40℃,在搅拌速率为110r/min条件下持续搅拌,之后,用滴管将硝酸铝溶液以为15mL/min的滴定速度匀速滴入荧光粉悬浮液中。滴定完毕后持续保温和搅拌1h,并用氢氧化钠溶液将pH值调整到7.0,得到包覆有Al2O3水合物薄膜的LuAG:Ce3+荧光粉。
使用包覆有Al2O3水合物薄膜的LuAG:Ce3+荧光粉进行离心分离,水洗、脱水4次,并在80℃下烘干,之后在300℃条件下煅烧5h,得到Al2O3包覆的LuAG:Ce3+荧光粉。
选用高纯度超细Al2O3粉末(粒径为0.1~1μm)与高纯度Al2O3粉末(粒径为1~10μm),按摩尔比20:1配置成混合Al2O3粉末。
配制3wt%的PEG4000-乙醇溶液,继而将混合Al2O3粉末加入其中,超声分散后,置于聚四氟乙烯球磨罐中,并加入适量的高纯氧化锆球,球磨8h。之后,将占总粉末重量45%的Al2O3包覆的LuAG:Ce3+荧光粉加入该球磨罐中,继续球磨30min。
将球磨后的浆料进行真空干燥,粉碎,过筛后,得到混合粉末。
称取适量的混合粉末,装入石墨模具中,在5MPa压强下进行预压制。之后将石墨模具放入热压烧结炉内,在氩气气氛下,在烧结温度为1300℃,烧结压力为50MPa时,保温180min。
烧结完成后,卸除压力并随炉冷却,即可得到陶瓷复合材料LuAG:Ce3+-Al2O3。
需要说明的是,利用实施例1-3所述的制备方法进行陶瓷复合材料的制备,氧化铝颗粒的三元体系有助于陶瓷复合材料的烧结过程,其中,小颗粒氧化铝可起到助溶剂的作用,而大颗粒氧化铝不仅可起到提高粉末装填时的填充效率之作用,在烧结时还能够改善液相烧结和防止晶粒的异常长大。并且,大颗粒氧化铝对光还具有散射作用,通过调整大颗粒氧化铝的含量可以改变
陶瓷复合材料对于激发蓝光的透射性能和反射性能,可以调整陶瓷复合材料的色温。此外,三元体系在进行烧结时,还有利于提高荧光粉颗粒和氧化铝基质之间结合程度,改善陶瓷复合材料的机械性能。
因此,利用实施例1-3所述的制备方法进行陶瓷复合材料的制备,可制得高光效、高热导率、高机械性能、蓝光透过率可调的陶瓷复合材料,可应用于高性能激光光源,特别是小型化的激光光源系统。
本发明还提出一种陶瓷复合材料,该陶瓷复合材料包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,其中氧化铝基质为连续的陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,荧光粉的粒径范围是13μm~20μm。
该陶瓷复合材料耐高温、导热性能好,而且机械性能优异。
本发明还提出一种波长转换器,该波长转换器包括如前所述的陶瓷复合材料。由于本波长转换器采用了前述所有实施例的全部技术方案,因此至少具有前述实施例的技术方案所带来的所有有益效果,在此不再一一赘述。该波长转换器可以应用于固定安装的环境,也可以应用于运动装置中(例如波长转换色轮)。该波长转换器可以应用到照明领域,如各种灯具——路灯、探照灯、舞台灯、汽车大灯;该波长转换器也可以应用到显示系统上,如投影机、电视机等,均能满足其使用需求。
以上所述仅为本发明的优选实施例,并非因此限制本发明的专利范围,凡是在本发明的发明构思下,利用本发明说明书内容所作的等效结构变换,或直接/间接运用在其他相关的技术领域均包括在本发明的专利保护范围内。
Claims (12)
- 一种陶瓷复合材料的制备方法,其特征在于,包括以下步骤:按Al2O3与荧光粉质量比(0.1~1):100,分别配置铝盐溶液与荧光粉;将所述荧光粉分散于pH值为4.5~5.5的缓冲溶液,得到悬浮液;用所述铝盐溶液对所述悬浮液进行滴定,得到包覆有Al2O3水合物薄膜的荧光粉;将所述包覆有Al2O3水合物薄膜的荧光粉进行煅烧,得到Al2O3包覆的荧光粉;将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好,得到混合氧化铝粉末;将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合,得到混合粉末,其中,所述Al2O3包覆的荧光粉占所述混合粉末重量的40%~90%;对所述混合粉末进行预压制、烧结,得到所述陶瓷复合材料。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述荧光粉包含Ca3Al2Si3O12、Ca3Sc2Si3O12、Gd3Al5O12、Gd3Ga5O12、Tb3Al5O12、Tb3Ga5O12、Y3Al5O12、Y3Ga5O12、Lu3Al5O12、Lu3Ga5O12及Y3Mg2AlSi2O12的掺杂有Ce3+的荧光粉中的至少一种。
- 如权利要求2所述的陶瓷复合材料的制备方法,其特征在于,所述荧光粉的粒径范围是13μm~20μm。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述铝盐溶液的浓度为0.01mol/L~1mol/L。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,在所述用所述铝盐溶液对所述悬浮液进行滴定的步骤中,所述悬浮液的温度为40℃~70℃,搅拌速率为100r/min~300r/min,滴定速度为5mL/min~50mL/min。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述煅烧过程中,煅烧温度为300℃~600℃,煅烧时间为2h~5h。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述预压制过程在5MPa~15MPa压强下进行。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,所述烧结过程在氩气气氛下进行,烧结温度为1250℃~1550℃,烧结压力为30MPa~200MPa,保温时间为30min~360min。
- 如权利要求1所述的陶瓷复合材料的制备方法,其特征在于,在所述将粒径为0.1μm~1μm的氧化铝粉末与粒径为1μm~10μm的氧化铝粉末按摩尔比100:(0.1~5)配置好的步骤中,还加入粒径为0.01μm~0.1μm的氧化铝粉末,所述0.01μm~0.1μm的氧化铝粉末与所述0.1μm~1μm的氧化铝粉末的摩尔比为(0.1~1):100。
- 如权利要求1-9任一项所述的陶瓷复合材料的制备方法,其特征在于,所述将所述Al2O3包覆的荧光粉与所述混合氧化铝粉末进行混合的步骤包括:将所述混合氧化铝粉末分散于质量百分浓度为1wt%~3wt%的PEG4000-乙醇溶液中,并置于球磨罐中,球磨6h~24h;将所述Al2O3包覆的荧光粉加入所述球磨罐中,继续球磨30min~60min。
- 一种陶瓷复合材料,其特征在于,包括氧化铝基质、均匀分布于所述氧化铝基质的荧光粉、及均匀分布于所述氧化铝基质的散射中心,所述氧化铝基质为氧化铝陶瓷,所述散射中心为氧化铝颗粒,且所述氧化铝颗粒的粒径范围是1μm~10μm,所述荧光粉的粒径范围是13μm~20μm。
- 一种波长转换器,其特征在于,包括如权利要求11所述的陶瓷复合材料。
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US16/468,112 US11267762B2 (en) | 2016-12-09 | 2017-11-03 | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter |
| EP17879386.5A EP3553041B1 (en) | 2016-12-09 | 2017-11-03 | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter |
| US17/647,810 US11697621B2 (en) | 2016-12-09 | 2022-01-12 | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611135583.4A CN108610023B (zh) | 2016-12-09 | 2016-12-09 | 陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 |
| CN201611135583.4 | 2016-12-09 |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US16/468,112 A-371-Of-International US11267762B2 (en) | 2016-12-09 | 2017-11-03 | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter |
| US17/647,810 Continuation US11697621B2 (en) | 2016-12-09 | 2022-01-12 | Preparation method for ceramic composite material, ceramic composite material, and wavelength converter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2018103481A1 true WO2018103481A1 (zh) | 2018-06-14 |
Family
ID=62492225
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CN2017/109317 Ceased WO2018103481A1 (zh) | 2016-12-09 | 2017-11-03 | 陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 |
Country Status (4)
| Country | Link |
|---|---|
| US (2) | US11267762B2 (zh) |
| EP (1) | EP3553041B1 (zh) |
| CN (1) | CN108610023B (zh) |
| WO (1) | WO2018103481A1 (zh) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115432957A (zh) * | 2022-08-30 | 2022-12-06 | 重庆大学 | 一种冷烧结制备ZnO-PTFE超疏水复合陶瓷的方法 |
| EP4328207A1 (en) * | 2022-08-24 | 2024-02-28 | Nichia Corporation | Sintered body and method for producing sintered body |
| CN118126717A (zh) * | 2024-01-26 | 2024-06-04 | 中国铁建投资集团有限公司 | 一种新型深红及近红外应力发光材料及其制备方法 |
| US12371383B2 (en) | 2020-08-07 | 2025-07-29 | Nichia Corporation | Rare earth aluminate sintered compact and method for producing rare earth aluminate sintered compact |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2020213456A1 (zh) * | 2019-04-18 | 2020-10-22 | ||
| CN110204324B (zh) * | 2019-05-15 | 2020-11-20 | 浙江大学 | 一种绿色荧光透明陶瓷的制备方法和应用 |
| JPWO2022107794A1 (zh) * | 2020-11-19 | 2022-05-27 | ||
| CN114478008B (zh) * | 2022-01-17 | 2023-04-07 | 江苏师范大学 | 一种固态照明用高显色指数高热稳定性的荧光陶瓷及其制备方法 |
| CN115947604A (zh) * | 2022-12-14 | 2023-04-11 | 福建臻璟新材料科技有限公司 | 一种氮化铝基质的荧光陶瓷及其制备方法 |
| CN116469609B (zh) * | 2023-04-29 | 2024-01-30 | 开开电缆科技有限公司 | 一种矿物质绝缘电缆及其制备方法 |
| CN117776705A (zh) * | 2023-12-27 | 2024-03-29 | 江苏师范大学 | 一种太阳光泵浦激光器用抗辐射复合透明陶瓷及其制备方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753457A (zh) * | 2016-02-02 | 2016-07-13 | 横店集团浙江英洛华电子有限公司 | 一种氧化铝荧光陶瓷材料及其制备方法和应用 |
| CN105906328A (zh) * | 2016-04-22 | 2016-08-31 | 横店集团浙江英洛华电子有限公司 | 一种氧化铝荧光陶瓷材料及其制备方法和应用 |
| CN106206904A (zh) * | 2015-04-29 | 2016-12-07 | 深圳市光峰光电技术有限公司 | 一种波长转换装置、荧光色轮及发光装置 |
Family Cites Families (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6150757A (en) * | 1995-08-08 | 2000-11-21 | U.S. Philips Corporation | Method of coating a luminescent material |
| JPH1121124A (ja) * | 1997-07-02 | 1999-01-26 | Shin Etsu Chem Co Ltd | イットリア/アルミナ混合微粒子及びその製造方法 |
| US7879258B2 (en) * | 2005-03-14 | 2011-02-01 | Koninklijke Philips Electronics N.V. | Phosphor in polycrystalline ceramic structure and a light-emitting element comprising same |
| CN100566490C (zh) * | 2005-03-14 | 2009-12-02 | 皇家飞利浦电子股份有限公司 | 多晶陶瓷结构中的磷光体和包括该磷光体的发光元件 |
| CN101370908B (zh) * | 2006-01-19 | 2012-04-18 | 宇部兴产株式会社 | 陶瓷复合体光转换构件和用其的发光装置 |
| CN1861738A (zh) * | 2006-06-09 | 2006-11-15 | 江西财经大学 | 一种碱土铝酸盐长余辉发光粉表面氧化铝致密膜层包覆方法 |
| DE102006054331A1 (de) * | 2006-11-17 | 2008-05-21 | Merck Patent Gmbh | Leuchtstoffkörper basierend auf plättchenförmigen Substraten |
| CN101560102B (zh) * | 2009-05-26 | 2012-02-22 | 上海大学 | C掺杂α-Al2O3透明陶瓷热释光和光释光材料的制备方法 |
| US8540173B2 (en) * | 2010-02-10 | 2013-09-24 | Imra America, Inc. | Production of fine particles of functional ceramic by using pulsed laser |
| US8324798B2 (en) * | 2010-03-19 | 2012-12-04 | Nitto Denko Corporation | Light emitting device using orange-red phosphor with co-dopants |
| CN103732354B (zh) * | 2011-07-08 | 2016-05-25 | 宇部兴产株式会社 | 光转换用陶瓷复合体的制造方法 |
| JP5842701B2 (ja) * | 2012-03-27 | 2016-01-13 | 信越化学工業株式会社 | 希土類元素が拡散された酸化物セラミック蛍光材料 |
| CN103367611B (zh) * | 2012-03-28 | 2017-08-08 | 日亚化学工业株式会社 | 波长变换用无机成型体及其制造方法以及发光装置 |
| JP6395701B2 (ja) * | 2012-03-29 | 2018-09-26 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung | 変換蛍光体および負の熱膨張係数を有する材料を含有する複合セラミック |
| JP2013227481A (ja) * | 2012-03-30 | 2013-11-07 | Covalent Materials Corp | セラミックス複合体 |
| CN102703056B (zh) * | 2012-05-09 | 2014-06-25 | 苏州英特华照明有限公司 | 一种复合包膜led荧光粉颗粒及其包膜方法 |
| JP6029962B2 (ja) * | 2012-12-11 | 2016-11-24 | 一般財団法人ファインセラミックスセンター | 構造物の歪・応力計測方法及び歪・応力センサ |
| CN103113097B (zh) * | 2013-01-20 | 2014-06-18 | 河北联合大学 | 一种铕、镝离子共掺杂的铝酸锶透明陶瓷的合成方法 |
| TWI601805B (zh) * | 2013-03-08 | 2017-10-11 | 宇部興產股份有限公司 | Process for producing nitride phosphors, silicon nitride phosphors for nitride phosphors, and nitride phosphors |
| KR101547734B1 (ko) * | 2013-03-19 | 2015-08-26 | 목포대학교산학협력단 | 폴리머 고착공정 및 알루미나 시드(seed)를 도입한 YAG:Ce3+ 형광체 분말의 제조방법 |
| CN104694124B (zh) * | 2013-12-10 | 2016-09-07 | 江南大学 | 氧化铝-稀土磷酸盐核-壳结构荧光材料及其制备方法 |
| CN103755345B (zh) * | 2014-01-02 | 2015-06-10 | 甘肃稀土新材料股份有限公司 | 一种小颗粒钇铈氧化物固溶体的制备方法 |
| MY177277A (en) * | 2014-03-03 | 2020-09-10 | Covalent Mat Corporation | Wavelength converting member |
| CN105314981A (zh) * | 2014-08-05 | 2016-02-10 | 北京化工大学 | 一种超重力技术制备氧化铝-氧化锆复合陶瓷粉体的方法 |
| JP2016204561A (ja) * | 2015-04-24 | 2016-12-08 | 太平洋セメント株式会社 | 蛍光部材、その製造方法および発光装置 |
| CN205539893U (zh) * | 2016-01-14 | 2016-08-31 | 深圳市光峰光电技术有限公司 | 一种波长转换装置、光源系统以及投影装置 |
| CN105753480B (zh) * | 2016-02-22 | 2019-02-26 | 厦门大学 | 一种发光陶瓷材料及其制备方法和应用 |
| CN105838351B (zh) * | 2016-04-21 | 2018-04-20 | 湖南农业大学 | 一种改善发光材料热稳定性的方法 |
| CN106631022B (zh) * | 2017-01-13 | 2020-03-24 | 中国计量大学 | 一种Tm敏化的氧化钇基激光陶瓷及其制备方法 |
| CN107384398A (zh) * | 2017-07-20 | 2017-11-24 | 中国科学院福建物质结构研究所 | 一种yag荧光粉及其制备方法和由其制备的yag荧光陶瓷 |
| US11584882B2 (en) | 2020-02-14 | 2023-02-21 | Osram Opto Semiconductors Gmbh | Wavelength converter; method of its making and light-emitting device incorporating the element |
-
2016
- 2016-12-09 CN CN201611135583.4A patent/CN108610023B/zh active Active
-
2017
- 2017-11-03 US US16/468,112 patent/US11267762B2/en active Active
- 2017-11-03 WO PCT/CN2017/109317 patent/WO2018103481A1/zh not_active Ceased
- 2017-11-03 EP EP17879386.5A patent/EP3553041B1/en active Active
-
2022
- 2022-01-12 US US17/647,810 patent/US11697621B2/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106206904A (zh) * | 2015-04-29 | 2016-12-07 | 深圳市光峰光电技术有限公司 | 一种波长转换装置、荧光色轮及发光装置 |
| CN105753457A (zh) * | 2016-02-02 | 2016-07-13 | 横店集团浙江英洛华电子有限公司 | 一种氧化铝荧光陶瓷材料及其制备方法和应用 |
| CN105906328A (zh) * | 2016-04-22 | 2016-08-31 | 横店集团浙江英洛华电子有限公司 | 一种氧化铝荧光陶瓷材料及其制备方法和应用 |
Non-Patent Citations (1)
| Title |
|---|
| See also references of EP3553041A4 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12371383B2 (en) | 2020-08-07 | 2025-07-29 | Nichia Corporation | Rare earth aluminate sintered compact and method for producing rare earth aluminate sintered compact |
| EP4328207A1 (en) * | 2022-08-24 | 2024-02-28 | Nichia Corporation | Sintered body and method for producing sintered body |
| CN115432957A (zh) * | 2022-08-30 | 2022-12-06 | 重庆大学 | 一种冷烧结制备ZnO-PTFE超疏水复合陶瓷的方法 |
| CN115432957B (zh) * | 2022-08-30 | 2023-09-08 | 重庆大学 | 一种冷烧结制备ZnO-PTFE超疏水复合陶瓷的方法 |
| CN118126717A (zh) * | 2024-01-26 | 2024-06-04 | 中国铁建投资集团有限公司 | 一种新型深红及近红外应力发光材料及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3553041B1 (en) | 2022-12-28 |
| US20220135487A1 (en) | 2022-05-05 |
| CN108610023B (zh) | 2021-07-23 |
| EP3553041A1 (en) | 2019-10-16 |
| US11697621B2 (en) | 2023-07-11 |
| US20200123063A1 (en) | 2020-04-23 |
| CN108610023A (zh) | 2018-10-02 |
| EP3553041A4 (en) | 2020-08-05 |
| US11267762B2 (en) | 2022-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2018103481A1 (zh) | 陶瓷复合材料的制备方法、陶瓷复合材料及波长转换器 | |
| He et al. | Red-shifted emission in Y3MgSiAl3O12: Ce3+ garnet phosphor for blue light-pumped white light-emitting diodes | |
| TWI534246B (zh) | Fluorescent particles and light-emitting diodes, and a lighting device using the same, and a backlight device for a liquid crystal panel | |
| WO2018045782A1 (zh) | 陶瓷复合材料的制备方法及陶瓷复合材料、光源装置 | |
| WO2017177924A1 (zh) | 一种氧化铝基质的荧光陶瓷的制备方法及相关荧光陶瓷 | |
| CN101760196B (zh) | 一种白光led用黄色荧光粉的合成方法 | |
| CN102627971A (zh) | 荧光体颗粒、制备方法及发光二极管 | |
| CN107474839A (zh) | 一种发光陶瓷 | |
| CN101905971B (zh) | 稀土离子掺杂钇铝石榴石激光陶瓷的制备方法 | |
| WO2019169868A1 (zh) | 荧光陶瓷及其制备方法 | |
| WO2021135883A1 (zh) | 荧光陶瓷的制备方法及荧光陶瓷 | |
| WO2018223544A1 (zh) | 一种发光陶瓷及其制备方法 | |
| CN102796493A (zh) | 一种球形单分散高铈抛光粉及其制备方法 | |
| CN100441658C (zh) | 钇铝石榴石荧光粉的制造方法 | |
| WO2018223632A1 (zh) | 单分散的核壳结构的荧光粉颗粒及其制备方法 | |
| US11097984B2 (en) | Composite ceramic and preparation method therefor | |
| Xinyu et al. | Photoluminescence enhancement of YAG: Ce3+ phosphor prepared by co-precipitation-rheological phase method | |
| CN106590657A (zh) | 一种镥铝酸盐绿色荧光粉及其制备方法和应用 | |
| WO2019200935A1 (zh) | 一种氮氧化铝基体的荧光陶瓷及其制备方法 | |
| WO2019179118A1 (zh) | 发光陶瓷及其制备方法 | |
| CN110590361B (zh) | 复合相荧光陶瓷及其制备方法、应用 | |
| CN103773362A (zh) | 偏硅酸钙发光材料及其制备方法 | |
| Lei et al. | Molten salt synthesis of color-tunable and single-component NaY (1− x− y)(WO4) 2: Eu3+ x, Tb3+ y phosphor for UV LEDs | |
| KR100419863B1 (ko) | 구상의 붕소산화물계 적색 형광체의 제조방법 | |
| CN109368682A (zh) | 一种超细铈氧硫复合物的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 17879386 Country of ref document: EP Kind code of ref document: A1 |
|
| NENP | Non-entry into the national phase |
Ref country code: DE |
|
| ENP | Entry into the national phase |
Ref document number: 2017879386 Country of ref document: EP Effective date: 20190709 |