WO2014067113A1 - 硅酸盐发光材料及其制备方法 - Google Patents
硅酸盐发光材料及其制备方法 Download PDFInfo
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- WO2014067113A1 WO2014067113A1 PCT/CN2012/083880 CN2012083880W WO2014067113A1 WO 2014067113 A1 WO2014067113 A1 WO 2014067113A1 CN 2012083880 W CN2012083880 W CN 2012083880W WO 2014067113 A1 WO2014067113 A1 WO 2014067113A1
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- luminescent material
- silicate luminescent
- silicate
- mixture
- compound
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- 239000000463 material Substances 0.000 title claims abstract description 83
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 8
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 8
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 7
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 43
- 239000004964 aerogel Substances 0.000 claims description 35
- 150000001875 compounds Chemical class 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910002651 NO3 Inorganic materials 0.000 claims description 9
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 9
- 239000012266 salt solution Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 229910052744 lithium Inorganic materials 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims 2
- 239000011363 dried mixture Substances 0.000 claims 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 abstract description 8
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 4
- 229910052909 inorganic silicate Inorganic materials 0.000 abstract description 3
- 239000002923 metal particle Substances 0.000 abstract description 3
- 239000011575 calcium Substances 0.000 description 29
- 239000000843 powder Substances 0.000 description 14
- 239000010949 copper Substances 0.000 description 13
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 11
- 229910004283 SiO 4 Inorganic materials 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910021645 metal ion Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
- 239000010431 corundum Substances 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000010944 silver (metal) Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 125000000101 thioether group Chemical group 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- QXDMQSPYEZFLGF-UHFFFAOYSA-L calcium oxalate Chemical compound [Ca+2].[O-]C(=O)C([O-])=O QXDMQSPYEZFLGF-UHFFFAOYSA-L 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- FIMTUWGINXDGCK-UHFFFAOYSA-H dibismuth;oxalate Chemical compound [Bi+3].[Bi+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O FIMTUWGINXDGCK-UHFFFAOYSA-H 0.000 description 2
- 201000000490 flat ductal epithelial atypia Diseases 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 238000001748 luminescence spectrum Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- UWZVBPNIJCKCMC-UHFFFAOYSA-N terbium(iii,iv) oxide Chemical compound O=[Tb]O[Tb](=O)O[Tb](=O)O[Tb]=O UWZVBPNIJCKCMC-UHFFFAOYSA-N 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/87—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing platina group metals
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/87—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing platina group metals
- C09K11/873—Chalcogenides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/77492—Silicates
Definitions
- the invention relates to the technical field of luminescent materials, in particular to a silicate luminescent material and a preparation method thereof. Background technique
- the fluorescent materials used in current field emission devices are mainly those used in conventional cathode ray tubes and projection television tubes, oxide series and oxide series luminescent materials.
- the luminescence brightness is higher and has certain conductivity, but it is easily decomposed under the bombardment of large beam electron beams, releasing the elemental sulfur "poisoning" cathode tip, and generating other The precipitate covers the surface of the luminescent material, which reduces the luminous efficiency of the luminescent material and shortens the service life of the field emission device.
- the value of X ranges from 0.02 ⁇ x ⁇ 0.10.
- the value of y ranges from lx l0_ 5 ⁇ y 5 ⁇ 10_ 3 .
- the above silicate luminescent material effectively overcomes the structural defects of the titanate luminescent material by doping the metal particles, reduces the probability of non-radiative transition, and makes the luminous efficiency of the titanate luminescent material under the same excitation condition extremely great. Raise, the wavelength of the emitted light does not change.
- the silicate luminescent material has good stability, overcomes the defects of easy decomposition of sulfide and sulfur oxide series luminescent materials, and can be used in field emission devices instead of sulfide and sulfur oxide series luminescent materials.
- a method for preparing a silicate luminescent material comprising the steps of:
- a molar ratio of M to Si ratio y of the element is added to the airgel Si0 2 M salt solution, the mixture was stirred at 50 ⁇ 75 ° C were mixed solution hook, the mixed solution was sonicated, The sonicated solution is dried at 60 to 150 ° C, and the mixture obtained after drying is uniformly ground and calcined at 600 to 1200 ° C to obtain a Si 2 aerogel containing M ions, wherein
- the M is at least one of Ag, Au, Pt, Pd, and Cu metal nanoparticles, and the range of y is 0 ⁇ y ⁇ lxl (T 2 ; according to the molar ratio of Li, Ca, Tb, and Si elements
- For the ratio of 2: ( 1 -x) :x: 1 weigh out the Li compound, the Ca compound and the Tb compound, and the M 2 -containing SiO 2 aerogel, and grind and mix uniformly to obtain a mixture, wherein X is taken
- the value range is 0 ⁇
- the mixture is subjected to calcination treatment at 500 to 1000 ° C, and the mixture is placed in a reducing atmosphere at 800 to 1200 ° C for reduction treatment, and then the reduced mixture is cooled to room temperature. Grinding to obtain the silicate luminescent material having the chemical formula of Li 2 Ca 1 ⁇ c SiO 4 :Tb x ,M y , wherein Tb and M are doped in Li 2 Ca 1-x SiO 4 , and Tb and M are doped particles.
- the solute in the salt solution of M is at least one of HAuCl 4 , H 2 PtCl 6 , AgN 0 3 , PdCl 2 —2H 2 0 and Cu(N0 3 ) 2 , and the solvent is ethanol.
- the concentration of the M salt solution is 5x lO_ 6 ⁇ lx lO_ 2 mol / L.
- the Li compound is an oxide, a carbonate, a nitrate, or a vinegar of Li.
- the Tb compound is an oxide, a carbonate, a nitrate, an acetic acid of Tb Salt or oxalate.
- the reducing atmosphere is a CO reducing atmosphere or a H 2 reducing atmosphere or a mixed reducing atmosphere having a volume fraction of 95% N 2 and 5% 3 ⁇ 4.
- X has a value range of 0.02 ⁇ x ⁇ 0.10; y has a value range of lxl (T 5 ⁇ y 5xl (T 3 ) .
- the method for preparing the above silicate luminescent material firstly adsorbs metal ions by a SiO 2 aerogel to obtain a SiO 2 aerogel containing metal ions, and then, a compound of Li, Ca, and Tb, and Si0 containing a metal ion.
- 2 aerogel is used as raw material to reduce metal ions into metal element under reducing atmosphere, ie, silicate luminescent material with chemical formula of Li 2 Ca 1 ⁇ c Si0 4 :Tb x ,M y is prepared, preparation process tube Single, low cost, non-polluting, easy to control reaction, suitable for industrial production, the resulting silicate luminescent materials have high luminosity efficiency and good stability, and have broad application prospects in field emission devices.
- 1 is a flow chart showing a method of preparing a silicate luminescent material according to an embodiment
- FIG. 2 is a comparison diagram of luminescence light of a luminescent material prepared in Example 3 under a cathode ray excitation at a voltage of 1.5 kV, wherein curve 1 is a metal doped Li 2 Ca 9 oSi0 4 : Tb i o, Ag 2.
- the luminescence spectrum of the 5xl o-4 luminescent material, and the curve 2 is the luminescence spectrum of the undoped metal Li Cao. oSiO ⁇ Tbo.K) luminescent material.
- the silicate luminescent material of one embodiment has a chemical formula of Li 2 Ca 1 ⁇ c Si0 4 :Tb x ,M y .
- Tb and M are doped in Li 2 Ca 1-x SiO 4
- Tb and M are doped particles.
- M is at least one of Ag, Au, Pt, Pd, and Cu metal nanoparticles.
- the value of X ranges from 0 ⁇ x ⁇ 0.2.
- y is the molar ratio of M to Si elements.
- the value of y ranges from 0 ⁇ y ⁇ lxl (T 2 .
- the value range of X may also be 0.02 ⁇ x ⁇ 0.10, and the range of y may also be lxl (T 5 ⁇ y ⁇ 5xl (T 3 ) .
- the embodiment further provides a method for preparing a silicate luminescent material, as shown in FIG. 1, which includes the following steps:
- Step S110 adding a SiO 2 aerogel to the salt solution of M according to the ratio of molar ratio of M to Si, and mixing and stirring at 50-75 ° C to obtain a mixed solution, and then performing the mixed solution.
- the mixture is sonicated, and the mixed solution after sonication is dried at 60 to 150 ° C.
- the mixture obtained after drying is uniformly ground and calcined at 600 to 1200 ° C to obtain a Si 2 aerogel containing M ions.
- M is at least one of Ag, Au, Pt, Pd and Cu metal nanoparticles.
- the value of y ranges from 0 ⁇ y ⁇ lxl (T 2 .
- the solute in the salt solution of M is at least one of HAuCl 4 , H 2 PtCl 6 , AgN0 3 , PdCl 2 -2H 2 0 and Cu(N0 3 ) 2 . species, and the solvent is ethanol.
- the concentration range of the M salt solution is 5x 10- 6 ⁇ lx l0- 2 mol / L.
- Step S120 weighing the Li compound, the Ca compound and the Tb compound, and the SiO 2 aerogel containing the M ion according to a molar ratio of Li, Ca, Tb and Si elements of 2:(lx):x:l, grinding Mix well and obtain a mixture.
- the Li compound is an oxide, carbonate, nitrate, acetate or oxalate of Li.
- Ca compound An oxide, carbonate, nitrate, acetate or oxalate of Ca.
- the Tb compound is an oxide, carbonate, nitrate, acetate or oxalate of Tb.
- Step S130 the mixture is placed at 500 ⁇ 1000 °C for calcination treatment, and then the mixture is placed in a reducing atmosphere at 800 ⁇ 1200 °C for reduction treatment, and then the reduced mixture is cooled to room temperature. Grinding to obtain a silicate luminescent material having a chemical formula of Li 2 Ca 1 ⁇ c SiO 4 :Tb x ,My. Wherein Tb and M are doped in Li 2 Ca 1-x SiO 4 , and Tb and M are doped particles.
- the reducing atmosphere may be a CO reducing atmosphere or a H 2 reducing atmosphere or a mixed reducing atmosphere having a volume fraction of 95% N 2 and 5% 3 ⁇ 4.
- the silicate luminescent material effectively overcomes the structural defects of the titanate luminescent material by doping the metal particles, reduces the probability of non-radiative transition, and makes the luminous efficiency of the titanate luminescent material under the same excitation condition extremely great. Raise, the wavelength of the emitted light does not change.
- the silicate luminescent material has good stability, overcomes the defects of easy decomposition of sulfide and sulfur oxide series luminescent materials, and can replace the sulphide and sulfur oxide series luminescent materials in field emission devices.
- the method for preparing the silicate luminescent material firstly adsorbing metal ions by a SiO 2 aerogel, To a SiO 2 aerogel containing a metal ion, and then using a compound of Li, Ca, and Tb and a SiO 2 aerogel containing a metal ion as a raw material, reducing the metal ion to a metal element under a reducing atmosphere, that is, preparing A silicate luminescent material having a chemical formula of Li 2 Ca 1 ⁇ c SiO 4 :Tb x ,M y is obtained, and the preparation process is simple, low in cost, non-polluting, easy to control, and suitable for industrial production, and the obtained silicic acid Salt luminescent materials have high luminescence efficiency and good stability, and have broad application prospects in field emission devices.
- the test of the different compositions of the silicate luminescent materials, the preparation method thereof, and the properties thereof will be described below in conjunction with specific examples.
- composition of the silicate luminescent material of this embodiment is Li 2 Ca 85 Si0 4 : Tb i5 , Au lxl ( ) -2 , and the preparation process is as follows:
- the mixture prepared above is placed in an agate mortar and fully ground to a mixing hook; then the powder is transferred to a corundum crucible, heat treated at 500 ° C for 15 h in a muffle furnace; and then reduced in a tube furnace at a C atmosphere. after sintering at 1000 ° C 2h, Au 3+ is reduced to about to elemental Au; cooled to room temperature, the sample was ground into a powder, to obtain the Au-doped Li 2 Cao 85 Si0 4: Tbo 15,.. Au lxl o- 2 luminescent material.
- composition of the silicate luminescent material of this embodiment is , the preparation process is as follows:
- Si0 2 aerogels were dissolved in 6mL concentration of 5 ⁇ 10_ 3 mol / L chloroplatinic acid (H 2 PtCl 6) in ethanol and the resulting mixture was stirred for 3 h at 50 ° C, Then, it was sonicated for 10 min, and then dried at 60 ° C. The sample obtained after drying was uniformly ground and then calcined at 600 ° C for 4 h to obtain Pt 4+. Si0 2 aerogel.
- H 2 PtCl 6 chloroplatinic acid
- Li 2 CO 3 lithium carbonate
- CaCO 3 0.3924 g of 4 carbonic acid
- Tb 2 (C0 3 ) 3 cesium carbonate
- 0.2404 g of the above-prepared Si 2 2 containing Pt 4+ were weighed. Aerogel, preparation of the mixture.
- the mixture prepared above is placed in an agate mortar and fully ground to a mixing hook; then the powder is transferred to a corundum crucible, heat treated at 1000 ° C for 2 h in a muffle furnace; and then reduced in a CO furnace at a CO atmosphere. After sintering at 1200 ° C for 0.5 h, that is, Pt 4+ is reduced to Pt elemental; after cooling to room temperature, the obtained sample is ground into a powder to obtain P 2 -doped Li 2 Cao. 98 Si0 4 : Tbo. 2 , Pt 5xl () - 3 luminescent materials.
- the mixture prepared above was placed in an agate mortar and thoroughly ground to a homogenous hook; then the powder was transferred to a corundum crucible, heat treated at 600 ° C for 4 h in a muffle furnace; and 95% N in a tube furnace.
- 2 + 5% 3 ⁇ 4 (volume fraction) in a mixed reducing atmosphere is sintered at 1000 ° C for 4 h, that is, after Ag + is reduced to Ag element; after cooling to room temperature, the obtained sample is ground into a powder to obtain Ag-doped Li 2 Ca 0 . 90 SiO 4 : Tb 0 . 10 , Ag 2 . 5 ⁇ 10 ⁇ 4 luminescent material.
- the doped metal Ag prepared in this embodiment is the doped metal Ag prepared in this embodiment.
- composition of the silicate luminescent material of this embodiment is Li 2 Ca 8() SiO 4 : Tb 2 (), Pd lxl () - 5 , and the preparation process is as follows:
- the mixture prepared above is placed in an agate mortar and thoroughly ground to a homogenous hook; then the powder is transferred to a corundum crucible, heat treated at 700 ° C for 5 h in a muffle furnace; and in a tubular furnace at H 2 Sintering at 800 ° C for 6 h in a reducing atmosphere, that is, Pd 4+ is reduced to Pd elemental; after cooling to room temperature, the obtained sample is ground into a powder to obtain Pd -doped Li 2 Cao. 8 oSi0 4 : Tbo. 2 o, Pd lxl o- 5 luminescent material.
- composition of the silicate luminescent material of this embodiment is Li 2 Ca 95 Si0 4 : Tb () 5 , Cu lxl (H , the preparation process is as follows:
- Si0 2 aerogel 0.3606 g of Si0 2 aerogel was weighed and dissolved in 12 mL of a solution of copper nitrate (Cu(N0 3 ) 2 ) having a concentration of 5 ⁇ 10_ 5 mol/L, and the obtained mixed solution was stirred at 70 ° C for 1 h. Then, it was ultrasonicated for 10 min, and then dried at 70 ° C. The sample obtained after drying was ground and hooked, and calcined at 800 ° C for 2 h to obtain a SiO 2 aerogel containing Cu 2+ .
- Cu(N0 3 ) 2 copper nitrate
- composition of the silicate luminescent material of this embodiment is Li 2 Ca 88 Si0 4 : Tb i2 , Ag 5 xl () -4 , and the preparation process is as follows:
- the mixture prepared above is placed in an agate mortar and fully ground to a homogenous hook; then the powder is transferred to a corundum crucible, heat treated at 500 ° C for 10 h in a muffle furnace; and then in a tubular furnace at H 2 After sintering at 1100 ° C for 3 h in a reducing atmosphere, the Ag + is reduced to Ag element; after cooling to room temperature, the obtained sample is ground into a powder to obtain Ag-doped Li 2 Ca 88 Si0 4 : Tb i2 , Ag 5 xl () -4 luminescent material.
- composition of the silicate luminescent material of this embodiment is Li Cao ⁇ SiO ⁇ Tbo.os Ago.s/Auo. ⁇ . xK ⁇ , and the preparation process is as follows:
- the mixture prepared above was placed in an agate mortar and thoroughly ground to a homogenous hook; then the powder was transferred to a corundum crucible, heat treated at 700 ° C for 8 h in a muffle furnace; and 95% N in a tube furnace.
- the obtained sample is ground into a powder to obtain I ⁇ Cao ⁇ SiO ⁇ Tbo.os Ago.s/Auo. ⁇ xK luminescent material doped with Ag and Au .
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Abstract
Description
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP12887525.9A EP2915863B1 (en) | 2012-10-31 | 2012-10-31 | Silicate luminescent material and preparation method therefor |
CN201280076460.1A CN104736666A (zh) | 2012-10-31 | 2012-10-31 | 硅酸盐发光材料及其制备方法 |
PCT/CN2012/083880 WO2014067113A1 (zh) | 2012-10-31 | 2012-10-31 | 硅酸盐发光材料及其制备方法 |
JP2015538247A JP5965551B2 (ja) | 2012-10-31 | 2012-10-31 | ケイ酸塩発光材料及びその製造方法 |
US14/438,450 US20150284631A1 (en) | 2012-10-31 | 2012-10-31 | Silicate luminescent material and preparation method therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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PCT/CN2012/083880 WO2014067113A1 (zh) | 2012-10-31 | 2012-10-31 | 硅酸盐发光材料及其制备方法 |
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US (1) | US20150284631A1 (zh) |
EP (1) | EP2915863B1 (zh) |
JP (1) | JP5965551B2 (zh) |
CN (1) | CN104736666A (zh) |
WO (1) | WO2014067113A1 (zh) |
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US20150275083A1 (en) * | 2012-10-31 | 2015-10-01 | Ocean's King Lighting Science & Technology Co., Ltd | Silicate luminescent material and preparation method therefor |
CN110452690A (zh) * | 2019-08-24 | 2019-11-15 | 宝艺新材料股份有限公司 | 一种用于纸板表面的防伪发光材料的制备方法 |
CN112408837A (zh) * | 2020-11-23 | 2021-02-26 | 保利长大工程有限公司 | 一种基于花岗岩石粉的复合矿物掺合料及其制备方法 |
CN112408836A (zh) * | 2020-11-23 | 2021-02-26 | 贵州四方联达科技有限公司 | 一种复合矿物掺合料及其制备方法 |
CN116376538B (zh) * | 2023-05-11 | 2024-04-19 | 广西师范大学 | 一种掺杂混合价态Eu离子的无机非光致变色荧光可调材料及其制备方法 |
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JP2006232906A (ja) * | 2005-02-23 | 2006-09-07 | Sumitomo Chemical Co Ltd | 蛍光体およびそれを用いた発光装置 |
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CN101760195B (zh) * | 2010-01-22 | 2013-05-08 | 海洋王照明科技股份有限公司 | 硅酸盐蓝色发光材料及其制备方法 |
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- 2012-10-31 JP JP2015538247A patent/JP5965551B2/ja active Active
- 2012-10-31 CN CN201280076460.1A patent/CN104736666A/zh active Pending
- 2012-10-31 US US14/438,450 patent/US20150284631A1/en not_active Abandoned
- 2012-10-31 EP EP12887525.9A patent/EP2915863B1/en active Active
- 2012-10-31 WO PCT/CN2012/083880 patent/WO2014067113A1/zh active Application Filing
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JP5965551B2 (ja) | 2016-08-10 |
US20150284631A1 (en) | 2015-10-08 |
EP2915863A1 (en) | 2015-09-09 |
JP2015532938A (ja) | 2015-11-16 |
EP2915863A4 (en) | 2016-06-08 |
EP2915863B1 (en) | 2019-11-06 |
CN104736666A (zh) | 2015-06-24 |
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