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A method for preparing silicon-aluminum nitride or nitrogen oxide phosphor

A technology of nitrogen oxides and nitrides, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as operability, low stability and repeatability, complex control factors such as solubility ratio, complex chemical reaction process, etc. , to achieve the effect of ensuring uniformity and stability, good crystallization and simple process

Active Publication Date: 2018-12-18
QINGDAO CUP NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese Patent Authorization Announcement No. CN101857441 B discloses a method for preparing b-silicon nitride powder. The method uses a foaming method to prepare a porous green body for combustion synthesis. It triggers the organic matter in the slurry by adding an initiator and catalyst. The monomer and the cross-linking agent undergo a cross-linking reaction to solidify the powder particles. After evaporating the solvent, a porous green body is obtained, while a large amount of high-molecular organic matter remains in the green body. This patent is through the generation of chain-like high-molecular organic matter To stabilize the porous structure, the inventors found that during the combustion synthesis process, a large amount of organic carbonization and evaporation will seriously affect the effective doping of rare earth ions in the synthesis process. In addition, the chemical reaction process is complicated, such as pH value adjustment, machine monomer, The control factors such as cross-linking agent, initiator, and catalyst solubility ratio are complex, so the operability, stability, and repeatability are low, and it is not suitable for industrial applications

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  • A method for preparing silicon-aluminum nitride or nitrogen oxide phosphor
  • A method for preparing silicon-aluminum nitride or nitrogen oxide phosphor
  • A method for preparing silicon-aluminum nitride or nitrogen oxide phosphor

Examples

Experimental program
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Effect test

Embodiment 1

[0044] A method for preparing silicon-aluminum nitride or oxynitride fluorescent powder, the steps of the method are as follows:

[0045] (1) According to the general chemical formula: Ca Si Al ON: xEu, where the value of m is 3.5, the value of n is 0.5, and x=0.08, the raw materials are weighed. The raw material powder is Si powder, particle size D50=5um; a-Si N powder, particle size D=1um; Al powder, particle size D=5um; AlN powder, particle size D=1um; CaO powder, particle size D=5um; Ca N powder , particle size D=5um; Eu O powder, particle size D=1um; wherein the mass ratio of Si powder to a-SiN powder is 0.65, and the mass ratio of Al powder to AlN powder is 2.6;

[0046] (2) PVB binder weighing 1% of raw material powder gross mass;

[0047] (3) Add raw material powder and binder into tert-butanol solvent, the volume ratio of raw material powder and tert-butanol is 15:85, use planetary ball mill and nitrogen protection ball mill for 2 hours, and obtain mixed uniform slur...

Embodiment 2

[0051] A method for preparing silicon-aluminum nitride or oxynitride fluorescent powder, the steps of the method are as follows:

[0052] (1) According to the general chemical formula: Si Al ON: xEu, where Z is 0.5 and x is 0.03, weigh the raw materials; the raw material powder is Si powder, particle size D=5um; a-Si N powder, particle size D=1um; AlO powder, particle size D=5um; AlN powder, particle size D=1um; EuO powder, particle size D=1um; wherein the mass ratio of Si powder to a-Si N powder is 2.3;

[0053] (2) PVB binder weighing 0.2% of raw material powder gross mass;

[0054] (3) Add the raw material powder and binder into the tert-butanol solvent, the volume ratio of the raw material powder and tert-butanol is 3:7, use a planetary ball mill to mill for 8 hours under the protection of nitrogen, and obtain a mixed homogeneous slurry material;

[0055] (4) Pour the obtained slurry into a mold and freeze and solidify it in an ethanol low-temperature bath at -60°C for 2...

Embodiment 3

[0058] A method for preparing silicon-aluminum nitride or oxynitride fluorescent powder, the steps of the method are as follows:

[0059] (1) According to the general chemical formula: Al Si Eu N, where y is 0.03 and x is 0.003, the raw material is weighed; the raw material powder is Al powder, particle size D=5um; AlN powder, particle size D=1um; Si powder, Particle size D=5um; EuO powder, particle size D=1um; wherein the mass ratio of Al powder to AlN powder is 3:2;

[0060] (2) PVB binding agent weighing 0.5% of raw material powder gross mass;

[0061] (3) Add raw material powder and binder into tert-butanol solvent, the volume ratio of raw material powder and tert-butanol is 1:4, use planetary ball mill to mill for 8 hours under the protection of nitrogen, and obtain mixed homogeneous slurry material;

[0062] (4) Pour the obtained slurry into a mold and freeze and solidify it in an ethanol low-temperature bath at -40°C for 2 hours; place the solidified green body in a f...

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Abstract

The invention belongs to the technical field of fluorescent powder preparation, particularly relates to a method for freeze drying and auxiliary combustion synthesis of silicon-aluminum nitride or oxynitride fluorescent powder, and is characterized in that the method is implemented according to the following steps: (1) weighing raw material powder and a PVB binder according to the stoichiometric proportion of a fluorescent material; (2) adding the raw material powder and the binder to a tertiary butanol solvent, and carrying out ball milling, to obtain an evenly mixed slurry; (3) freezing and curing the obtained slurry for 2 h to 6 h; (4) placing the cured blank in a freezing dryer, carrying out vacuum drying to obtain a porous blank; and (5) placing the porous blank in a combustion synthesis reaction kettle, placing a Ti powder on the upper surface of the front end of the blank to be used as an igniting agent, vacuumizing, then filling nitrogen gas, and triggering the blank to carry out combustion synthesis reaction. The prepared silicon-aluminum nitride or oxynitride fluorescent powder has the advantages of uniform particle size distribution and good crystallization, allows the product to have no sintering agglomeration phenomenon, has no need for a subsequent crushing treatment process, and has significant advantages in preparation cost.

Description

technical field [0001] The invention belongs to the technical field of fluorescent powder preparation, and in particular relates to a method for synthesizing silicon-aluminum nitride or nitrogen oxide fluorescent powder with freeze-drying assisted combustion. Background technique [0002] Silicon-aluminum nitride or oxynitride phosphors have a very rich crystal structure. By changing the local crystal structure around the active ion, the energy level of the active ion can be split by crystal field, so as to obtain near-ultraviolet and blue light excitation and rich The emission spectrum, including red, green, yellow, and blue luminescence, has attracted great attention from the scientific and industrial circles. [0003] At present, the synthesis and preparation methods of silicon-aluminum nitride or nitrogen oxide phosphor mainly include high-temperature solid-state reaction method, gas phase reduction nitriding method, carbothermal reduction nitriding method, direct nitrid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/64C09K11/80
CPCC09K11/0883C09K11/7721C09K11/7728C09K11/7734C09K11/7749
Inventor 葛一瑶袁轩一邹艺峰陈克新
Owner QINGDAO CUP NEW MATERIALS CO LTD
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