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A method of adding ammonium citrate to prepare nanoscale yttrium aluminum garnet powder

A technology of yttrium aluminum garnet and ammonium citrate, which is applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problem of uneven grain size distribution of YAG powder, hinder the application of sol-gel method, and cause china Uneven density and other problems, to achieve the effect of uniform grain size distribution, uniform density, and easy uniform mixing

Active Publication Date: 2015-09-02
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

L.Yang et al. (L.Yang, T.C.Lu, H.Xu, N.Wei, synthesis of YAG powder by the modified sol–gel combustion method, J.Alloys.Compd.484(2009) 449–451) reported Using citric acid monohydrate as the chelating agent and alcohol instead of deionized water as the solvent can reduce the powder agglomeration after mixing and stirring, but the agglomeration phenomenon of the YAG powder prepared by this method is still serious and the dispersibility is poor, and the YAG powder prepared by this method The grain size distribution of the body is not uniform
This will lead to uneven density of the green body after the YAG powder is formed, and the transparency of the ceramics obtained by sintering is not high, which hinders the application of the sol-gel method in the field of YAG polycrystalline ceramics

Method used

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  • A method of adding ammonium citrate to prepare nanoscale yttrium aluminum garnet powder
  • A method of adding ammonium citrate to prepare nanoscale yttrium aluminum garnet powder
  • A method of adding ammonium citrate to prepare nanoscale yttrium aluminum garnet powder

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Experimental program
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Effect test

Embodiment 1

[0031] In this embodiment, the preparation method of nanoscale yttrium aluminum garnet powder is as follows:

[0032] (1) Preparation of raw material mixture

[0033] Weigh 0.015mol Y(NO 3 ) 3 ·6H 2 O, 0.025mol Al(NO 3 ) 3 9H 2 O, 0.04mol anhydrous citric acid (C 6 h 8 o 7 ) and 0.04mol ammonium citrate (C 6 h 17 N 3 o 7 ), they were added to 200mL of absolute ethanol and mixed evenly to form a raw material mixture.

[0034] (2) Preparation of sols and gels

[0035] Heat the raw material mixture to 60°C at a stirring speed of 100rpm and keep stirring at this temperature, so that the raw material mixture turns into a white slurry, see figure 1 (a), the probe of the pH meter is placed in the white slurry to test the change of pH value of the white slurry for 1h thereafter (read the pH value once every 3min), and the test results are as follows figure 2 As shown in (a), the white slurry finally turned into a sol under stirring conditions, and then the resulting sol ...

Embodiment 2

[0061] In this embodiment, the preparation method of nanoscale yttrium aluminum garnet powder is as follows:

[0062] (1) Preparation of raw material mixture

[0063] Weigh 0.03mol YCl 3 ·6H 2 O, 0.05mol AlCl 3 ·6H 2 O, 0.08mol anhydrous citric acid (C 6 h 8 o 7 ) and 0.12mol ammonium citrate (C 6 h 17 N 3 o 7 ), they were added to 320mL of absolute ethanol and mixed evenly to form a raw material mixture.

[0064] (2) Preparation of sols and gels

[0065] The raw material mixture was heated to 60°C at a stirring speed of 90rpm and kept at this temperature to continue stirring, so that the raw material mixture was transformed into a white slurry, and continued stirring was used to transform the white slurry into a sol. Heating to 100°C under stirring speed and maintaining the temperature to continue stirring to transform the sol into a transparent gel.

[0066] (3) Roasting

[0067] The transparent gel was heated to 160°C and kept at this temperature until no smok...

Embodiment 3

[0069] In this embodiment, the preparation method of nanoscale yttrium aluminum garnet powder is as follows:

[0070] (1) Preparation of raw material mixture

[0071] Weigh 0.045mol Y(NO 3 ) 3 ·6H 2 O, 0.075mol Al(NO 3 ) 3 9H 2 O, 0.12mol anhydrous citric acid (C 6 h 8 o 7 ) and 0.216mol ammonium citrate (C 6 h 17 N 3 o 7 ), they were added to 720mL of absolute ethanol and mixed evenly to form a raw material mixture.

[0072] (2) Preparation of sols and gels

[0073] The raw material mixture was heated to 70°C at a stirring speed of 110rpm and kept at this temperature to continue stirring, so that the raw material mixture was transformed into a white slurry, and continued stirring was used to transform the white slurry into a sol, and then the resulting sol was mixed at 110rpm Heat to 110° C. under stirring speed and keep stirring at this temperature to transform the sol into a transparent gel.

[0074] (3) Roasting

[0075] The transparent gel was heated to 18...

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Abstract

The invention relates to a method for preparing nano-scale yttrium aluminum garnet powder by adding ammonium citrate. The process comprises the following steps: (1) adding yttrium salt, aluminum salt, ammonium citrate and anhydrous citric acid into anhydrous alcohol and uniformly mixing to form raw material mixed solution; (2) heating the raw material mixed solution to 60-80 DEG C under stirring, stirring continuously at the temperature to change the raw material mixed solution into sol, then heating the obtained sol to 90-130 DEG C under stirring and continuously stirring at the temperature to convert the sol into transparent gel; (3) heating the transparent gel to 150-200 DEG C, preserving heat and stopping heating until no smoke is produced, then grinding the obtained fluffy blocky materials into powder, baking the powder at 50-700 DEG C under normal pressure for 1-2 hours, and then baking precursor powder at 800-1,000 DEG C under normal pressure for 2-4 hours to obtain the nano-scale yttrium aluminum garnet powder.

Description

technical field [0001] The invention belongs to the field of preparation methods of yttrium aluminum garnet powder, and relates to a method for preparing nanoscale yttrium aluminum garnet powder by adding ammonium citrate. Background technique [0002] Yttrium aluminum garnet (chemical formula Y 3 al 5 o 12 , referred to as YAG) belongs to the cubic crystal system, has excellent optical properties, high temperature stability and creep resistance, and is a good solid-state laser matrix material. YAG single crystal is widely used as the basic material of laser and other light emitting materials due to its excellent optical properties and stable chemical properties. Compared with the YAG single crystal prepared by the traditional process, the polycrystalline YAG ceramics prepared by YAG nanopowder has a simple preparation process, low cost, easy to control the size and shape of the required product, and can achieve the same optical quality as the single crystal. And mechani...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00C04B35/44C04B35/626B82Y30/00
Inventor 卢铁城陈兴涛黎峰魏念江芬芬
Owner SICHUAN UNIV
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