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A kind of mn4+ ion-doped titanate-based red fluorescent powder and preparation method thereof
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A technology of red phosphor and ion doping, applied in chemical instruments and methods, luminescent materials, climate sustainability, etc., can solve the problems of poor rare earth sources and expensive raw materials, and achieve wide excitation spectrum range and high color rendering , the effect of good thermal stability
Active Publication Date: 2018-12-04
徐州博创建设发展集团有限公司
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[0003] At present, phosphors doped with rare earth ions have been widely studied, but it is well known that the source of rare earth is poor and the raw materials are expensive
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[0034] The preparation method of the red fluorescent powder includes: a high-temperature solid-phase method and a sol-gel method. The red fluorescent powder with high luminous intensity and good stability is prepared by using the two preparation methods, and is applied to the preparation of LED lighting devices.
[0035] Described high-temperature solid phase method, comprises the steps:
[0036] (1) According to the chemical formula MgAl 8 Ti 6(1-x) mn 6x o 25 The stoichiometric ratio of each element in , where 0.0005≤x≤0.025, respectively weighed Mg containing magnesium ions 2+ Compounds containing aluminum ions Al 3+ Compounds containing manganese ions Mn 4+ Compounds containing titanium ions Ti 4+ compound, grind and mix well to obtain a homogeneous mixture;
[0037] (2) Calcining the mixture obtained in step (1) in an air atmosphere, the calcination temperature is 400-900° C., and the calcination time is 3-12 hours;
[0038] (3) After the mixture obtained in step ...
Embodiment 1
[0046] Embodiment 1: according to chemical formula MgAl 8 Ti 5.94 mn 0.06 o 25 The stoichiometric ratio of each element in, respectively weighed magnesium oxide MgO: 0.269 grams, aluminum oxide Al 2 o 3 : 2.719 g, manganese oxide MnO 2 : 0.035 g, titanium dioxide TiO 2 : 3.163 grams, after adding an appropriate amount of acetone to the agate mortar, mixing and grinding evenly, pre-calcining in the air atmosphere, calcining at 850 ° C for 10 hours and cooling in the furnace, taking out the sample and using the same method again for the pre-calcined raw materials Thoroughly mix and grind evenly, then calcinate again in the air atmosphere, calcinate at 1350°C for 10 hours, cool to room temperature, take it out and thoroughly grind to obtain the sample.
[0047] See attached figure 1 , is the X-ray powder diffraction pattern of the sample prepared by the technical scheme of this embodiment; the XRD test results show that the prepared sample has good crystallinity and no impur...
Embodiment 2
[0052] Embodiment 2: according to chemical formula MgAl 8 Ti 5.997 mn 0.003 o 25 The stoichiometric ratio of each element in the formula, weigh basic magnesium carbonate 4MgCO 3 ·Mg(OH) 2 ·5H 2 O: 0.972 g, aluminum carbonate Al 2 (CO 3 ) 3 : 9.360 g, manganese carbonate MnCO 3 : 0.004 g, titanium dioxide TiO 2 : 4.790 grams, add an appropriate amount of acetone to the agate mortar, mix and grind evenly, then pre-calcine in the air atmosphere, calcined at 750 ° C for 8 hours and cool in the furnace, take out the sample, and use the same method to fully dry the pre-calcined raw materials again. Mix and grind evenly, then calcinate again in the air atmosphere, calcinate at 1250°C for 8 hours, cool to room temperature, take it out and grind it thoroughly to get the sample.
[0053] The X-ray powder diffraction pattern, diffuse reflectance pattern, excitation spectrum pattern, luminescence spectrum pattern, luminescence decay curve, and SEM pattern of the sample prepared ...
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Abstract
The invention discloses Mn<4+> ion-doped titanate-based red fluorescent powder and a preparation method and belongs to a preparation method and application of titanate-based red fluorescent powder. A chemical formula of a red fluorescent powder material is MgAl8Ti6(1-x)Mn6xO25, wherein x is a mol ratio of Mn<4+> doping and x is more than or equal to 0.0005 and less than or equal to 0.025; the mass percent of the MgAl8Ti6(1-x)Mn6xO25 is obtained by multiplying the amount-of-substance ratio of each element by respective mol mass; the red fluorescent powder can emit red fluorescent light with the wavelength range of 620nm to 750nm when the red fluorescent powder is excited by excitation light sources including ultraviolet light, near ultraviolet light or blue light and the like; the preparation method of the red fluorescent powder comprises a high-temperature solid-phase method and a sol-gel method; two preparation methods are adopted and are used for preparing the red fluorescent powder with high light emitting intensity and good stability; the red fluorescent powder is applied to preparation of an LED (Light Emitting Diode) illumination device. The Mn<4+> ion-doped titanate-based red fluorescent powder and the preparation method have the advantages that the preparation method is simple and the production cost is low; the Mn<4+> ion-doped titanate-based red fluorescent powder is the red fluorescent powder material with a good light emitting performance and can emit the red fluorescent light with the wavelength range of 620nm to 750nm; an excitation spectrum range is relatively wide and light is greatly absorbed at a part with the wavelength of 355nm; the material is used for manufacturing ultraviolet light excited white-light LED fluorescent powder.
Description
technical field [0001] The invention relates to a titanate-based red fluorescent powder and a preparation method thereof, in particular to a titanate-based red fluorescent powder doped with Mn4+ ions and a preparation method thereof. Background technique [0002] Light-emitting diodes (LEDs), as one of the more efficient solid-state light-emitting devices, can effectively convert electrical energy into light energy. Since its appearance in the 1960s, it has been widely used in the fields of display and lighting because of its advantages such as long life, high energy conversion efficiency, good stability, and low price. Especially since the successful development of high-power white LEDs, this "green" light source with ultra-high superior performance is regarded as another major revolution in the history of lighting. White light is actually formed by mixing polychromatic light. According to the principles of luminescence and photometry, white light can be formed by mixing t...
Claims
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