Method for preparation of silicon-aluminum nitride or oxynitride fluorescent powder

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: 2016-07-20
QINGDAO CUP NEW MATERIALS CO LTD
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Problems solved by technology

Chinese Patent Authorization Announcement No. CN101857441B discloses a method for preparing b-silicon nitride powder. The method uses a foaming method to prepare a porous green body for combustion synthesis. The body and the cross-linking agent undergo a cross-linking reaction to solidify the powder particles. After evaporating the solvent, a porous body is obtained, while a large amount of high-molecular organic matter remains in the green body. This patent is to generate 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, exchange The control factors such as the solubility ratio between the coupling agent, the initiator, and the catalyst are complicated, so the operability, stability, and repeatability are low, and it is not suitable for industrial applications.

Method used

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  • Method for preparation of silicon-aluminum nitride or oxynitride fluorescent powder
  • Method for preparation of silicon-aluminum nitride or oxynitride fluorescent powder
  • Method for preparation of silicon-aluminum nitride or oxynitride fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0045] (1) According to the general chemical formula: CaSiAlON: xEu, where m value is 3.5, n value is 0.5, and x=0.08, the raw materials are weighed. The raw material powder is Si powder, particle size D50=5um; a-SiN powder, particle size D=1um; Al powder, particle size D=5um; AlN powder, particle size D=1um; CaO powder, particle size D=5um; CaN powder, particle size D=5um; EuO powder, particle size D=1um; 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) Weigh the PVB binder of 1% of the total mass of the raw material powder;

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

Embodiment 2

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

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

[0053] (2) Weighing the PVB binder of 0.2% of the total mass of the raw material powder;

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

[0055] (4) Pour the obtained slurry into a mold and place it in a low temperature bath of -60°C ethanol to freeze and solidify for 2 hours; place th...

Embodiment 3

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

[0059] (1) According to the general chemical formula: AlSiEuN, where y is 0.03 and x is 0.003, weigh the raw materials; 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; The mass ratio of Al powder to AlN powder is 3:2;

[0060] (2) Weighing the PVB binder of 0.5% of the total mass of the raw material powder;

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

[0062] (4) Pour the obtained slurry into a mold and place it in a low temperature bath of -40°C ethanol to freeze and solidify for 2 hours; place the solidified body in a freeze dryer for vacuum d...

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

Claims

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Application Information

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