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Preparation of complex fluoride and complex fluoride phosphor

A technology of composite fluoride and fluoride, which is applied in the direction of fluoride preparation, tin compound, germanium compound, etc., can solve the problem of phosphors without emission performance, and achieve high yield effect

Active Publication Date: 2012-10-17
SHIN ETSU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction product has no emission properties and cannot be used as a phosphor

Method used

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  • Preparation of complex fluoride and complex fluoride phosphor
  • Preparation of complex fluoride and complex fluoride phosphor
  • Preparation of complex fluoride and complex fluoride phosphor

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0070] K 2 MnF 6 preparation of

[0071] Potassium hexafluoromanganate (K 2 MnF 6 ).

[0072] The reaction vessel of the vinyl chloride resin is divided into two chambers by the middle partition of the fluorine resin ion exchange membrane. Install platinum plates as anode and cathode in two chambers separated by an ion exchange membrane. An aqueous hydrofluoric acid solution in which manganese(II) fluoride is dissolved is fed to the chamber on the anode side, and aqueous hydrofluoric acid is fed to the chamber on the cathode side. A power supply was connected to the electrodes to perform electrolysis at a voltage of 3V and a current of 0.75A. At the end of the electrolysis, aqueous hydrofluoric acid containing saturated levels of potassium fluoride was added in excess to the reaction solution in the anode side chamber. Thus a yellow solid product was formed which was filtered and used as K 2 MnF 6 Recycle.

Embodiment 1

[0074] By dissolving 4.8g of silica in 100cm 3 48 wt% hydrofluoric acid aqueous solution and cooling the solution to room temperature to prepare an aqueous solution of silicon fluoride. K in the preparation example 1 2 MnF 6 The powder (1.19 g) was added to an aqueous solution of silicon fluoride and dissolved therein by stirring to obtain a compound containing silicon fluoride and K 2 MnF 6 aqueous solution as the first solution. separately, through the 40cm 313.95 g of potassium fluoride was dissolved in a 48 wt % hydrofluoric acid aqueous solution and the solution was cooled to room temperature to prepare an aqueous potassium fluoride solution as a second solution. With stirring, the second solution was slowly added to the first solution over about 3 minutes. Stirring was continued for about 10 minutes further, whereupon a pale orange solid precipitated. The solid product was filtered, washed with a small volume of 20 wt% aqueous hydrofluoric acid followed by ethanol...

Embodiment 2

[0079] By dissolving 4.8g of silica in 100cm 3 48 wt% hydrofluoric acid aqueous solution and cooling the solution to room temperature to prepare an aqueous solution of silicon fluoride. K in the preparation example 1 2 MnF 6 The powder (1.19 g) was added to an aqueous solution of silicon fluoride and dissolved therein by stirring to obtain a compound containing silicon fluoride and K 2 MnF 6 aqueous solution as the first solution. separately, through the 25cm 3 23.24 g of potassium fluoride was dissolved in water and the solution was cooled to room temperature to prepare an aqueous potassium fluoride solution as a second solution. With stirring, the second solution was slowly added to the first solution, whereupon a pale orange solid precipitated. The solid product was filtered, washed with a small volume of 20 wt% aqueous hydrofluoric acid and then ethanol, and dried under vacuum to yield 16.79 g of reaction product.

[0080] By powder X-ray diffractometer, the product...

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Abstract

A complex fluoride A 2 MF 6 wherein M is a tetravalent element Si, Ti, Zr, Hf, Ge or Sn, A is an alkali metal Li, Na, K, Rb or Cs is prepared by providing a first solution containing a fluoride of M, providing a second solution containing a compound of A and / or the compound of A in solid form, mixing the first solution with the second solution and / or the solid for reacting the fluoride of M with the compound of A, and recovering the resulting solid product via solid-liquid separation.

Description

field of invention [0001] The present invention relates to a method for preparing composite fluorides in a safe and effective manner, and a method for preparing composite fluoride phosphors with improved emission properties. Background technique [0002] In order to add a red tint to the light emission of white LEDs to impart warmth to the emission color, a phosphor capable of emitting red light when excited with near UV to blue LEDs is required. A lot of work has been done on this, WO 2007 / 100824 describes a Mn-doped compound of the formula A 2 MF 6 A compound fluoride of which A is Na, K, Rb, etc., and M is Si, Ge, Ti, etc. [0003] The preparation method described therein is by dissolving or dispersing raw materials in hydrofluoric acid and heating to evaporate to dryness. Since a solution containing a high concentration of hydrofluoric acid must be heated at a high temperature, a large amount of hydrogen fluoride, which is harmful to the human body, is volatilized. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61C09K11/67
CPCC01G17/00C01G23/002C01G17/006C01G25/006C01G27/00C01P2004/03C01G25/00C01P2004/61C01P2002/84C01G27/006C09K11/617C01G23/00C01G19/006C01G19/00C01B9/08C01P2004/62C09K11/61C09K11/66
Inventor 金吉正实高井康
Owner SHIN ETSU CHEM CO LTD
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