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Preparation method for small particle nitrogen oxide of green emitting phosphor

A technology of green fluorescent powder and nitrogen oxides, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of harsh synthesis conditions, low brightness, and reduced luminous intensity of powders, and achieve the effect of maintaining crystal integrity

Inactive Publication Date: 2011-11-23
IRICO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis conditions of the conventional method are relatively harsh, and the crystal phase purity of the obtained product is relatively low, resulting in a slightly lower brightness than other systems, and the powder synthesized by the high-temperature solid-phase method has relatively high hardness, which requires physical crushing in the later stage to be applicable For the production of LED lamps, as we all know, this kind of physical fragmentation will greatly destroy the crystal structure of the powder, thereby greatly reducing the luminous intensity of the powder

Method used

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  • Preparation method for small particle nitrogen oxide of green emitting phosphor
  • Preparation method for small particle nitrogen oxide of green emitting phosphor
  • Preparation method for small particle nitrogen oxide of green emitting phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Phosphor Sr 0.98 Si 2 O 2 N 2 : Preparation of 0.02Eu

[0028] 1) Forebody Sr 1.96 SiO 4 : Preparation of 0.04Eu

[0029] According to Sr 1.96 SiO 4 : Stoichiometric ratio of 0.04Eu, weigh SrCO 3 173.6g, SiO 2 36.05g, Eu 2 O 3 4.22g was mixed and thoroughly ground to obtain the first mixture; 3% by mass of the flux NH was added to the first mixture 4 After the Cl is mixed and fully ground, it is placed in an alumina crucible, and the crucible is placed in a tube furnace. 3 When the temperature is raised to 600℃~1000℃, the gas flow rate is ≥30ml / min; when the temperature is increased to 1000~1250℃, the gas flow rate is ≤20ml / min, and then sintered at 1250℃ for 3 hours and then cooled to obtain the precursor Sr 1.96 SiO 4 :0.04Eu;

[0030] Synthesized precursor Sr 1.96 SiO 4 : 0.04Eu is in the form of a block. After physically crushing it with an agate mortar, it is sieved with a 150-mesh sieve, and the sieved Sr 1.96 SiO 4 : 0.04Eu is prepar...

Embodiment 2

[0035] Example 2 Phosphor Sr 0.97 Si 2 O 2 N 2 : Preparation of 0.03Eu

[0036] 1) Forebody Sr 1.94 SiO 4 : Preparation of 0.06Eu

[0037] According to the forebody Sr 1.94 SiO 4 : 0.06Eu stoichiometric ratio, weigh SrCO 3 173.6g, SiO 2 36.42g, Eu 2 O 3 6.4g and 3wt% catalyst NH 4 After the Cl is mixed and fully ground, it is placed in an alumina crucible, and the crucible is placed in a tube furnace. 2 / H 2 When the temperature is raised to 600℃~1000℃, the gas flow rate is ≥30ml / min; when the temperature is increased to 1000℃~1300℃, the gas flow rate is ≤20ml / min, and then sintered at 1300℃ for 1 hour and then cooled to obtain the precursor Sr 1.94 SiO 4 :0.06Eu;

[0038] forebody Sr 1.94 SiO 4 : The steps of crushing and sieving of 0.06Eu are the same as in Example 1.

[0039] 2) Phosphor Sr 0.97 Si 2 O 2 N 2 : Preparation of 0.03Eu

[0040] According to Sr 0.97 Si 2 O 2 N 2 : 0.03Eu stoichiometric ratio, the Sr 1.94 SiO 4 : 0.03Eu Weigh 20g, an...

Embodiment 3

[0044] Example 3 Phosphor Sr 0.96 Si 2 O 2 N 2 : Preparation of 0.04Eu

[0045] 1) Body Sr 1.92 SiO 4 : Preparation of 0.08Eu

[0046] According to the forebody Sr 1.92 SiO 4 : 0.08Eu stoichiometric ratio, weigh SrCO 3 173.6g, SiO 2 36.796g, Eu 2 O 3 8.621g and 1% catalyst NH 4 Cl1%H 3 BO 3 , after mixing and fully grinding, put it in an alumina crucible, place the crucible in a tube furnace, and put it in a protective gas N 2 / H 2 When the temperature is raised to 600℃~1000℃, the gas flow rate is ≥30ml / min; when the temperature is increased to 1000℃~1300℃, the gas flow rate is ≤20ml / min, and then sintered at 1100℃ for 2 hours and then cooled to obtain the precursor Sr 1.92 SiO 4 :0.08Eu;

[0047] The steps of crushing and sieving of the precursor are the same as in Example 1.

[0048] 2) Phosphor Sr 0.96 Si 2 O 2 N 2 : Preparation of 0.04Eu

[0049] According to Sr 0.96 Si 2 O 2 N 2 : 0.04Eu stoichiometric ratio, the Sr 1.92 SiO 4 : 0.08Eu Weigh ...

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Abstract

The invention discloses a preparation method for small particle nitrogen oxide of green emitting phosphor, comprising the following steps of: firstly, synthesizing a precursor A(1-x)2BO4:2xRe of the nitrogen oxide of green emitting phosphor; and secondly, synthesizing the small particle nitrogen oxide of green emitting phosphor A1-xByOzN2 / 3+4 / 3y-2 / 3z:xRe, wherein the emission wavelength of the green emitting phosphor can be adjusted by adjusting the doping amount of Eu. The later physical crushing process is avoided. In addition, a relatively-mild ultrasound dispersion and water sedimentation method is adopted, thus the crystal completeness of powder particles can be maintained and the granularity of the powder meets the production requirement of an industrial LED (Light Emitting Diode) lamp.

Description

technical field [0001] The invention belongs to the technical field of fluorescent powder for LEDs, and relates to a preparation method of small-particle oxynitride green fluorescent powder. Background technique [0002] White light emitting devices can excite three primary color (red, green and blue) phosphors by using UV light emitting diodes (UV LEDs) as light sources, red and green phosphors by using blue LEDs as light sources, or by using blue LEDs as light sources However, the white light LED produced by this mode has the defects of low color rendering and high color temperature due to the lack of red components, which greatly limits its application field. One of the solutions that can be used to obtain white LEDs with high color rendering index and different color temperatures is to add red / green phosphors to blue chips. Therefore, it is necessary to develop green phosphors with excellent performance. [0003] Due to its unique excitation spectrum (excitation range c...

Claims

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Application Information

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IPC IPC(8): C09K11/64C09K11/59
Inventor 赵莉
Owner IRICO