Preparation method of phosphate luminescent material

A luminescent material and phosphate technology, which is applied in the field of preparation of phosphate luminescent materials, can solve the problems of reducing calcination temperature and calcination time, and poor particle size uniformity of products, so as to achieve lower calcination temperature, good product performance consistency, and simple process Effect

Inactive Publication Date: 2011-03-02
XIAN UNIV OF TECH
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Problems solved by technology

[0007] The purpose of the present invention is to propose a method for preparing phosphate luminescent materials, which can not only significantly reduce the calcination temperature and calcination time, but also overcome the activator ion doping and The problem of poor particle size uniformity of the product, and can improve the fluorescence properties of phosphate

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  • Preparation method of phosphate luminescent material

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preparation example Construction

[0028] The invention provides a method for preparing a phosphate luminescent material, wherein the phosphate is a single metal cation phosphate or a single-phase multi-metal cation phosphate;

[0029] Such as figure 1 Shown, its preparation method comprises the following steps:

[0030] Step 1, prepare raw materials and pH regulator:

[0031] According to the phosphate molecular formula to be prepared PO 4 3- Take raw material A and raw material B with the mol ratio of metal cation;

[0032] The raw material A contains PO 4 3- Substances that are soluble in acid or water;

[0033] The raw material B contains metal cations corresponding to the phosphate to be prepared, is soluble in acid or water and is compatible with PO 4 3- Substances that can directly react to form phosphate precipitates that are insoluble in the aqueous liquid phase system;

[0034] The pH regulator is urea or hexamethylenetetramine;

[0035] Step 2,

[0036] After mixing raw material A, raw mat...

Embodiment 1

[0044] A kind of preparation YPO 4 : Dy 3+ (Single-phase multi-metal cationic phosphate) method of phosphor luminescent material:

[0045] Step 1, prepare raw materials and pH regulator:

[0046] YPO as prepared 4 : Dy 3+ The Y in the phosphate formula 3+ 、Dy 3+ and PO 4 3- The molar ratio of each weighs 1.12g of Y 2 o 3 , 0.019g Dy 2 o 3 and 1.32g (NH 4 ) 2 HPO 4 ; The pH regulator is urea;

[0047] Step 2,

[0048] 1.12g Y 2 o 3 , 0.019gDy 2 o 3 , 1.32g (NH 4 ) 2 HPO 4 After mixing evenly with 25g of urea, first add 25ml of concentrated nitric acid with a concentration of 69%, then add 40ml of water, fully dissolve the mixture with acid and water, and obtain a clear solution C with a solution temperature of 40°C and a pH value of 1;

[0049] Step 3,

[0050] Heating solution C at a heating temperature of 90°C and stirring continuously, after the complete reaction of urea, the pH value of solution C reaches 7, and then aging for 5 hours, after filterin...

Embodiment 2

[0058] A kind of preparation YPO 4 :Eu 3+ (Single-phase multi-metal cationic phosphate) method of phosphor luminescent material:

[0059] Step 1, prepare raw materials and pH regulator:

[0060] YPO as prepared 4 :Eu 3+ The Y in the phosphate formula 3+ 、Eu 3+ and PO 4 3- The molar ratio weighs 1.12g of Y 2 o 3 , 0.018g Eu 2 o 3 and 1.32g (NH 4 ) 2 HPO 4 ; The pH regulator is urea;

[0061] Step 2,

[0062] 1.12g Y 2 o 3 , 0.018g Eu 2 o 3 , 1.32g (NH 4 ) 2 HPO 4 After mixing evenly with 35g of urea, first add 15ml of concentrated nitric acid with a concentration of 69%, then add 60ml of water, fully dissolve the mixture with acid and water, and obtain a clear solution C with a solution temperature of 20°C and a pH value of 3;

[0063] Step 3,

[0064] Heating solution C at a heating temperature of 95°C and stirring continuously, after the complete reaction of urea, the pH value of solution C reaches 9, and then aging for 5 hours, after filtering, washin...

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Abstract

The invention discloses a preparation method of phosphate luminescent material, which is used for preparing monometallic cation phosphate and single-phase polymetallic cation phosphate. In a liquid phase system containing water, the raw materials comprise substance which contains PO4<3-> and can be dissolved into acid or water, and substance which contains corresponding metallic cation, can be dissolved into acid or water and directly reacts with PO4<3-> to generate water-fast phosphate precipitate. The raw materials and the pH value regulator are mixed to be dissolved into acid and water to obtain settled solution. Urea is heated and decomposed to evenly release OH<-> to cause the pH value of the solution to rise, and meanwhile, the phosphate which is not dissolved in the liquid phase system is generated. The final product is obtained by washing, drying, ball milling and high-temperature calcining. The invention has the advantages of simple technology, short flow, easy control, low cost, low calcination temperature, even particle size distribution, good fluorescence performance and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic solid luminescent materials, and relates to a preparation method of phosphate luminescent materials. Background technique [0002] Inorganic solid luminescent materials are generally composed of three parts: matrix material, activator, and sensitizer. The matrix material is the main body of the luminescent material, which provides a dispersed matrix for the activator and sensitizer ions, can work with the sensitizer to absorb radiation energy and transmit it to the activator, and can also directly affect the emission spectrum of the activator ion through its own crystal field. structure. The cation as the matrix of the inorganic solid luminescent material must be optically inert, that is, its valence electron shell must be fully filled, and the anion as the matrix material must have light transmission. In general, different substrates have different effects on the behavior of lu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/81C01B25/37
Inventor 何毓阳宋衍滟赵麦群艾璇李峰赵高扬
Owner XIAN UNIV OF TECH
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