CN109179481B - Quadrivalent manganese ion doped barium fluoscandate red light-emitting material and preparation method thereof - Google Patents
Quadrivalent manganese ion doped barium fluoscandate red light-emitting material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a tetravalent manganese ion doped barium fluoscandate red light material and a preparation method thereof. The material is doped with Ba3Sc2F12As a matrix, with Mn4+As an activator, the chemical composition is Ba3Sc2F12:Mn4+. The preparation method comprises the following steps: with Sc2O3As a source of scandium, with Ba (NO)3)2As a barium source, with K2MnF6In order to activate the ionic manganese source, aqueous HF solution is used as a medium and a fluorinating agent. During the preparation, Sc2O3Placing the solid in a container, and adding HF aqueous solution and Ba (NO) respectively3)2And K2MnF6And reacting for 1-12 hours at normal temperature to 180 ℃, filtering, and naturally airing to obtain the product. The material can be applied to white light LEDs with two primary colors so as to improve the color rendering index of the white light LEDs. The product does not contain rare earth, the preparation method is simple, high-temperature sintering is not needed, and the method is suitable for industrial production.
Description
Technical Field
The invention relates to a luminescent material, in particular to a red light material which can be used for a white light LED; in particular to a quadrivalent manganese ion doped barium fluoscandate luminescent material with an excitation wavelength in a blue light region and an emission wavelength in a red light region and a preparation method thereof.
Background
Compared with the traditional light source, the semiconductor white light LED is increasingly favored by people due to excellent characteristics such as energy conservation, adjustable light, vibration resistance, difficult damage, instant start, no flash frequency, long service life and the like. The dominant white light LED product in the market is a yellow-blue dichromatic white light LED formed by packaging yellow fluorescent powder YAG: Ce and a blue light LED, in the LED structure, electroluminescent blue light (450-470 nm) of a GaN chip excites the fluorescent powder YAG: Ce to generate yellow light of 550nm, and the electroluminescent blue light of the chip and the yellow light of the fluorescent powder are complemented into white light. Because the spectrum of the white light LED is lack of red light components, the color temperature of the white light LED is higher, white light with low color temperature (2700-3000K) cannot be obtained, the color rendering index is lower, warm white light with high color rendering (Ra >90) cannot be obtained, namely, the color reduction capability is poor, the white light LED is distorted when being irradiated on an object, and the indoor illumination requirement cannot be met.
In order to improve the color rendering index of white LED lamps by improving the excitation of red phosphor in the blue region, but the effect is not obvious, and the emission intensity is sacrificed while red-shifting the emission band [ see documents Y.X.Pan, M.M.Wu, Q.Su. "Tailoredphotoluminescences of YAG: Ce phosphor through variations methods", J.Phys.chem.solid.65(2004) 845)]。Eu2+The preparation of nitride-doped red phosphors is currently the major commercial red phosphor because of its high quantum efficiency and strong absorption in the blue region [ see document x.q.piao, t.horikawa, h.hanzawa, k.machida, "charaterization and luminescence properties of sr2Si5N8:Eu2+phosphor for white light-emitting-diode illumination”,Appl.Phys.Lett.88(2006)161908.Y.Q.Li,DeWith G,H.T.Hintzen,“The effect of replacement of Sr byCa on the structural and luminescence properties of thered-emitting Sr2Si5N8:Eu2+LED conversion phosphor”,J.Solid State Chem.181(2008)515-524.]. However, the scarcity of nitride fluorescent powder and the whole process of mixing and preparing need to avoid water and oxygen, and the conditions are severe, so that the nitride red light material is high in price.
In recent years, Mn is doped into the alloy4+The red phosphor composed of octahedral complex alkali metal fluoride has attracted the great interest of researchers because of its excellent photoluminescence characteristics for potential application in white LED lamps [ see text ]The document Y.K.xu, S.Adachia, "Properties of Na2SiF6:Mn4+and Na2GeF6:Mn4+red phosphorssynthesized by wet chemical etching”,J.Appl.Phys.105(2009)013525.S.Adachia,T.Takahashi,“Direct synthesis and properties of K2SiF6:Mn4+phosphorby wetchemical etching of Si wafer”,Appl.Phys.104(2008)023512.Xi L,Pan Y,Chen X,Huang S,Wu M.Optimized photoluminescence of red phosphor Na2SnF6:Mn4+as redphosphor in theapplication in“warm”whiteLEDs.J Am Ceram Soc.2017；100:2005–2015]. However, in order to synthesize these red alkali metal fluoride phosphors, high-purity silicon or metals (zirconium, germanium and titanium) are required, the problem of oxidation corrosion (due to the large amount of HF and KMnO4 contained in the solution) is solved, and the manganese oxide compound in the product affects the luminous efficiency. Doping Mn in composite fluoride4+Synthesis of Red phosphor A2XF6:Mn4+(A is potassium or sodium; X is silicon, titanium, germanium or zirconium) and BaXF6:Mn4+(X is silicon or titanium) has a broad absorption band, which overlaps with the electroluminescent band of the GaN chip, and large Stokes shift and sharp emission peaks can be shown because they are more Eu-doped2+Nitrides are more suitable because they produce little reabsorption when mixed with the phosphor YAG: Ce. From the LED tube coating experiment, the materials are suitable for improving the color rendering index of the two-primary-color white light LED and reducing the color temperature. Therefore, the red light material added into the YAG-GaN LED can effectively supplement the red light component in the LED, thereby obtaining warm white light suitable for indoor illumination. However, the preparation of such red light materials requires expensive metal simple substances (such as titanium, germanium, silicon, etc.) as raw materials, and when the metal simple substances are refined, the energy consumption is extremely high in the industry, and the requirements on synthesis equipment are high, which is not favorable for large-scale industrial production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a red light material for an inorganic white light LED, which can efficiently absorb blue light of a GaN chip and emit red light, and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a quadrivalent manganese ion doped barium fluoscandate red light material is prepared from Ba3Sc2F12As a matrix, with Mn4+As an activator, the chemical composition is Ba3Sc2F12:Mn4+。
Mn can be realized through the dissolution-diffusion-substitution-crystallization process under the normal temperature or hydrothermal condition4+Partially substituted Sc3 +Become a luminescence center and emit Mn4+Characteristic red light.
The red light material is a light yellow crystal particle, the light is emitted uniformly, the maximum excitation wavelength is in a blue light region, the blue light of the white light LED can be effectively absorbed, the emission wavelength is in a red light region, and the red light component lacking in the LED can be supplemented. Specifically, the excitation spectrum of the ammonium salt red light material consists of 2 broadband bands respectively positioned at 363nm and 466nm, the maximum excitation band is positioned at 466nm, and the maximum excitation band is matched with the electroluminescent wavelength of a blue light LED chip. The emission spectrum consists of three groups of peaks respectively positioned at 615nm, 632nm and 650nm, and the highest peak is positioned at 632 nm. The material can supplement red components lacking in the white light LED so as to improve the color rendering index of the white light LED.
The preparation method of the tetravalent manganese ion doped barium scandium fluoride acid red light material comprises the following steps: with Sc2O3As scandium source, with BaF2As a barium source, with K2MnF6In order to activate the ionic manganese source, aqueous HF solution is used as a medium and a fluorinating agent. During the preparation, Sc2O3Placing the solid in a plastic container, adding HF aqueous solution and solid Ba (NO)3)2And K2MnF6Reacting for a certain time at normal temperature, filtering, and naturally airing to obtain a product with complete crystallization. The product does not contain rare earth, the preparation method is simple, high-temperature sintering is not needed, and the method is suitable for industrial production.
Preferably, the mass concentration of the HF aqueous solution is 15-25 wt%.
Preferably, said K2MnF6The molar concentration in the reaction system is 0.1-0.8% (relative to Sc)3+)。
Preferably, the temperature of the reaction is from room temperature to 100 ℃.
Preferably, the reaction time is 3-8 hours.
Compared with the prior art, the invention has the following advantages and effects:
1) compared with the commercial nitride red powder, the preparation method has the advantages that the preparation process does not need to avoid water and oxygen, and the cost is far lower than that of the commercial nitride red powder.
2) The present invention and the Mn of the invention4+Compared with red light material, the red light material does not contain alkali metal, so that the stability of the matrix is high
3) Inventive Ba3Sc2F12:Mn4+The red light material product has simple components, does not contain rare earth, has simple preparation method, does not need high-temperature sintering, is suitable for large-scale industrial production and has obvious production advantages.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of the product of example 1; wherein (a) in the figure is Ba3Sc2F12:+XRD standard card data of (a); (b) is the product Ba synthesized in example 13Sc2F12:Mn4+XRD pattern of (a);
FIG. 2 shows Ba as a product synthesized in example 13Sc2F12:Mn4+The excitation spectrum of (1); a: monitoring wavelength of 630nm) and emission spectrum (b: excitation wavelength 467 nm);
FIG. 3 shows Ba as a product synthesized in example 13Sc2F12:Mn4+Scanning Electron Micrograph (SEM).
Detailed Description
The invention will be further described with reference to examples and figures, but the scope of the invention as claimed is not limited to the examples shown.
Example 1
0.1382g of Sc were accurately weighed2Placing the O solid in a plastic container, and adding 30ml of HF aqueous solution with the mass concentration of 40% and 0.5260g of Ba (NO) in sequence3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.5% (relative to Sc)3+). And magnetically stirring for 5 hours at normal temperature, filtering, washing with water, and naturally drying to obtain light yellow crystal powder. The product emits bright red light under an ultraviolet lamp. XRD of the product was measured with Bruker D8Advance X-ray diffractometer as shown in FIG. 1, showing that the product was pure Ba3Sc2F12And (4) phase(s). Tests show that the product obtained in the embodiment is a faint yellow crystal under natural light and emits bright red light under an ultraviolet lamp. The luminescence property of the product was measured at room temperature using a Fluoromax-4 fluorescence spectrometer (horiba jobin Yvon Inc.), as shown in FIG. 2, the excitation spectrum of the material consisted of 2 broad bands at 385nm and 467nm, respectively, with the maximum excitation band at 467nm, which is matched with the electroluminescence wavelength of the blue LED chip. The highest peak of the emission spectrum is located at 630 nm. The material can supplement red components lacking in the white light LED so as to improve the color rendering index of the white light LED and reduce the color temperature. Scanning electron microscopy was performed on a novannosem 200, under the influence of an electron beam; as shown in FIG. 3, the magnification is 20000 times, and the product is observed to be about lamellar cubic block with the diameter of about 5-10 microns, the particle size is uniform, the dispersibility is good, and the coating of LED is facilitated.
Example 2
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 5% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.01% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 100 ℃ for 1 hour, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits bright red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 3
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 15% and 0.5260g of Ba (Ba: (B))NO3)2And K2MnF6Solid, in the reaction system K2MnF6Is 1% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 120 ℃ for 12 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits weak red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 4
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 25% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.1% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 160 ℃ for 3 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits bright red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 5
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 20% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.8% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 180 ℃ for 8 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits weak red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 6
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 20% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.05% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 100 ℃ for 8 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits weak red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 7
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 20% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.2% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 100 ℃ for 8 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits weak red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
Example 8
0.1382g of Sc were accurately weighed2Placing the O solid in a polytetrafluoroethylene reaction kettle lining, and adding 30ml of HF aqueous solution with the mass concentration of 20% and 0.5260g of Ba (NO)3)2And K2MnF6Solid, in the reaction system K2MnF6Is 0.3% (relative to Sc)3+). And (3) uniformly stirring by magnetic force, putting into a reaction kettle, heating at 100 ℃ for 8 hours, taking out, cooling, carrying out suction filtration, washing with water, and naturally airing to obtain light yellow crystal powder. The product emits bright red light under an ultraviolet lamp. The XRD pattern, fluorescence spectrum and SEM pattern of the yellowish crystal powder material are substantially the same as those in FIGS. 1 to 3.
The invention does not use expensive metal simple substance to synthesize the red light material by an etching method, does not use a high-temperature sintering method with harsh conditions to synthesize the red light material, and does not use water and oxygen avoidance in a preparation process with more harsh conditionsThe material Ba of the invention is synthesized by a low-temperature hydrothermal method3Sc2F12:Mn4+。
Claims (5)
1. A preparation method of a tetravalent manganese ion doped barium scandium fluoride acid red light material is characterized by comprising the following steps:
the quadrivalent manganese ion doped barium fluoscandate red light-emitting material is prepared from Ba3Sc2F12As a matrix, with Mn4+As an activator, the chemical composition is Ba3Sc2F12:Mn4+；Mn4+Partially substituted Ba3Sc2F12Sc in (1)3+Becomes a luminescence center, Mn4+Has a molar doping concentration of Sc3+0.01-1.0%; the barium fluoscandate red light material is a faint yellow crystal particle, the luminescence is uniform, the maximum excitation wavelength is in a blue light area, the barium fluoscandate red light material can be effectively excited by a GaN blue light chip, the emission wavelength is in a red light area, and the red light component lacking in an LED can be supplemented;
the preparation process comprises the following steps: subjecting Sc to2O3Placing the solid in a reaction container, adding HF aqueous solution and solid Ba (NO)3)2And K2MnF6And carrying out reaction, suction filtration and natural drying to obtain a product with complete crystallization, namely the quadrivalent manganese ion doped barium fluoscandate red light material.
2. The method for preparing a tetravalent manganese ion doped barium scandium fluoride acid red light material according to claim 1, wherein the method comprises the following steps: the mass concentration of the HF aqueous solution is 5-40 wt%.
3. The method for preparing a tetravalent manganese ion doped barium scandium fluoride acid red light material according to claim 1, wherein the method comprises the following steps: k2MnF6Molar concentration in the reaction system with respect to Sc3+0.1 to 0.8%.
4. The method for preparing a tetravalent manganese ion doped barium scandium fluoride acid red light material according to claim 1, wherein the method comprises the following steps: the reaction temperature is from normal temperature to 180 ℃.
5. The method for preparing a tetravalent manganese ion doped barium scandium fluoride acid red light material according to claim 1, wherein the method comprises the following steps: the reaction time is 1-12 hours.
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Application publication date: 20190111 Assignee: ZHEJIANG YONGGUANG ELECTRIC APPLIANCES Co.,Ltd. Assignor: Wenzhou University Contract record no.: X2020330000082 Denomination of invention: A red luminescent material of barium scandate doped with tetravalent manganese ion and its preparation method Granted publication date: 20200901 License type: Common License Record date: 20201028 |