CN107699236A - One kind mixes manganese (IV) potassium fluosilicate fluorescent material and preparation method thereof - Google Patents
One kind mixes manganese (IV) potassium fluosilicate fluorescent material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- -1 manganese (IV) potassium Chemical compound 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 68
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 61
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 61
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 61
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 61
- 239000000843 powder Substances 0.000 claims abstract description 36
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 31
- 239000011572 manganese Substances 0.000 claims abstract description 30
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 21
- 229910003638 H2SiF6 Inorganic materials 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 13
- 239000011591 potassium Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910020440 K2SiF6 Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 229910004074 SiF6 Inorganic materials 0.000 claims abstract description 3
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 32
- 239000011698 potassium fluoride Substances 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 20
- 235000003270 potassium fluoride Nutrition 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000013049 sediment Substances 0.000 claims description 11
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 10
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 4
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 150000003112 potassium compounds Chemical class 0.000 claims description 3
- 150000002697 manganese compounds Chemical class 0.000 claims description 2
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium peroxide Inorganic materials [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000003086 colorant Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 238000001035 drying Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/617—Silicates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The embodiment of the invention discloses one kind to mix manganese (IV) red fluorescence powder, mainly including potassium fluosilicate (K2SiF6) matrix and photolytic activity composition Mn (IV).Chemical formula is K2Si1‑x F6:xMn4+.The preparation method that one kind mixes manganese (IV) red fluorescence powder is also disclosed, is comprised the following steps：By chemical formula precise Si, K, F and Mn respective compound；Control mol ratio nKF/nSiO2,nH2O2/nSiO2,nHF/nSiO2,nKMnO4/nSiO2Respectively (0 0.3):1,(2‑12):1,(50‑200):1,(0.5‑3.5):1.First by SiO2Powder is dissolved in hydrofluoric acid, forms H2SiF6Solution；Then by KMnO4H is dissolved in KF2SiF6In solution；Again through hydrogen peroxide oxidation, filter and be dried to obtain and mix the potassium fluosilicate red fluorescence powder of manganese (IV) ion, technical problem to be solved of the embodiment of the present invention is to find the novel inorganic fluorescent material that can substitute doped rare earth element, rare earth element is substituted with relatively inexpensive metallic element, prepare relatively inexpensive inorganic fluorescent powder, and this fluorescent material can light with 465 nm of LED chip and be effectively matched, thus it can be used as three primary colours (red) fluorescent material of LED illuminating sources.
Description
Technical field
The present invention relates to fluorescent material field, more particularly to one kind to mix manganese (IV) red fluorescence powder and preparation method thereof.
Background technology
Inorganic red fluorescence powder is widely used on LED light source, kinescope, all kinds of colorful display screens.Traditional nothing
The red fluorescence powder of machine is the compound of doped rare earth element mostly, and the rare earth element of these incorporations triggers as photolytic activity center
Red fluorescence.This kind of rare earth element is mostly Eu (III) or Sm (III) etc..Because rare earth resources relatively lack general, price,
The highly desirable other inorganic red fluorescent material of research and development, such as inorganic red fluorescent material of non-terres rares.
The content of the invention
The technical problems to be solved by the invention are, there is provided a kind of cost is low, illumination effect is good mixes manganese (IV) red
Fluorescent material.
It is described to mix manganese (IV) red fluorescence powder, mainly including potassium fluosilicate (K2SiF6) matrix and photolytic activity composition Mn
(IV) ion.Chemical formula is K2Si1-x F6: xMn4+。
The photolytic activity composition Mn (IV) is to mix containing Mn (VII) or Mn (IV), Mn (II) compound.
It is described to mix containing Mn (VII) or Mn (IV), predominantly Mn (II) compound, potassium permanganate, manganese dioxide, acetic acid
One kind in manganese or manganese nitrate.
Present invention also offers a kind of simple to operate, production efficiency it is high mix the preparation method of manganese (IV) through color fluorescent material.
The preparation method for mixing manganese red fluorescence powder, comprises the following steps：
（1）By chemical formula precise Si, K, F and Mn respective compound；
（2）Si compound powders are dissolved in hydrofluoric acid, form H2SiF6Solution；
（3）Manganese compound and potassium compound are dissolved in H2SiF6K is formed in solution2SiF6Solution；
（4）Peroxide is added, K is formed through peroxidating or reduction2Si1-x F6: xMn4+Sediment；
（5）By above-mentioned sediment is filtered, ethanol is washed and is dried to obtain and mixes the potassium fluosilicate red fluorescence powder of manganese (IV) ion.
The step (1) is to the compound of manganese described in (4), predominantly potassium permanganate, manganese dioxide, manganese acetate or nitre
One kind in sour manganese, potassium compound are potassium fluoride, and peroxide is hydrogen peroxide.In the step (1), mol ratio nKF/
nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2 Respectively (0-0.3):1, (2-12):1, (50-200):1,
(0.5-3.5):1。
Implement the embodiment of the present invention, have the advantages that：
Technical problem to be solved of the embodiment of the present invention is to find that the inorganic fluorescent powder of doped rare earth element can be substituted, with relative
Cheap metallic element substitutes rare earth element, prepares relatively inexpensive inorganic fluorescent powder, and this fluorescent material can be with LED core
465 nm of piece are luminous to be effectively matched, thus can be used as three primary colours (red) fluorescent material of LED illuminating sources.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention will be made below further detailed
Description.
Embodiment 1：
By chemical formula precise Si, K, F and Mn respective compound；
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2 Respectively 0.2:1, 12:1, 100:
1, 2.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.2 mole of its dosage；
Hydrogen peroxide, 12 moles of its dosage；
Hydrofluoric acid, 100 moles of its dosage；
Potassium permanganate, 2.5 moles of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, reduction, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed by reduction2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Contrast: nKF/nSiO2Material rate is constant, but other three this respective changes（nH2O2/nSiO2, nHF/nSiO2,
nKMnO4/nSiO2）In the case of, and the experimental result in the case of manganese (IV) is not mixed.Manganese (IV) red fluorescence powder is mixed in synthesis
The data cases of (experiment numbers 1,2,3,4) are shown in Table 1.
Embodiment 2：
By chemical formula precise Si, K, F and Mn respective compound；
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2Respectively 0.1:1, 8:1, 200:1,
1.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.1 mole of its dosage；
Hydrogen peroxide, 8 moles of its dosage；
Hydrofluoric acid, 200 moles of its dosage；
Potassium permanganate, 1.5 moles of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, reduction, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed by reduction2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Contrast: nKF/nSiO2Material rate is constant, but other three this respective changes（nH2O2/nSiO2, nHF/nSiO2,
nKMnO4/nSiO2）In the case of, and the experimental result in the case of manganese (IV) is not mixed.Manganese (IV) red fluorescence powder is mixed in synthesis
The data cases of (experiment numbers 5,6,7,8) are shown in Table 1.
Embodiment 3：
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2Respectively 0.3:1, 4:1, 150:1,
3.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.3 mole of its dosage；
Hydrogen peroxide, 4 moles of its dosage；
Hydrofluoric acid, 150 moles of its dosage；
Potassium permanganate, 3.5 moles of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, oxidation, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed through peroxidating2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Contrast: nKF/nSiO2Material rate is constant, but other three this respective changes（nH2O2/nSiO2, nHF/nSiO2,
nKMnO4/nSiO2）In the case of, and the experimental result in the case of manganese (IV) is not mixed.Manganese (IV) red fluorescence powder is mixed in synthesis
The data cases of (experiment numbers 9,10,11,12) are shown in Table 1.
Embodiment 4：
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2Respectively 0:1, 2:1, 50:1,
0.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0 mole of its dosage；
Hydrogen peroxide, 2 moles of its dosage；
Hydrofluoric acid, 50 moles of its dosage；
Potassium permanganate, 0.5 mole of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, oxidation, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed through peroxidating2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Contrast: nKF/nSiO2Material rate is constant, but other three this respective changes（nH2O2/nSiO2, nHF/nSiO2,
nKMnO4/nSiO2）In the case of, and the experimental result in the case of manganese (IV) is not mixed.Manganese (IV) red fluorescence powder is mixed in synthesis
The data cases of (experiment numbers 13,14,15,16) are shown in Table 1.
Above-mentioned specific embodiment 1 is contained in different n into specific embodiment 4KF/nSiO2, nH2O2/nSiO2, nHF/
nSiO2, nKMnO4/nSiO2Experimental result under the conditions of (mol ratio), and have the results of comparison for not mixing Mn (IV) relatively.Synthesis
Mixing manganese (IV) red fluorescence powder molecular fluorescence spectroscopy instrument, determination sample excites and emission spectrum, compares luminous intensity respectively,
Appearance luster is observed, measurement result is shown in Table 1.
The comparing result of table 1 shows：The present invention's mixes manganese (IV) red fluorescence powder, is excellent non-to mix the red inorganic of rare earth
Fluorescent material, and this novel red inorganic fluorescent powder, the nm of excitation peak 458, it is sufficiently close to the blue-light-emitting of LED chip
465 nm, it therefore, can highly desirable be matched with the luminous of LED chip, be used as the three excellent bases of LED
Color (red) fluorescent material.Plus the relatively inexpensive of manganese, the market competitiveness of this fluorescent material can be bigger.
Embodiment 5：
By chemical formula precise Si, K, F and Mn respective compound；
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2 Respectively 0.2:1, 12:1, 100:
1, 2.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.2 mole of its dosage；
Hydrogen peroxide, 12 moles of its dosage；
Hydrofluoric acid, 100 moles of its dosage；
Manganese nitrate, 0.5 mole of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, oxidation, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed by reduction2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Embodiment 6：
By chemical formula precise Si, K, F and Mn respective compound；
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2 Respectively 0.2:1, 12:1, 100:
1, 2.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.2 mole of its dosage；
Hydrogen peroxide, 12 moles of its dosage；
Hydrofluoric acid, 100 moles of its dosage；
Manganese acetate, 2.5 moles of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, oxidation, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed by reduction2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
Embodiment 7：
By chemical formula precise Si, K, F and Mn respective compound；
Control mol ratio nKF/nSiO2, nH2O2/nSiO2, nHF/nSiO2, nKMnO4/nSiO2 Respectively 0.2:1, 12:1, 100:
1, 2.5:1, i.e.,:
Silica, 1 mole of its dosage;
Potassium fluoride, 0.2 mole of its dosage；
Hydrogen peroxide, 12 moles of its dosage；
Hydrofluoric acid, 100 moles of its dosage；
Manganese dioxide, 2.5 moles of its dosage；
In preparation process, including：The processes such as batch mixing, dissolving, oxidation, precipitation, filtering, washing, drying.First by silicon dioxide powder
End is dissolved in hydrofluoric acid, forms H2SiF6Solution, then potassium permanganate and potassium fluoride are dissolved in H2SiF6Formed in solution
K2SiF6Solution, finally hydrogen peroxide is added, K is formed by reduction2Si1-x F6: xMn4+Sediment, then filtered, second
Alcohol washs and is dried to obtain the potassium fluosilicate red fluorescence powder for mixing manganese (IV) ion.
The above disclosed power for being only a kind of preferred embodiment of the present invention, the present invention can not being limited with this certainly
Sharp scope, therefore the equivalent variations made according to the claims in the present invention, still belong to the scope that the present invention is covered.
Claims (5)
1. one kind mixes manganese (IV) red fluorescence powder, it is characterised in that mainly including potassium fluosilicate (K2SiF6) matrix and photolytic activity
Composition Mn (IV)；The chemical formula for mixing manganese (IV) red fluorescence powder is K2Si1-x F6: xMn4+。
2. according to claim 1 mix manganese (IV) red fluorescence powder, it is characterised in that the photolytic activity composition Mn (IV),
Contain Mn (VII) or Mn (IV), Mn (II) compound to mix.
3. according to claim 1 mix manganese (IV) red fluorescence powder, it is characterised in that described to mix containing Mn (VII) or Mn
(IV) one kind in, Mn (II) compound, predominantly potassium permanganate, manganese dioxide, manganese acetate or manganese nitrate.
4. the preparation method for mixing manganese (IV) red fluorescence powder according to any one of claim 1-3, it is characterised in that bag
Include following steps：
（1）By chemical formula precise Si, K, F and Mn respective compound；
（2）Si compound powders are dissolved in hydrofluoric acid, form H2SiF6Solution；
（3）Manganese compound and potassium compound are dissolved in H2SiF6K is formed in solution2SiF6Solution；
（4）Peroxide is added, K is formed through peroxidating2Si1-x F6: xMn4+Sediment；
（5）By above-mentioned sediment is filtered, ethanol is washed and is dried to obtain and mixes the potassium fluosilicate red fluorescence powder of manganese (IV) ion.
5. the preparation method according to claim 4 for mixing manganese (IV) red fluorescence powder, it is characterised in that the step (1)
To the compound of the manganese described in (4), predominantly one kind in potassium permanganate, manganese dioxide, manganese acetate or manganese nitrate, potassium
Compound is potassium fluoride, and peroxide is hydrogen peroxide；In the step (1), mol ratio nKF/nSiO2, nH2O2/nSiO2,
nHF/nSiO2, nKMnO4/nSiO2 Respectively (0-0.3):1, (2-12):1, (50-200):1, (0.5-3.5):1.
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| CN113097368A (en) * | 2021-03-26 | 2021-07-09 | 湖北三峡夷丰光电科技有限公司 | Production method of red fluorescent film |
| CN114621756A (en) * | 2022-03-28 | 2022-06-14 | 南昌大学 | Method for preparing Mn4+ activated fluoride red fluorescent powder by using recycled silicon sawdust powder |
| WO2023221551A1 (en) * | 2022-05-20 | 2023-11-23 | 中山大学 | Transition-metal-doped narrow-band luminescent gel material, and preparation method therefor and use thereof |
| CN115093849A (en) * | 2022-08-06 | 2022-09-23 | 烟台希尔德材料科技有限公司 | Preparation method of red fluorescent powder for high-brightness low-attenuation backlight |
| CN115093849B (en) * | 2022-08-06 | 2023-10-31 | 烟台希尔德材料科技有限公司 | Preparation method of red fluorescent powder for high-brightness low-attenuation backlight |
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