Method for producing and method for processing complex fluoride phosphor

一种复合氟化物、制造方法的技术，应用在化学仪器和方法、发光材料等方向，达到耐湿性优异的效果

Active Publication Date: 2016-09-28
SHIN ETSU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, Japanese Patent Application Laid-Open No. 2010-45328 (Patent Document 6) describes that the problem of moisture resistance can be alleviated by coating these composite fluoride phosphors with resin or the like before the production of LEDs.

Method used

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  • Method for producing and method for processing complex fluoride phosphor
  • Method for producing and method for processing complex fluoride phosphor
  • Method for producing and method for processing complex fluoride phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] Potassium silicofluoride (manufactured by Morita Chemical Industry Co., Ltd., K 2 SiF 6 ) powder 26.43g and potassium hexafluoromanganate (made by the method described in Reference Example 1 described later, K 2 MnF 6 ) powder 2.46g was put into the same polyethylene zipper bag. Shake or swirl slowly by hand for 5 minutes to mix. The mixing ratio is such that Mn corresponds to 0.083 mol with respect to 1 mol of Si.

[0087] Potassium hydrogen fluoride (acid potassium fluoride manufactured by STELLA CHEMIFA, KHF 2 ) powder 14.06g, mixed in the same manner as above. Ratio is 1 mole relative to Si, KHF 2 Equivalent to 1.5 moles. 2.0 g (mixed powder) was taken out from the powder mixture for later evaluation.

[0088] Put the powder mixture in figure 1 Airtight in the double container 1 shown in . here, figure 1 Among them, the double container 1 is formed by forming the inner layer 3 made of polytetrafluoroethylene on the inner wall of the container body 2 made ...

reference example 1

[0101] [K 2 MnF 6 preparation]

[0102] According to the method described in Non-Patent Document 4, it was prepared by the following method.

[0103] A spacer (diaphragm) of a fluororesin-based ion-exchange membrane was installed in the center of a reaction tank made of vinyl chloride resin, and an anode and a cathode made of platinum plates were installed in each of the two chambers sandwiching the ion-exchange membrane. An aqueous solution of hydrofluoric acid for dissolving manganese (II) fluoride is placed on the anode side of the reaction tank, and an aqueous solution of hydrofluoric acid is placed on the cathode side. Both electrodes were connected to a power supply, and electrolysis was performed at a voltage of 3V and a current of 0.75A. After completion of the electrolysis, a solution of potassium fluoride saturated in an aqueous hydrofluoric acid solution was added in excess to the reaction liquid on the anode side. The yellow solid product that generates is filt...

Embodiment 2

[0105] 14.06g of potassium hydrogen fluoride is replaced by 11.72g, and 4.08g of potassium hydrogen sulfate (Wako Pure Chemicals special grade, KHSO 4 ), except that, operate in the same manner as in Example 1, and obtain K of 31.0g 2 SiF 6 : Powder product of Mn. As a result of the particle size distribution measured in the same manner as in Example 1, D10 = 8.2 μm, D50 = 22.1 μm, and D90 = 35.4 μm.

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Abstract

Provided is a method for producing a red phosphor which is a Mn-activated complex fluoride represented by formula (1), A2MF6: Mn (1) (M is one type or more of a tetravalent element selected from Si, Ti, Zr, Hf, Ge, and Sn, and A is one type or more of an alkali metal selected from Li, Na, K, Rb, and Cs, and includes at least Na and / or K.), wherein, as a reactive source, a solid of a complex fluoride represented by formula (2), A2MF6 (2) (M and A are as described above) and a solid of a manganese compound represented by formula (3), A2MnF6 (3) (A is as described above) are mixed and heated at a temperature of from 100 DEG C to 500 DEG C. According to the present invention, a Mn-activated complex fluoride phosphor having favorable luminescence properties can be obtained without using hydrofluoric acid in a main step.

Description

technical field [0001] The present invention relates to can be used as the red fluorescent substance of blue LED by formula A 2 MF 6 : Mn (in the formula, M is one or more tetravalent elements selected from Si, Ti, Zr, Hf, Ge and Sn, A is selected from Li, Na, K, Rb and Cs and contains at least One or two or more alkali metals of Na and / or K.) A method for producing a Mn-activated composite fluoride red phosphor (composite fluoride phosphor). Moreover, this invention relates to the processing method of this phosphor. Background technique [0002] In order to improve the color rendering of white LEDs (Light Emitting Diodes) or to improve the color reproducibility when using white LEDs as backlights for liquid crystal displays, it is necessary to excite red light from near-ultraviolet to blue LEDs. Phosphors were studied. Among them, it is described in Japanese PCT publication No. 2009-528429 (Patent Document 1) in A 2 MF 6 (A is Na, K, Rb, etc., and M is Si, Ge, Ti, etc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/08C09K11/61
CPCC09K11/616C09K11/617C09K11/57C09K11/59
Inventor 金吉正实
Owner SHIN ETSU CHEM CO LTD
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