CN108728082B - Blue light excited fluoromanganate red light material and preparation method and application thereof - Google Patents
Blue light excited fluoromanganate red light material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000000975 co-precipitation Methods 0.000 claims abstract description 5
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000590 K2MnF6 Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- DSFLPAXQDSLSKU-UHFFFAOYSA-L [Mn](=O)(=O)(O)O.[F] Chemical compound [Mn](=O)(=O)(O)O.[F] DSFLPAXQDSLSKU-UHFFFAOYSA-L 0.000 abstract description 9
- 238000005286 illumination Methods 0.000 abstract description 4
- 229910052792 caesium Inorganic materials 0.000 abstract description 3
- 229910052700 potassium Inorganic materials 0.000 abstract description 3
- 238000009877 rendering Methods 0.000 abstract description 3
- 229910052701 rubidium Inorganic materials 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 229910003202 NH4 Inorganic materials 0.000 abstract description 2
- 239000003112 inhibitor Substances 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- 238000000695 excitation spectrum Methods 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XPIIDKFHGDPTIY-UHFFFAOYSA-N F.F.F.P Chemical compound F.F.F.P XPIIDKFHGDPTIY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000002284 excitation--emission spectrum Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 229910003564 SiAlON Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- 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
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
The invention belongs to the field of luminescent materials, and discloses a blue light excited fluoromanganate red-light material, and a preparation method and application thereof. The chemical formula of the blue light excited fluorine manganate red light material is A2MnF6Wherein A is Li, Na, K, Rb, Cs, NH4Any one or a combination of two or more of them. The preparation method comprises the following steps: AHF (hydrogen peroxide inhibitor)2Dissolving in hydrofluoric acid solution, and adding KMnO4Stirring and dissolving uniformly, then dripping hydrogen peroxide solution to carry out coprecipitation reaction, filtering and collecting precipitate, washing and drying to obtain A2MnF6A red light material. The fluorine manganate red light material has good luminous performance, can effectively improve the light color performance of a white light LED, reduce the color temperature and improve the color rendering index, and can be applied to the fields of white light LED illumination and backlight source display.
Description
Technical Field
The invention belongs to the field of luminescent materials, and particularly relates to a blue light excited fluoromanganate red-light material, and a preparation method and application thereof.
Background
Compared with the traditional incandescent lamp and fluorescent lamp which are used as illumination light sources, the white light LED has the outstanding advantages of low heat productivity, low power consumption, quick response, no stroboflash, long service life and the like, and is known as a new generation of solid-state illumination light source. The current mainstream commercial white light LED consists of a blue light chip and yellow fluorescent powder Y3Al5O12:Ce3+(YAG:Ce3+) The white light LED has a lack of red light component in the emission spectrum, resulting in a high color temperature (CCT) of the light source>4000K) Lower color rendering index (CRI, Ra)<80) It is difficult to satisfy the indoor lighting requirements. The mainstream commercial backlight white light LED is formed by combining, packaging and synthesizing a blue light chip and SiAlON, and has strong demand on narrow-band red light materials, so that the requirement of a wide color gamut Liquid Crystal Display (LCD) backlight can be met.
In order to improve the light color performance of the white light LED, a proper amount of red light luminescent material needs to be added into the device. Mn4+The doped fluoride red light material can be effectively excited by 300-400 nm near ultraviolet light and 400-500 nm blue light, and a narrow-band red light emission peak located in a naked eye sensitive area is arranged in the range of 610-650 nm. The strongest absorption peak is matched with the emission peak (450 nm) of the blue LED chip, and the red light emitting material is an ideal red light emitting material for the white light LED. Such fluoride red phosphors have been reported, mainly comprising A2MF6:Mn4+、BMF6:Mn4+ 3NF6:Mn4+LnF4:Mn4+(A：Li、Na、K、Rb、Cs、NH4(ii) a B: be. Mg, Ca, Sr, Ba, Zn; m is Si, Ge, Sn, Ti, Zr, Hf; n is Al, Ga, In; ln is a trivalent rare earth ion), most of which have high luminous efficiency and can be applied to white light LEDs (fluoride phosphor materials and semiconductor light emitting devices thereof, CN 102827601 a; preparation method of fluoride phosphor material, CN 103980896 a). The red light materials mentioned above are all doped with other light-emitting active ions, the experimental process is relatively complex, the number of steps is large, and in addition, the defect of the materials can be improved inevitably by doping. At present, the novel luminescent materials with high luminous efficiency are still deficient, so that the development of novel, rapidly synthesized and fluoride red light materials without doping is of great practical significance.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a blue light excited fluorine manganate red light material.
The invention also aims to provide a preparation method of the blue light excited fluoromanganate red light material.
The invention further aims to provide application of the blue light excited fluorine manganate red light material in white light LED devices or backlight source display.
The purpose of the invention is realized by the following technical scheme:
a blue light excited fluorine manganate red light material has a chemical formula of A2MnF6Wherein A is Li, Na, K, Rb, Cs, NH4Any one or a combination of two or more of them.
Further, the blue light excited fluorine manganate red light material generates red light with the strongest emission peak at the wavelength of 620-640 nm under the excitation of light with the wavelengths of 300-400 nm and 400-500 nm.
The preparation method of the blue light excited fluoromanganate red light material comprises the following preparation steps:
AHF (hydrogen peroxide inhibitor)2Dissolving in hydrofluoric acid solution, and adding KMnO4Stirring and dissolving uniformly, then dripping hydrogen peroxide solution to carry out coprecipitation reaction, filtering and collecting precipitate, washing and drying to obtain A2MnF6A red light material.
Further, the mass fraction of the hydrofluoric acid solution is 49%, and the mass fraction of the hydrogen peroxide solution is 30%.
Further, the washing refers to washing with acetone, and the drying refers to drying at a temperature of 80 ℃ for 2 h.
Further, A is2MnF6Adding red light material into hydrofluoric acid solution, adding another fluoride A for ion exchange reaction, filtering, washing and drying the product to obtain different A2MnF6A red light material.
The blue light excited fluorine manganate red light material is applied to a white light LED device or a backlight source.
The material and the preparation method of the invention have the following advantages and beneficial effects:
(1) the fluorine manganate red light material has good luminous performance, and can effectively improve the light color performance of a white light LED.
(2) The fluorine manganate red light material is a powder material, is easy to be mixed with other fluorescent materials and dispersed in epoxy resin or silica gel, and can be widely and commercially applied to the fields of white light LED illumination and backlight source display.
(3) The preparation method comprises a coprecipitation method and an ion exchange method, has simple and easy preparation process, one-step completion, mild conditions and low cost, and can realize large-scale industrial production.
Drawings
FIG. 1 shows K prepared in example 12MnF6XRD diffractogram of red material.
FIG. 2 shows K prepared in example 12MnF6Room temperature excitation spectrum and emission spectrum of red light material.
FIG. 3 shows Cs prepared in example 22MnF6XRD diffractogram of red material.
FIG. 4 shows Cs prepared in example 22MnF6Room temperature excitation spectrum and emission spectrum of red light material.
FIG. 5 shows Cs prepared in example 22MnF6The red light material is used for packaging photoluminescence spectrograms of the white light LED device.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
Example K2MnF6The red light material is prepared by a coprecipitation method, and the preparation steps are as follows:
10g KHF was weighed out2Dissolving in 50ml 49% hydrofluoric acid solution, adding 1g KMnO4Stirring until the solid is completely dissolved, gradually dropwise adding 30% hydrogen peroxide solution until the solution is changed from purple to yellow, immediately stopping dropwise adding, filtering, collecting precipitate sample, washing with acetone for 3 times, drying at 80 deg.C for 2 hr to obtain K2MnF6A red light material.
K obtained in this example2MnF6The XRD diffraction pattern of the red light material is shown in figure 1, and the diffraction peak of the sample is shown in figure 1 to be matched with the standard card JCPDS 77-2133 (K)2MnF6) And (3) consistent, no hetero-phase diffraction peak appears, and the synthesized red light material sample is a pure phase.
K obtained in this example2MnF6The room temperature excitation spectrum and the emission spectrum of the red light material are shown in FIG. 2, and it can be seen from FIG. 2 that the sample has strong broadband excitation peaks in the ultraviolet region (320 nm-390 nm) and the blue region (400 nm-500 nm), and has a light spectrum at 460nmUnder excitation, a strong narrow-band red light emission peak is positioned in a wave band range of 575-675 nm.
Example 2
This example Cs2MnF6The red light material is prepared by an ion exchange method, and the preparation method comprises the following specific steps:
weighing 2.46g K2MnF6Adding into 10ml of 40% hydrofluoric acid solution, adding 6.06g of CsF for reaction for 30 minutes, filtering, washing and drying the obtained sample to obtain Cs2MnF6A red light material.
Cs obtained in this example2MnF6The XRD diffraction pattern of the red light material is shown in FIG. 3. from FIG. 3, the diffraction peak of the sample is shown to be similar to that of JCPDS 77-1301 (Cs) of standard card2MnF6) And (3) consistent, no hetero-phase diffraction peak appears, and the synthesized red light material sample is a pure phase.
Cs obtained in this example2MnF6The room temperature excitation spectrum and the emission spectrogram of the red light material are shown in fig. 4, and as can be seen from fig. 4, a sample has stronger broadband excitation peaks in an ultraviolet region (320 nm-390 nm) and a blue region (400 nm-500 nm), and has stronger narrow-band red light emission peaks in a wavelength range of 575-675 nm under the excitation of 465nm light.
Cs obtained in this example2MnF6The photoluminescence spectrogram of the white light LED device which is formed by combining and packaging the red light material, the blue light LED chip and the green fluorescent powder beta-SiALON is shown in figure 5, and warm white light with the color temperature of 3390K and the color rendering index of 78.3 is obtained.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (4)
1. Blue light-excited fluoromanganate red-light material Cs2MnF6The preparation method is characterized by comprising the following steps: will K2MnF6Addition of Red-emitting materials to hydrofluoric acidAdding CsF into acid solution for ion exchange reaction, filtering, washing and drying the product to obtain Cs2MnF6A red light material.
2. The blue-excited fluoromanganate red-light material Cs according to claim 12MnF6The preparation method is characterized by comprising the following steps: said K2MnF6The red light material is prepared by the following method:
mixing KHF2Dissolving in hydrofluoric acid solution, and adding KMnO4Stirring and dissolving uniformly, then dripping hydrogen peroxide solution for coprecipitation reaction, filtering and collecting precipitate, washing and drying to obtain K2MnF6A red light material.
3. The blue-excited fluoromanganate red-light material Cs according to claim 22MnF6The preparation method is characterized by comprising the following steps: the mass fraction of the hydrofluoric acid solution is 49%, and the mass fraction of the hydrogen peroxide solution is 30%.
4. The blue-excited fluoromanganate red-light material Cs according to claim 22MnF6The preparation method is characterized by comprising the following steps: the washing refers to washing with acetone, and the drying refers to drying at the temperature of 80 ℃ for 2 hours.
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| CN109920352B (en) * | 2019-03-18 | 2021-03-19 | 龙港市三星交通标牌有限公司 | Warm white light sign convenient to change |
| CN110157414B (en) * | 2019-05-13 | 2023-01-24 | 江西理工大学 | Red fluoromanganate fluorescent material and preparation method thereof |
| CN114958350B (en) * | 2022-05-25 | 2023-08-18 | 华南理工大学 | Fluoromanganate red fluorescent material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980896A (en) * | 2014-04-29 | 2014-08-13 | 中国科学院福建物质结构研究所 | Preparation method of fluoride fluorescent powder material |
| CN104789214A (en) * | 2015-04-01 | 2015-07-22 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method for red fluorescent powder for LED |
| CN105462582A (en) * | 2015-12-16 | 2016-04-06 | 华南理工大学 | Mn<4+> doping red fluorescent material for white light LED and preparation method of Mn<4+> doping red fluorescent material |
| CN105950143A (en) * | 2016-05-24 | 2016-09-21 | 张书生 | Red phosphor, preparation method thereof and light emitting device using red phosphor |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980896A (en) * | 2014-04-29 | 2014-08-13 | 中国科学院福建物质结构研究所 | Preparation method of fluoride fluorescent powder material |
| CN104789214A (en) * | 2015-04-01 | 2015-07-22 | 苏州工业园区晶冠瓷材料科技有限公司 | Preparation method for red fluorescent powder for LED |
| CN105462582A (en) * | 2015-12-16 | 2016-04-06 | 华南理工大学 | Mn<4+> doping red fluorescent material for white light LED and preparation method of Mn<4+> doping red fluorescent material |
| CN105950143A (en) * | 2016-05-24 | 2016-09-21 | 张书生 | Red phosphor, preparation method thereof and light emitting device using red phosphor |
Non-Patent Citations (1)
| Title |
|---|
| Red and Deep Red Emissions from Cubic K2SiF6:Mn4+ and Hexagonal K2MnF6 Synthesized in HF/KMnO4/KHF2/Si Solutions;Ryota Kasa, Sadao Adachi;《Journal of The Electrochemical Society》;20120118;第159卷(第4期);J89-J95 * |
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