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Hydroxide phosphate compound and method for preparing fluorophor by same

A technology of hydroxyphosphate compounds and phosphors, which is applied in the fields of phosphates, rare earth metal compounds, chemical instruments and methods, etc., and can solve the problems of easy deviation of the ratio of hydrogen phosphate and oxalate, impurity of the final product phase, and decrease of luminous intensity and other problems, to achieve the effect of reducing the decline of luminous performance, reducing the sintering temperature, and the ratio is easy to control

Inactive Publication Date: 2011-09-07
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some problems to be solved urgently in the wet chemical synthesis method used to prepare phosphorus-containing phosphors involved in the current literature, such as the hydrogen phosphate-oxalate (or hydrogen phosphate-carbonate) co- In the precipitation method, because the ratio of hydrogen phosphate and oxalate (or carbonate) is easy to deviate, the phase state of the final product is impure, resulting in a decrease in luminous intensity
In addition, for this precipitation system, the ammonium halide added in the later stage will still cause agglomeration of the roasted product, and high-strength crushing treatment is still required, which will cause the same problems as the solid-phase method

Method used

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  • Hydroxide phosphate compound and method for preparing fluorophor by same
  • Hydroxide phosphate compound and method for preparing fluorophor by same
  • Hydroxide phosphate compound and method for preparing fluorophor by same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh and prepare SrCl 2 , BaCl 2 , CaCl 2 , MgCl 2 and EuCl 3 Solution, the concentration of which is accurately calibrated is 2.5485mol / L, 1.008mol / L, 1.8528mol / L, 0.7562mol / L, 0.656mol / L. The dosage of each solution is shown in Table 1, mixed into solution A; weigh 22.37g (NH 4 ) 3 PO 4 , dissolved in 500ml of water, adjusted to pH 10.5 with ammonia water, and recorded as solution B.

[0038]Add solution A to solution B, and keep stirring. During the reaction, use ammonia water to control the pH value to 10.5, and the reaction time is 0.5h. After the reaction is completed, age the precipitate for 10h, filter, wash, and oven-dry at 110°C to obtain the precursor powder.

[0039] Adding the corresponding alkaline earth metal chlorides and 25% NH as shown in Table 1 is 5% by mass relative to the total amount of raw material in the precursor 4 Cl, ground and mixed evenly, and fired for 1 h in a reducing atmosphere of carbon powder at 1200 °C.

Embodiment 2～12

[0041] SrCl 2 , BaCl 2 , CaCl 2 , MgCl 2 and EuCl 3 The concentration of the solution is the same as in Example 1. The consumption of each embodiment solution is shown in Table 1, and is mixed into solution A; Weigh 19.81g (NH 4 ) 2 HPO 4 , dissolved in 500ml of water, adjusted to pH 10.7 with ammonia water, and recorded as solution B.

[0042] Add solution A to solution B, and keep stirring. During the reaction, use ammonia water to control the pH value to 10.7, and the reaction time is 1h. After the reaction is completed, age the precipitate for 12h, filter, wash, and dry in an oven at 110°C to obtain the precursor powder. .

[0043] Adding the corresponding alkaline earth metal chlorides and 6% NH as shown in Table 1 is 15% by mass relative to the total amount of raw material in the precursor 4 Cl, ground and mixed evenly, and fired for 1 h in a reducing atmosphere of carbon powder at 1000 °C. After washing with water and drying, the phosphors with the composition...

Embodiment 13～15

[0050] Weigh Sr(NO 3 ) 2 , Ba(NO 3 ) 2 , Ca(NO 3 ) 2 and Eu(NO 3 ) 3 And prepare the corresponding solution, and accurately calibrate the concentration of xxxxxxxxxxxxxxxxxx to be 2.4475mol / L, 1.105mol / L, 1.5684mol / L, and 0.478mol / L respectively. The dosage of each embodiment solution is shown in Table 3, and 5.23ml EuCl 3 The solutions were mixed into solution A; weighed 17.26g NH 4 h 2 PO 4 , dissolved in 500ml of water, adjusted to pH 11.4 with sodium hydroxide, and recorded as solution B.

[0051] Add solution B to solution A, and keep stirring. During the reaction, the pH value is controlled by sodium hydroxide to 11.4, and the reaction time is 0.5h. After the reaction is completed, the precipitate is aged for 16h, filtered, washed, and oven-dried at 110°C to obtain Precursor powder.

[0052] As shown in Table 3, adding the corresponding alkaline earth metal halide and 10% ammonium halide relative to the mass percentage of the total amount of raw materials int...

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Abstract

The present invention relates to a hydroxide phosphate compound, the chemical formula of which is as follows: (SrxBayCazMgw)m(PO4)n(OH)2m-3n.qEuPO4.pEu(OH)3, and x, y, z, w, m, n, p and q are integers or non-integers meeting the following relation: x is more than or equal to 0 and is less than or equal to 1, y is more than or equal to 0 and is less than or equal to 1, z is more than or equal to 0 and is less than or equal to 1, w is more than or equal to 0 and is less than or equal to 0.5, the summation of x, y, z and w is 1, the proportion of the summation of m, q and p and the summation of n and q is more than 1 and is less than or equal to 5 / 3, and the proportion of the summation of q and p and the summation of n and q is more than 0 and is less than or equal to 0.3. The compound can be used for preparing high efficient fluorophor containing phosphor.

Description

technical field [0001] The invention relates to a hydroxyl phosphate compound and its preparation method, as well as a method for preparing a phosphorus-containing phosphor by using the compound as a precursor. Background technique [0002] Phosphorus-containing phosphors are an important branch of luminescent materials, and they are widely used in many fields such as lighting and display. For example, europium-activated halophosphate phosphors are mainly used as blue phosphor components in rare-earth three-color fluorescent lamps and cold-cathode fluorescent lamps for LCD backlights. [0003] Phosphorus-containing phosphors are usually prepared by a high-temperature solid-phase method, such as Chinese invention patents CN1128785A, CN1621491A, U.S. invention patent US4500443, British invention patent GB1264422, etc. In these preparation methods, the raw materials are usually phosphorus-containing compounds and other components that make up the phosphor. The compound corresp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/81C01F17/00C01B25/26
Inventor 罗新宇胡运生赵春雷庄卫东胡晓珊鱼志坚何华强
Owner GRIREM ADVANCED MATERIALS CO LTD
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