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Preparation method of single-substrate Ca2SiO3Cl2:xTb<3+> fluorescent powder for white-light LEDs (light-emitting diodes)

A phosphor powder and a single technology, applied in the field of preparation of single matrix phosphor powder for white light LED, can solve the problems of easy existence of impurity phase, long synthesis route, easy introduction of impurities, etc., and achieve the effect of good dispersion and uniform particles

Inactive Publication Date: 2014-12-03
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The phosphor powder prepared by the solid phase method has a large particle size and uneven particle size distribution, it is difficult to obtain spherical particles, and impurity phases are prone to exist, which reduces the luminous efficiency of the phosphor powder; the chemical precipitation method has higher requirements on the purity of raw materials, and the synthetic route Longer, it is easy to introduce impurities, thereby affecting the luminescent performance of the phosphor; the hydrothermal method has serious limitations, and this method is often only suitable for the preparation of oxides or a small number of sulfides that are not sensitive to water, so a more efficient method is needed. simple preparation method

Method used

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  • Preparation method of single-substrate Ca2SiO3Cl2:xTb&lt;3+&gt; fluorescent powder for white-light LEDs (light-emitting diodes)
  • Preparation method of single-substrate Ca2SiO3Cl2:xTb&lt;3+&gt; fluorescent powder for white-light LEDs (light-emitting diodes)
  • Preparation method of single-substrate Ca2SiO3Cl2:xTb&lt;3+&gt; fluorescent powder for white-light LEDs (light-emitting diodes)

Examples

Experimental program
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Effect test

Embodiment 1

[0024] The invention provides an alkaline earth chlorosilicate-based white light phosphor for white light LED, the chemical composition formula of which is Ca 2 SiO 3 Cl 2 :xTb3+ , where the value of x is 0.001. The technical solution is:

[0025] 1) According to the stoichiometric ratio, weigh and synthesize 0.02 mol Ca 2 SiO 3 Cl 2 :xTb 3+ Required SiO 2 0.02mol, and the SiO used 2 The particle size of SiO is 1~5μm, measure 20ml of ammonia solution with a concentration of 15wt%, put the two in a hydrothermal reaction kettle, and treat SiO at 230°C 2 Perform hydrothermal treatment for 15 hours, wherein the filling degree of the hydrothermal reactor is 75%, then cool and dry to form powder A.

[0026] 2) Measure and synthesize 0.02mol of Ca according to the stoichiometric ratio 2 SiO 3 Cl 2 Anhydrous CaCl required 2 and Ca(NO 3 ) 2 4H 2 O, each 0.02mol, add it into 4~6ml of deionized water, and keep stirring until all the raw materials are dissolved to form sol...

Embodiment 2

[0031] The invention provides an alkaline earth chlorosilicate-based white light phosphor for white light LED, the chemical composition formula of which is Ca 2 SiO 3 Cl 2 :xTb 3+ , where the value of x is 0.002. The technical solution is:

[0032] 1) According to the stoichiometric ratio, weigh and synthesize 0.02mol Ca 2 SiO 3 Cl 2 :xTb 3+ Required SiO 2 0.02mol, and the SiO used 2 The particle size of SiO is 1~5μm, measure 20ml of ammonia solution with a concentration of 15wt%, put the two in a hydrothermal reaction kettle, and treat SiO at 230°C 2 Perform hydrothermal treatment for 18 hours, wherein the filling degree of the hydrothermal kettle is 75%, then cool and dry to form powder A.

[0033] 2) Measure and synthesize 0.02mol of Ca according to the stoichiometric ratio 2 SiO 3 Cl 2 Anhydrous CaCl required 2 and Ca(NO 3 ) 2 4H 2 O, each 0.02mol, add it into 4-6ml of deionized water, and keep stirring until all the raw materials are dissolved to form sol...

Embodiment 3

[0039] The invention provides an alkaline earth chlorosilicate-based white light phosphor for white light LED, the chemical composition formula of which is Ca 2 SiO 3 Cl 2 :xTb 3+ , where the value of x is 0.003. The technical solution is:

[0040] 1) According to the stoichiometric ratio, weigh and synthesize 0.02mol Ca 2 SiO 3 Cl 2 :xTb 3+ Required SiO 2 0.02mol, and the SiO used 2 The particle size of SiO is 1~5μm, measure 20ml of ammonia solution with a concentration of 15wt%, put the two in a hydrothermal reaction kettle, and treat SiO at 240°C 2 Carry out hydrothermal treatment for 20 hours, wherein the filling degree of the hydrothermal kettle is 75%, then cool and dry to form powder A.

[0041] 2) Measure and synthesize 0.02mol of Ca according to the stoichiometric ratio 2 SiO 3 Cl 2 Anhydrous CaCl required 2 and Ca(NO 3 ) 2 4H 2 O, each 0.02mol, add it into 4-6ml of deionized water, and keep stirring until all the raw materials are dissolved to form s...

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Abstract

The invention provides a preparation method of single-substrate Ca2SiO3Cl2:xTb<3+> fluorescent powder for white-light LEDs (light-emitting diodes), which comprises the following steps: carrying out hydrothermal treatment on the raw material SiO2 with the particle size of 1-5 mu m in an alkaline environment to obtain SiO2 powder A with higher reaction activity, dissolving CaCl2 and Ca(NO3)2 in deionized water to form a mixed transparent solution B, and dissolving terbium oxide in a nitric acid solution to obtain a Tb-containing rare earth ion solution C; mixing the powder A, mixed solution B and solution C, dispersing uniformly under ultrasonic action to form a mixture, adding a composite suspending agent into the mixture to form a stable suspension, and carrying out spray drying to obtain powder; and finally, putting the powder in an aluminum oxide crucible, putting the crucible in a zirconium oxide tank filled with carbon powder, sealing, and sintering in a resistance furnace.

Description

technical field [0001] The invention relates to a preparation method of a single-matrix fluorescent powder for white light LEDs, in particular to a preparation method of a single-matrix phosphor powder for white light LEDs. Background technique [0002] White LED has the characteristics of environmental protection, energy saving, high efficiency, long life and easy maintenance, and has been widely used in the field of display and lighting. At present, high-quality white LEDs mainly use the method of (near) ultraviolet light tube core to excite three primary color phosphors and the method of combining LED chips and phosphors to achieve white light emission. The performance of the former, such as lumen efficiency and color reproduction, is greatly affected by the problems of color reabsorption and ratio control between the mixtures. The latter converts the short-wavelength light emitted by the chip into visible light partially or completely through phosphor powder. Finally, i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/61
Inventor 宁青菊郭芳芳乔畅君李向龙史永胜于成龙
Owner SHAANXI UNIV OF SCI & TECH
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