CN101591533A - A kind of red long afterglow luminous material and preparation method thereof - Google Patents
A kind of red long afterglow luminous material and preparation method thereof Download PDFInfo
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- CN101591533A CN101591533A CNA200910112064XA CN200910112064A CN101591533A CN 101591533 A CN101591533 A CN 101591533A CN A200910112064X A CNA200910112064X A CN A200910112064XA CN 200910112064 A CN200910112064 A CN 200910112064A CN 101591533 A CN101591533 A CN 101591533A
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 3
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000012153 distilled water Substances 0.000 claims description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 238000004364 calculation method Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 230000002688 persistence Effects 0.000 abstract description 10
- 239000002243 precursor Substances 0.000 abstract description 4
- 238000009841 combustion method Methods 0.000 abstract description 3
- 239000000941 radioactive substance Substances 0.000 abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000011572 manganese Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 10
- 239000011701 zinc Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 5
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003836 solid-state method Methods 0.000 description 2
- SCYYUUINVKYGRP-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[Zn+2].[Mn+2] Chemical compound P(=O)([O-])([O-])[O-].[Zn+2].[Mn+2] SCYYUUINVKYGRP-UHFFFAOYSA-K 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000904 thermoluminescence Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The present invention provides a kind of red long afterglow luminous material and preparation method thereof, and the chemical formula of described luminescent material is: (Zn
The 1-alpha-betaMn
αA
β)
3(P
1-0.8 γSi
γO
4)
2, wherein the chemical element represented of A is: one or more chemical elements among Ca, Sr, Mg, Eu, Dy, Zr, Pr, Y, Sm, Ce or the La, and α, β, γ represent the mole coefficient of each element; Described luminescent material adopts burning-calcining connection method for making to be prepared.Proportioning raw materials of the present invention is scientific and reasonable, adopt combustion method to prepare precursor, again in conjunction with high-temperature calcination, the luminescent properties of the product of preparation is significantly improved, and preparation time is shorter, and cost reduces, and the luminescent properties of material is better, through ultra violet lamp 15 minutes, in the dark can observe bright-coloured ruddiness after stopping to shine, range estimation was 9 hours time of persistence.Do not contain radioactive substance, have remarkable economic efficiency.
Description
Technical field
The invention belongs to the material technology field, more specifically relate to a kind of red long afterglow luminous material and preparation method thereof.
Background technology
Long-afterglow material has the significance of energy-conserving and environment-protective because of its widespread use in fields such as fire-fighting emergent, military installations, communications and transportation, architectural decoration and daily necessities obtains Materials science worker's attention.Aluminate long after glow luminous material is commercialization, and develops commodity such as luminous paint, light-emitting film, luminous printing ink, luminescent ceramic, luminescent plastics, luminescent fibre, luminescent paper.Red long afterglow luminous material research and development as one of three primary colours material comparatively lag behind, and it has purposes widely.Systems such as some red long afterglow luminous materials such as titanate, silicate, sulfide are all unsatisfactory at aspects such as time of persistence and chemical stabilities.The preparation method of the long after glow luminous material zinc phosphate of publication CN1228415C, need pass through during preparation at 200-500 ℃ of following pre-burning 2-6 hour, again in 500-1100 ℃ of following sintering 4-10 hour, consuming time longer, and the 4 hours only time of persistence of range estimation of preferred materials, especially the light that needs to absorb the ultraviolet region wave band could be luminous, thereby can't reach the commercialization application requiring.
Though the high temperature solid-state method batch mixing is simpler, but its calcining temperature is very high and calcination time is long, this be since each solid reactant can not fully contact with the level of molecule or atom and participate in the reaction, and unlike solution the solid matter velocity of diffusion very long response time is very long.And adopt the softening solution method of learning to overcome the above-mentioned shortcoming of high temperature solid-state method, each substance dissolves that participates in reaction in solution, make all reactants fully to contact with the level of molecule, pass through as co-precipitation again, form collosol and gel or directly carry out solution combustion to reach quick generation product, thereby shorten preparation cycle significantly, reduce production costs; Solution method also has advantages such as reaction good uniformity, can make doping and twinkler element can better enter into host lattice.
Summary of the invention
The purpose of this invention is to provide a kind of red long afterglow luminous material and preparation method thereof, proportioning raw materials is scientific and reasonable, adopt combustion method to prepare precursor, in conjunction with high-temperature calcination, the luminescent properties of the product of preparation is significantly improved again, preparation time is shorter, cost reduces, and the luminescent properties of material is better, does not contain radioactive substance, has remarkable economic efficiency.
Red long afterglow luminous material of the present invention: the chemical formula of described luminescent material is: (Zn
The 1-alpha-betaMn
αA
β)
3(P
1-0.8 γSi
γO
4)
2Wherein the chemical element represented of A is: one or more chemical elements among Ca, Sr, Mg, Eu, Dy, Zr, Pr, Y, Sm, Ce or the La, α, β, γ represent the mole coefficient of each element, and its value is respectively α=0.001-0.07, β=0.001-0.08, γ=0.003-0.2; Described luminescent material adopts burning-calcining connection method for making to be prepared.
Remarkable advantage of the present invention is: the present invention adopts combustion method to prepare precursor, can in 5-20 minute, generate product fast, but because reaction times short sawn timber crystal property is bad, the luminescent properties of material is relatively poor, through the calcining between high temperature, short time, the crystal property and the luminescent properties of material significantly improve the precursor product.Not only preparation time is shorter to compare the present invention with patent CN1228415C, and the luminescent properties of material is better, and the initial strength of material reaches 523mcd/m
2, still reach 8mcd/m after 2 hours
2, range estimation reaches 9 hours time of persistence.
Embodiment
Preparation process comprises the steps:
(1) elementary composition in the chemical formula according to described luminescent material, mole coefficient according to element, calculate the molar ratio of each element, and take by weighing oxide compound, nitrate, phosphoric acid salt, carbonate or the silicate of respective element and tetraethoxy according to this molar ratio;
(2) with material dissolution soluble in water in the described raw material in water, indissoluble or water-fast raw material mixed the back or add the nitric acid of certain volume concentration separately respectively and be heated to 75 ℃ it is dissolved fully, add distilled water diluting, then add fusing assistant and ignition dope, be made into settled solution; The nitric acid mass percent concentration is 60-98% in the described step (2), and its consumption is: according to the amount of Theoretical Calculation product, and each product of moles, the nitric acid of interpolation is 0.1-1L; The amount that adds distilled water in the described step (2) is: according to the amount of Theoretical Calculation product, and each product of moles, the distilled water of interpolation is 2-15L.
(3) with the settled solution of step (2) preparation in 500-900 ℃ of stove precombustion 5-20 minute, take out to grind and place High Temperature Furnaces Heating Apparatus again, under 800-1100 ℃, in reducing atmosphere, calcined 0.5-2 hour, take out behind the naturally cooling, obtain the red long afterglow luminous material product; Described fusing assistant is a boric acid, the 1-23% of the amount of the adding molar weight that to be described red long afterglow luminous material product go out according to Theoretical Calculation; Described ignition dope is a urea, and the 1-10 of the amount of the adding molar weight that to be described red long afterglow luminous material product go out according to Theoretical Calculation doubly; Reducing atmosphere in the described step (3) is CO or H
2Or N
2And H
2A kind of in the mixed gas.
The product performance measurement result: above-mentioned luminescent material product is carried out luminescent properties test through ultra violet lamp 15 minutes, in the dark can observe bright-coloured ruddiness after stopping to shine, original intensity is 523mcd/m
2, still reach 8mcd/m after 2 hours
2, range estimation was 9 hours time of persistence, and luminescent powder does not contain radioactive substance.
The silicon doping zinc phosphate manganese red look long after glow luminous material of the present invention's preparation, because preparation technology's difference can have two kinds of different thing phases, its X-ray diffraction data are consistent with 30-1490 or 30-1489 in the PDF standard card.The luminescence center of material is Mn
2+Ion, Mn
2+Replace the position of part Zn in the material of main part, be hexa-coordinate, an amount of Mn ion could guarantee that material has good luminescent properties.By introducing other suitable dopant ions, can improve the luminescent properties of material significantly and show that through the thermoluminescence experiment energy level trap depth of its relevant dopant material is more suitable.
Below be several specific embodiment of the present invention, but the present invention is not limited only to this.
Embodiment 1
(Zn
0.942Mn
0.05Mg
0.008)
3(P
0.996Si
0.005O
4)
2
Press chemical formula (Zn
0.942Mn
0.05Mg
0.008)
3(P
0.996Si
0.005O
4)
2Accurately take by weighing 2.862mol ZnO, 0.15mol MnCO
3, 0.024mol MgO, 1.992mol NH
4H
2PO
4, the 0.01mol tetraethoxy is the ZnO that weighs up, MnCO
3, to add 0.3 liter mass percent concentration be to be heated to 75 ℃ of stirrings in 85% nitric acid it is dissolved fully to MgO, adds 1 liter distilled water diluting wiring solution-forming 1, the NH that weighs up
4H
2PO
4Be dissolved in wiring solution-forming 2 in 1 liter the distilled water, tetraethoxy is added 0.1 liter the dehydrated alcohol back that is mixed add wiring solution-forming 3 in 1 liter the distilled water, solution 1, solution 2 and solution 3 are mixed urea that the back adds 0.02mol boric acid and 3mol stir and form settled solution.Settled solution is placed 650 ℃ of stoves, burnt 10 minutes, obtain the white powder of loose swollen shape, the cooling back is ground and is mixed, and places 1000 ℃ of High Temperature Furnaces Heating Apparatuss in CO reducing atmosphere sintering 45 minutes again, takes out and surveys its method optical property and XRD.
Through ultra violet lamp after 15 minutes, in the dark to observe and glow, range estimation time of persistence is 45 minutes, its X-ray diffraction data are consistent with the 30-1490 in the PDF standard card.
Embodiment 2
(Zn
0.9148Mn
0.08Eu
0.002Sm
0.005)
3(P
0.992Si
0.01O
4)
2
Press chemical formula (Zn
0.9148Mn
0.08Eu
0.002Sm
0.005)
3(P
0.992Si
0.01O
4)
2Accurately take by weighing 2.7444mol ZnO, 0.24molMnCO
3, 0.003mol Eu
2O
3, 0.0075mol Sm
2O
3, 1.984mol NH
4H
2PO
4, the 0.02mol tetraethoxy is the ZnO that weighs up, MnCO
3, Eu
2O
3, Sm
2O
3Adding 0.45 mass per liter percentage concentration is to be heated to 75 ℃ of stirrings in 70% nitric acid it is dissolved fully, adds 3 liters distilled water diluting wiring solution-forming 1, the NH that weighs up
4H
2PO
4Be dissolved in wiring solution-forming 2 in 1.2 liters the distilled water, tetraethoxy is added 0.15 liter the dehydrated alcohol back that is mixed add wiring solution-forming 3 in 1 liter the distilled water, solution 1, solution 2 and solution 3 are mixed urea that the back adds 0.04mol boric acid and 7mol stir and form settled solution.Settled solution is placed 600 ℃ of stoves, burnt 17 minutes, obtain the white powder of loose swollen shape, the cooling back is ground and is mixed, and places 950 ℃ of High Temperature Furnaces Heating Apparatuss in 5%H again
2+ 95%N
2Sintering is 1 hour in the reducing atmosphere, takes out and surveys its method optical property and XRD.
Through ultra violet lamp after 15 minutes, in the dark to observe and glow, range estimation time of persistence is 7 hours, its X-ray diffraction data are consistent with the 30-1490 in the PDF standard card.
Embodiment 3
Press chemical formula (Zn
0.946Mn
0.04Pr
0.004Sm
0.01)
3(P
0.988Si
0.015O
4)
2Accurately take by weighing 2.838mol ZnO, 0.12molMnCO
3, 0.006mol Pr
2O
3, 0.015mol Sm
2O
3, 1.976mol NH
4H
2PO
4, the 0.03mol tetraethoxy is the ZnO that weighs up, MnCO
3, Pr
2O
3, Sm
2O
3Adding 0.50 mass per liter percentage concentration is to be heated to 75 ℃ of stirrings in 60% nitric acid it is dissolved fully, adds 4 liters distilled water diluting wiring solution-forming 1, the NH that weighs up
4H
2PO
4Be dissolved in wiring solution-forming 2 in 2 liters the distilled water, tetraethoxy is added 0.2 liter the dehydrated alcohol back that is mixed add wiring solution-forming 3 in 2 liters the distilled water, solution 1, solution 2 and solution 3 are mixed urea that the back adds 0.03mol boric acid and 9mol stir and form settled solution.Settled solution is placed 800 ℃ of stoves, burnt 15 minutes, obtain the white powder of loose swollen shape, the cooling back is ground and is mixed, and places 1050 ℃ of High Temperature Furnaces Heating Apparatuss in 5%H again
2+ 95%N
2Sintering is 50 minutes in the reducing atmosphere, takes out and surveys its method optical property and XRD.
Through ultra violet lamp after 15 minutes, in the dark to observe and glow, range estimation time of persistence is 9 hours, its X-ray diffraction data are consistent with the 30-1490 in the PDF standard card.
Embodiment 4
Press chemical formula (Zn
0.92Mn
0.05Pr
0.01Sm
0.02)
3(P
0.984Si
0.02O
4)
2Accurately take by weighing 2.76mol ZnO, 0.15mol Mn (NO
3)
2, 0.015mol Pr
2O
3, 0.03mol Sm
2O
3, 1.968mol NH
4H
2PO
4, the 0.04mol tetraethoxy is the ZnO that weighs up, Pr
2O
3, Sm
2O
3The mass percent concentration that adds 0.3 liter is to be heated to 75 ℃ of stirrings in 98% nitric acid it is dissolved fully, adds 3 liters distilled water diluting wiring solution-forming 1, the NH that weighs up
4H
2PO
4And Mn (NO
3)
2Be dissolved in wiring solution-forming 2 in 3 liters the distilled water, tetraethoxy is added 0.2 liter the dehydrated alcohol back that is mixed add wiring solution-forming 3 in 3 liters the distilled water, solution 1, solution 2 and solution 3 are mixed urea that the back adds 0.2mol boric acid and 10mol stir and form settled solution.Settled solution is placed 800 ℃ of stoves, burnt 15 minutes, obtain the white powder of loose swollen shape, the cooling back is ground and is mixed, and places 1000 ℃ of High Temperature Furnaces Heating Apparatuss in CO reducing atmosphere sintering 1 hour 20 minutes again, takes out and surveys its method optical property and XRD.
Through ultra violet lamp after 15 minutes, in the dark to observe and glow, range estimation time of persistence is 9 hours, its X-ray diffraction data are consistent with the 30-1490 in the PDF standard card.
Embodiment 5
Press chemical formula (Zn
0.9Mn
0.07Eu
0.01Dy
0.08)
3(P
0.96Si
0.05O
4)
2Accurately take by weighing 2.7mol ZnO, 0.21mol Mn (NO
3)
2, 0.015mol Eu
2O
3, 0.04mol Dy
2O
3, 1.92mol NH
4H
2PO
4, the 0.1mol tetraethoxy is the ZnO that weighs up, Eu
2O
3, Dy
2O
3Adding 0.3 mass per liter percentage concentration is to be heated to 75 ℃ of stirrings in 80% nitric acid it is dissolved fully, adds 3.5 liters distilled water diluting wiring solution-forming 1, the NH that weighs up
4H
2PO
4And Mn (NO
3)
2Be dissolved in wiring solution-forming 2 in 4 liters the distilled water, tetraethoxy is added 0.25 liter the dehydrated alcohol back that is mixed add wiring solution-forming 3 in 3.5 liters the distilled water, solution 1, solution 2 and solution 3 are mixed urea that the back adds 0.3mol boric acid and 8mol stir and form settled solution.Settled solution is placed 800 ℃ of stoves, burnt 20 minutes, obtain the white powder of loose swollen shape, the cooling back is ground and is mixed, and places 900 ℃ of High Temperature Furnaces Heating Apparatuss in CO reducing atmosphere sintering 1 hour 40 minutes again, takes out and surveys its method optical property and XRD.
Through ultra violet lamp after 15 minutes, in the dark to observe and glow, range estimation time of persistence is 1 hour, its X-ray diffraction data are consistent with the 30-1490 in the PDF standard card.
Claims (7)
1. red long afterglow luminous material, it is characterized in that: the chemical formula of described luminescent material is: (Zn
The 1-alpha-betaMn
αA
β)
3(P
1-0.8 γSi
γO
4)
2Wherein the chemical element represented of A is: one or more chemical elements among Ca, Sr, Mg, Eu, Dy, Zr, Pr, Y, Sm, Ce or the La, α, β, γ represent the mole coefficient of each element, and its value is respectively α=0.001-0.07, β=0.001-0.08, γ=0.003-0.2.
2. the preparation method of a red long afterglow luminous material as claimed in claim 1 is characterized in that: adopt burning-calcining connection method for making to be prepared.
3. the preparation method of red long afterglow luminous material according to claim 2 is characterized in that: the preparation process of described employing burning-calcining connection method for making comprises the steps:
(1) elementary composition in the chemical formula according to described luminescent material, mole coefficient according to element, calculate the molar ratio of each element, and take by weighing oxide compound, nitrate, phosphoric acid salt, carbonate or the silicate of respective element and tetraethoxy according to this molar ratio;
(2) with material dissolution soluble in water in the described raw material in water, indissoluble or water-fast raw material mixed the back or add the nitric acid of certain volume concentration separately respectively and be heated to 75 ℃ it is dissolved fully, add distilled water diluting, then add fusing assistant and ignition dope, be made into settled solution;
(3) with the settled solution of step (2) preparation in 500-900 ℃ of stove precombustion 5-20 minute, take out to grind and place High Temperature Furnaces Heating Apparatus again, under 800-1100 ℃, in reducing atmosphere, calcined 0.5-2 hour, take out behind the naturally cooling, obtain the red long afterglow luminous material product.
4. the preparation method of red long afterglow luminous material according to claim 3, it is characterized in that: described fusing assistant is a boric acid, the 1-23% of the amount of the adding molar weight that to be described red long afterglow luminous material product go out according to Theoretical Calculation.
5. the preparation method of red long afterglow luminous material according to claim 3, it is characterized in that: described ignition dope is a urea, the 1-10 of the amount of the adding molar weight that to be described red long afterglow luminous material product go out according to Theoretical Calculation is doubly.
6. the preparation method of red long afterglow luminous material according to claim 3, it is characterized in that: the nitric acid mass percent concentration is 60-98% in the described step (2), consumption is: according to the amount of Theoretical Calculation product, and each product of moles, the nitric acid of interpolation is 0.1-1L; The amount that adds distilled water in the described step (2) is: according to the amount of Theoretical Calculation product, and each product of moles, the distilled water of interpolation is 2-15L.
7. the preparation method of red long afterglow luminous material according to claim 3, it is characterized in that: the reducing atmosphere in the described step (3) is CO or H
2Or N
2And H
2A kind of in the mixed gas.
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|---|---|---|---|
| CN200910112064.XA CN101591533B (en) | 2009-06-25 | 2009-06-25 | Red long afterglow luminescent material and preparation method thereof |
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|---|---|---|---|
| CN200910112064.XA CN101591533B (en) | 2009-06-25 | 2009-06-25 | Red long afterglow luminescent material and preparation method thereof |
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|---|---|
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| CN101591533B CN101591533B (en) | 2014-03-19 |
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| CN102329617A (en) * | 2010-07-14 | 2012-01-25 | 海洋王照明科技股份有限公司 | Phosphorous silicate fluorescent powder and preparation method thereof |
| CN103666468A (en) * | 2014-01-08 | 2014-03-26 | 轻工业部南京电光源材料科学研究所 | Purple light LED (Light-emitting Diode) excited broadband spectrum fluorescent powder and preparation method thereof |
| CN106010525A (en) * | 2016-06-03 | 2016-10-12 | 闽南师范大学 | Green long afterglow luminescent material and preparation method thereof |
| CN106010533A (en) * | 2016-06-03 | 2016-10-12 | 闽南师范大学 | Energy-storage red luminescent stone and preparation method thereof |
| CN107629790A (en) * | 2017-11-09 | 2018-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for LED blue light perovskite fluorescent material and products thereof and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1228415C (en) * | 2003-04-17 | 2005-11-23 | 中国科学院长春应用化学研究所 | Preparation method of long-afterglow luminescent material zine phosphate |
-
2009
- 2009-06-25 CN CN200910112064.XA patent/CN101591533B/en not_active Expired - Fee Related
Cited By (9)
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| CN101982521B (en) * | 2010-09-25 | 2013-04-17 | 西安理工大学 | Preparation method of phosphate luminescent material |
| CN103666468A (en) * | 2014-01-08 | 2014-03-26 | 轻工业部南京电光源材料科学研究所 | Purple light LED (Light-emitting Diode) excited broadband spectrum fluorescent powder and preparation method thereof |
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| CN106010533A (en) * | 2016-06-03 | 2016-10-12 | 闽南师范大学 | Energy-storage red luminescent stone and preparation method thereof |
| CN106010533B (en) * | 2016-06-03 | 2018-01-12 | 闽南师范大学 | A kind of accumulating type emitting red light stone and preparation method thereof |
| CN106010525B (en) * | 2016-06-03 | 2018-03-09 | 闽南师范大学 | A kind of green long afterglow luminescent material and preparation method thereof |
| CN107629790A (en) * | 2017-11-09 | 2018-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for LED blue light perovskite fluorescent material and products thereof and application |
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