CN105950137A - Mn<4+> doped fluoride red fluorescent powder, preparation method and application thereof - Google Patents
Mn<4+> doped fluoride red fluorescent powder, preparation method and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 18
- 229910000590 K2MnF6 Inorganic materials 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 14
- -1 difluoro potassium cyanide Chemical compound 0.000 claims abstract description 13
- 229910020440 K2SiF6 Inorganic materials 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VBKNTGMWIPUCRF-UHFFFAOYSA-M potassium;fluoride;hydrofluoride Chemical compound F.[F-].[K+] VBKNTGMWIPUCRF-UHFFFAOYSA-M 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910003638 H2SiF6 Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229960002163 hydrogen peroxide Drugs 0.000 claims 2
- 239000012467 final product Substances 0.000 claims 1
- ZEFWRWWINDLIIV-UHFFFAOYSA-N tetrafluorosilane;dihydrofluoride Chemical compound F.F.F[Si](F)(F)F ZEFWRWWINDLIIV-UHFFFAOYSA-N 0.000 claims 1
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 abstract 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 229910004074 SiF6 Inorganic materials 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910003564 SiAlON Inorganic materials 0.000 description 1
- VOMLAVHHAXSZJG-UHFFFAOYSA-N [Mn](=O)(=O)([O-])[O-].[K+].[F].[K+] Chemical compound [Mn](=O)(=O)([O-])[O-].[K+].[F].[K+] VOMLAVHHAXSZJG-UHFFFAOYSA-N 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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 invention discloses a Mn<4+> doped fluoride red fluorescent powder, a preparation method and application thereof. The Mn<4+> doped fluoride red fluorescent powder has a molecular formula of K2SiF6:xMn<4+>, wherein x is 0-0.15 excluding zero. The preparation method comprises the steps of: dissolving K2MnF6 powder in a hydrofluoric acid solution, then adding a difluoro potassium cyanide solution and a fluosilicic acid solution to carry out reaction, performing filtration and collecting the precipitate so as to obtain the Mn<4+> doped fluoride red fluorescent powder. The product prepared by a wet chemical coprecipitation method has good luminescent properties, use of monocrystalline silicon and other precious raw materials is avoided, the product cost is reduced, and the yield is high, thus being suitable for batch production. The red fluorescent powder provided by the invention has very uniform appearance, and has a very sharp emission peak, and is suitable for use as a backlight.
Description
Technical field
The present invention relates to a kind of Mn4+Fluoride red fluorescence powder of doping and preparation method and application, belongs to inorganic non-
Metal field of light emitting materials.
Background technology
At present, it is mainly with red fluorescence powder with nitrogen (oxygen) compound, germanate garnet system and tungsten/molybdate body
System is substrate, and its active ions are mainly Eu2+、Cr3+And Eu3+.Wherein the redness headed by nitrogen (oxygen) compound is glimmering
Light powder is because the stability of its brilliance enjoys favor and research.The nitrogen (oxygen) currently mainly having three kinds of comparative maturities is changed
Thing red fluorescence powder: M2Si5N8:Eu2+(M=Ca, Sr, Ba), CaAlSiN3:Eu2+With and M-SiAlON this
Three kinds they all there is the advantage such as resistance to oxidation, corrosion-resistant, heat stability is high, rub resistance.But nitrogen (oxygen) compound is red
Color fluorescent material also has many deficiencies.First being exactly that working condition is the most harsh, production cost is high；Secondly, nitrogen (oxygen)
Compound fluorescent material has from excitation spectrum wide for about 380nm to about 650nm, can cover whole blue-ray LED
Launch wavelength and the transmitting wavelength of major part YAG:Ce yellow fluorescent powder, blue light can not only be absorbed, and can also
Absorbing green-yellow light, i.e. its re-absorption phenomenon ratio more serious, therefore luminous for LED color can change, and total luminous flux is also
Can decline；Finally, the transmitting wavelength of the fluorescent material of this system is relatively wider, has most beyond human eye
Outside insensitive 650nm, reduce light efficiency.Therefore, in the urgent need to develop a kind of novel can be by blue light core
What sheet excited has wide absorption band and narrow transmitting band, and the use that can coordinate warm white LED that luminous efficiency is high
Red fluorescence powder.
Summary of the invention
It is an object of the invention to provide a kind of Mn4+Fluoride red fluorescence powder of doping and preparation method and application.This
Invention good luminous performance, reduces production cost, and yield is high.
The Mn that the present invention provides4+The fluoride red fluorescence powder of doping, its molecular formula is: K2SiF6: xMn4+, its
Middle x is the number between 0～0.15, and does not include zero.
In the present invention, molecular formula K2SiF6: xMn4+In, x concretely 0.06.
In the present invention, described Mn4+The K of doping2SiF6Red fluorescence powder is the fluorescent material of visible yellow color under natural light,
Under blue light or ultraviolet light, red color visible is luminous.
Present invention also offers the preparation method of described red fluorescence powder, comprise the steps: K2MnF6Powder body
Dissolve in a solution of hydrofluoric acid, add difluoro potassium cyanide and silicate fluoride solution reaction, precipitation is collected by filtration, i.e. obtains
Mn4+The fluoride red fluorescence powder of doping.
In above-mentioned preparation method, the temperature of described reaction can be-20～0 DEG C, concretely-10 DEG C；
The time of described reaction can be 2～6h, concretely 4h.
In above-mentioned preparation method, described K2MnF6Powder body, described difluoro potassium cyanide (KHF2) and described hexafluosilicic acid
Hexafluosilicic acid (H in solution2SiF6) mol ratio can be 1:0.35～0.92:0.65～1.23；
Described K2MnF6Powder body can be 1:50.5～70.3 with the mol ratio of Fluohydric acid. in described Fluohydric acid. (HF) solution；
The concentration of described silicate fluoride solution can be 30%～32%；
The concentration of described Fluohydric acid. (HF) solution can be 30～60%, concretely 49%, 45～50% or 40～55%.
In above-mentioned preparation method, described K2MnF6The preparation of powder body comprises the steps: potassium permanganate (KMnO4)
Solution, difluoro potassium cyanide solution, hydrogen peroxide (H2O2) solution and hydrofluoric acid solution hybrid reaction, it is heavy to be collected by filtration
Form sediment and i.e. obtain K2MnF6Powder body.
In the present invention, described K2MnF6The concrete reactional equation of the preparation of powder body is: 2KMnO4+2KHF2+8
HF+3H2O2→2K2MnF5+8H2O+3O2。
In above-mentioned preparation method, described K2MnF6The reaction temperature of the preparation of powder body can be 0～5 DEG C, concretely
5 DEG C, the response time can be 2～6h, concretely 4h or 3～5h；
The mol ratio of described potassium permanganate, described difluoro potassium cyanide, described Fluohydric acid. and described hydrogen peroxide is 2:2:8:3.
In above-mentioned preparation method, described filtration uses vacuum apparatus；
The step described precipitation cleaned successively, be dried also is included after described collection precipitation.
In above-mentioned preparation method, described precipitation uses alcohol washes；
Described wash number is 1～6 time, concretely 2 times；
The time of described cleaning is 1min～2h, concretely 2h；
Described precipitation is dried and carries out in an oven；
Described dry temperature can be 50～150 DEG C, concretely 90 DEG C；
The described dry time can be 2～8h, concretely 6h.
Mn of the present invention4+The fluoride red fluorescence powder of doping is applied to prepare in LED.
The invention have the advantages that
The present invention utilizes product good luminous performance prepared by wet-chemical coprecipitation, it is to avoid use monocrystal silicon etc. is valuable former
Material, reduces production cost, and yield is high, is suitable for batch production.Red fluorescence powder pattern of the present invention is visibly homogeneous,
There is the most sharp-pointed emission peak, it is adaptable to use as backlight.
Accompanying drawing explanation
Fig. 1 is K in the embodiment of the present invention 12SiF6:Mn4+Excitation-emission spectrogram.
Fig. 2 is K in the embodiment of the present invention 12SiF6:Mn4+Red fluorescence powder XRD material phase analysis.
Fig. 3 is K in the embodiment of the present invention 12SiF6:Mn4+Red fluorescence powder SEM shape appearance figure.
Fig. 4 is that (molecular formula is K to red fluorescence powder in the embodiment of the present invention 12SiF6:0.06Mn4+) knot of packaging and testing
Really, wherein Fig. 4 (a) is blue chip+K2SiF6:0.06Mn4+Fluorescent material, Fig. 4 (b) is blue chip
K2SiF6:0.06Mn4+Fluorescent material: Ce+K2SiF6:0.06Mn4+Fluorescent material.
Detailed description of the invention
Experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, the most commercially obtain.
Embodiment 1, doping Mn4+The K of ion2SiF6The preparation of red fluorescence powder
According to K to be prepared2MnF6In molecular formula, the mol ratio of different elements is by potassium permanganate (KMnO4), fluorine hydrogenation
Potassium (KHF2), hydrogen peroxide (H2O2) solution and Fluohydric acid. (HF) solution reacts according to 2:2:8:3, at 5 DEG C
At a temperature of react 4h, to prepare fluorine potassium manganate (K2MnF6) powder body.
The K that will have prepared2MnF6Powder body (0.05mol), is dissolved in HF solution (49wt.%, with 1000mL)
Middle 2h, during now solution is in the water-bath of-10 DEG C, adds KHF2(0.333mol)、H2SiF6Solution (30%～32%,
220mL) fully reacting 4h, the waste liquid in product is removed by vacuum apparatus, and the powder body obtained utilizes ethanol to enter
Row cleaning twice, cleans 2h, is then placed in 6h in 90 DEG C of baking ovens and dries, i.e. prepares K2SiF6:Mn4+Red fluorescence powder.
Fig. 1 is K in the embodiment of the present invention 12SiF6:Mn4+Excitation-emission spectrogram.It can be seen that abscissa is
The wavelength (nm) of spectrum, vertical coordinate is the relative intensity of spectrum, can be seen that inventive samples exists from exciting spectrogram
There is the strongest excitation peak at 450nm, go out the emission peak having comparison sharp-pointed at 632nm.
Fig. 2 is K in the embodiment of the present invention 12SiF6:Mn4+Red fluorescence powder XRD material phase analysis.That following is K2SiF6
Standard PDF card.As can be seen from the figure the phase of sample and K2SiF6Standard mutually the most identical.
Fig. 3 is K in the embodiment of the present invention 12SiF6:Mn4+Red fluorescence powder SEM shape appearance figure.From SEM figure permissible
Find out K of the present invention2SiF6:Mn4+The pattern of red fluorescence powder is visibly homogeneous, and size is between 10～15 μm.
Fig. 4 is that (molecular formula is K to red fluorescence powder in the embodiment of the present invention 12SiF6:0.06Mn4+) knot of packaging and testing
Really, wherein Fig. 4 (a) is blue chip+K2SiF6:0.06Mn4+Fluorescent material, Fig. 4 (b) be blue chip+
K2SiF6:0.06Mn4+Fluorescent material.From encapsulated result, can be seen that red fluorescence powder of the present invention has the most sharp-pointed sending out
Penetrate peak, it is adaptable to use as backlight, have a very important role to improving colour gamut.
Claims (9)
1. a Mn4+The fluoride red fluorescence powder of doping, its molecular formula is: K2SiF6: xMn4+, wherein x is
Number between 0～0.15, and do not include zero.
2. the preparation method of the red fluorescence powder described in claim 1, comprises the steps: K2MnF6Powder body is molten
Solution in a solution of hydrofluoric acid, adds difluoro potassium cyanide solution and silicate fluoride solution reaction, precipitation is collected by filtration, to obtain final product
To Mn4+The fluoride red fluorescence powder of doping.
Preparation method the most according to claim 2, it is characterised in that: the temperature of described reaction is-20～0 DEG C；
The time of described reaction is 2～6h.
4. according to the preparation method described in Claims 2 or 3, it is characterised in that: described K2MnF6Powder body, described
Difluoro potassium cyanide (KHF2) and described silicate fluoride solution in hexafluosilicic acid (H2SiF6) mol ratio can be 1:0.35～0.92:
0.65～1.23；
Described K2MnF6Powder body can be 1:50.5～70.3 with the mol ratio of Fluohydric acid. in described Fluohydric acid. (HF) solution；
The concentration of described silicate fluoride solution is 30%～32%；
The concentration of described Fluohydric acid. (HF) solution is 30～60%.
5. according to the preparation method according to any one of claim 2-4, it is characterised in that: described K2MnF6Powder body
Preparation comprise the steps: molten to potassium permanganate solution, difluoro potassium cyanide solution, hydrogenperoxide steam generator and Fluohydric acid.
Liquid hybrid reaction, is collected by filtration precipitation and i.e. obtains K2MnF6Powder body.
Preparation method the most according to claim 5, it is characterised in that: described K2MnF6The preparation of powder body anti-
Answering temperature is 0～5 DEG C, and the response time is 2～6h；
The mol ratio of described potassium permanganate, described difluoro potassium cyanide, described Fluohydric acid. and described hydrogen peroxide is 2:2:8:3.
7. according to the preparation method according to any one of claim 2-6, it is characterised in that: described filtration uses vacuum
Defecator；
The step described precipitation cleaned successively, be dried also is included after described collection precipitation.
Preparation method the most according to claim 7, it is characterised in that: described precipitation uses alcohol washes；
Described wash number is 1～6 time；
The time of described cleaning is 1min～2h；
Described precipitation is dried and carries out in an oven；
Described dry temperature is 50～150 DEG C；
The described dry time is 2～8h.
9. Mn described in claim 14+The application in preparation LED of the fluoride red fluorescence powder of doping.
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Cited By (5)
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| CN112573924A (en) * | 2020-12-14 | 2021-03-30 | 新沂市锡沂高新材料产业技术研究院有限公司 | Novel red fluorescent ceramic sheet and preparation method thereof |
| CN113355088A (en) * | 2021-04-30 | 2021-09-07 | 东南大学 | K2SiF6:Mn4+Preparation method of nano fluorescent powder |
| CN114479842A (en) * | 2022-03-16 | 2022-05-13 | 兰州大学 | Narrow-band red fluoride fluorescent powder synthesized by microwave assistance and preparation method thereof |
| 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 |
| CN116970394A (en) * | 2023-07-31 | 2023-10-31 | 四川师范大学 | Solid solution fluoride red fluorescent powder and preparation method and application thereof |
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| CN112573924A (en) * | 2020-12-14 | 2021-03-30 | 新沂市锡沂高新材料产业技术研究院有限公司 | Novel red fluorescent ceramic sheet and preparation method thereof |
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| CN113355088B (en) * | 2021-04-30 | 2022-04-12 | 东南大学 | K2SiF6:Mn4+Preparation method of nano fluorescent powder |
| CN114479842A (en) * | 2022-03-16 | 2022-05-13 | 兰州大学 | Narrow-band red fluoride fluorescent powder synthesized by microwave assistance and preparation method thereof |
| CN114479842B (en) * | 2022-03-16 | 2023-08-18 | 兰州大学 | Microwave-assisted synthesized narrow-band red fluoride fluorescent powder and preparation method thereof |
| 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 |
| CN116970394A (en) * | 2023-07-31 | 2023-10-31 | 四川师范大学 | Solid solution fluoride red fluorescent powder and preparation method and application thereof |
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Application publication date: 20160921 |