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Mn<4+> doped red fluorescent material and preparation method thereof

A technology for red fluorescence and raw materials, applied in the field of Mn4+-doped red fluorescent materials and their preparation, can solve the problems of low light emission color rendering index of white LEDs, harm to human health and environment, poor chemical stability, etc., and achieve enhanced photoluminescence. , low cost, good stability

Pending Publication Date: 2020-05-26
SHANGHAI APPLIED TECHNOLOGIES COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are problems with this solution: the lack of visible red light spectrum leads to low color rendering index, high color temperature, poor color rendering and cold light characteristics of white LEDs.
mn 4+ Ion-activated fluoride red phosphors have excellent red luminescent properties, but high concentrations of hydrofluoric acid, which is extremely harmful to human health and the environment, are required to be used in the synthesis process, and fluoride red phosphors are chemically stable in humid environments Poor performance, has certain limitations in commercial application

Method used

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  • Mn&lt;4+&gt; doped red fluorescent material and preparation method thereof
  • Mn&lt;4+&gt; doped red fluorescent material and preparation method thereof
  • Mn&lt;4+&gt; doped red fluorescent material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: adopt high-temperature solid phase method to prepare (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x o 4 :xMn 4+ (B=Zr; x=0.001, y=0, z=0.01), the raw materials used are analytically pure MgO, TiO 2 , ZrO 2 and MnO 2 ; Then accurately weigh the raw materials and add 5wt% NH according to the molar ratio in the chemical reaction equation 4 F flux, grind and mix evenly with an agate mortar to obtain a precursor; put the precursor into a 25×25mm alumina crucible, then place it in a muffle furnace, and heat it up to 800°C in an air atmosphere for pre-sintering. Insulate for 6 hours, take it out and re-grind it to make it evenly mixed, and heat it for 10 hours under the condition of air atmosphere and 1400°C for the second sintering, put the obtained sample in an agate mortar and grind it, and finally get Mg 2 (Ti 0.99 Zr 0.01 ) 0.999 o 4 :0.1%Mn 4+ Phosphor. X-ray powder diffraction (XRD) analysis result shows, the XRD pattern of sample and M g2 TiO 4 Stand...

Embodiment 2

[0033] Embodiment 2: adopt high temperature solid state method to prepare (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x o 4 :xMn 4+ (A=Ca, B=Zr; x=0.0015, y=0.01, z=0.01), the raw materials used are analytically pure MgO, CaCO 3 、TiO 2 , ZrO 2 and MnO 2 Then, according to the proportion of the chemical reaction equation, accurately weigh the raw materials and add 3wt% LiF flux, grind and mix them evenly with an agate mortar to obtain a precursor, put the precursor into a 25×25mm alumina crucible, and then place it in In the muffle furnace, the temperature is raised to 600°C in the air atmosphere for pre-sintering, and the temperature is kept for 8 hours. After taking it out, it is re-grinded to make it evenly mixed. The samples were ground in an agate mortar to obtain (Mg 0.99 Ca 0.01 ) 2 (Ti 0.99 Zr 0.01 ) 0.9985 o 4 :0.15%Mn 4+ Phosphor. The X-ray powder diffraction analysis results show that the XRD pattern of the sample is consistent with M g2 TiO 4 The standard P...

Embodiment 3

[0034] Embodiment 3: adopt high-temperature solid phase method to prepare (Mg 1-y A y ) 2 (Ti 1-z B z ) 1-x o 4 :xMn 4+ (A=Ca, B=Si; x=0.001, y=0.01, z=0.005), the raw materials used are analytically pure MgO, CaCO 3 、TiO 2 , SiO 2 and MnO2 Then, according to the proportion of the chemical reaction equation, accurately weigh the raw materials and add 5wt% LiF flux, grind and mix them evenly with an agate mortar to obtain a precursor, put the precursor into a 25×25mm alumina crucible, and then place it in In the muffle furnace, the temperature is raised to 600°C in the air atmosphere for pre-sintering, and the temperature is kept for 8 hours. After taking it out, it is re-ground to make it evenly mixed. The second sintering is held in the air atmosphere and 1150°C for 8 hours. The sample was placed in an agate mortar and ground to obtain (Mg 0.99 Ca 0.01 ) 2 (Ti 0.995 Si 0.005 ) 0.999 o 4 :0.1%Mn 4+ Phosphor. X-ray powder diffraction analysis results show that...

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Abstract

The invention relates to a Mn<4+> doped red fluorescent material and a preparation method thereof. The general formula of the fluorescent material is (Mg1-yAy)2(Ti1-zBz)1-xO4: xMn<4+> (A = Ca, Sr, Ba;B=Zr, Si; 0.01 at% < / = x < / = 1.0 at%; 0 < / = y < / = 5 at%; 0 < / = z < / = 10 at%). The preparation method comprises the following steps OF: taking MgO, caCO3, SrCO3, BaCO3, TiO2, ZrO2, SiO2 and MnO2 as raw materials, weighing the raw materials according to the element molar ratio, after uniformly grinding in an agate mortar, carrying out high-temperature solid-phase reaction, adding a proper amount offluxing agent under the condition that a pure phase is guaranteed, and finally acquiring the Mn<4+> doped red fluorescent powder material ((Mg1-yAy)2(Ti1-zBz)1-xO4: xMn<4+>), the obtained Mn<4+> doped red fluorescent powder material having excellent red light-emitting performance. According to the prepared red fluorescent material, Mn<4+> is used as an activator, rare earth elements are not contained, raw materials and final products do not contain harmful substances such as fluorine, the preparation method is simple, and the production cost is low. The red fluorescent powder can emit red fluorescence with the wavelength range of 630-730 nm when excited by excitation light sources such as ultraviolet, near ultraviolet or blue light LEDs, and is suitable for being applied to the field of warm white light LED device illumination and display.

Description

technical field [0001] The invention belongs to the field of solid luminescent materials, in particular to a Mn material used in the field of warm white LED lighting and display. 4+ Doped red fluorescent material and preparation method thereof. Background technique [0002] Compared with traditional incandescent lamps and fluorescent lamps, the new generation of solid-state light sources - semiconductor white light-emitting diodes (white LEDs) have many advantages such as low power consumption, high efficiency, long life, small size, and environmental protection. They are widely used in lighting, display panels, Medical imaging, military and other fields. There are two main schemes for synthesizing white LEDs: blue-light chips compounded with yellow phosphors and near-ultraviolet chips compounded with trichromatic phosphors. Currently, commercial white LEDs are based on InGaN blue LED chips excited by YAG:Ce 3+ The white light obtained by the yellow phosphor powder is mai...

Claims

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Application Information

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IPC IPC(8): C09K11/67
CPCC09K11/673C09K11/676
Inventor 张彦袁军平徐家跃田甜储耀卿申慧罗宽宽黄礼武余枭
Owner SHANGHAI APPLIED TECHNOLOGIES COLLEGE
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