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Method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder

A doping technology of yttrium aluminum garnet and rare earth, which is applied in the field of laser ceramic materials, can solve the problems of unfavorable late molding and serious powder agglomeration, and achieve the effects of increasing molding density, good mechanical properties, and improving powder fluidity

Inactive Publication Date: 2011-05-18
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a kind of wet chemical method, coprecipitation method has the advantage of low cost, but the disadvantage is that the powder agglomeration is serious, which is not conducive to the later molding

Method used

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  • Method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder
  • Method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder
  • Method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] According to Nd 0.06 Y 2.94 al 5 o 12 Molecular formula, respectively weigh 11.5629g of Al(NO3)3, 6.8190g of Y(NO3)3, 0.1510g of Nd(NO3)3, and prepare a metal mother solution with a total metal ion concentration of 0.1mol / L, under stirring , dropwise into 0.5mol / L excess ammonium bicarbonate solution at a rate of 5ml / min, wherein the two solvents are ethanol-water system, aged for 36 hours, filtered with suction, washed 5 times with deionized water, and washed 2 times with alcohol , the obtained filter cake was dried at 50°C for 24 hours, pulverized and sieved, and the obtained precursor was calcined at 1200°C for 2 hours to obtain 2at% Nd:YAG powder. The powder X-ray diffraction pattern is shown in figure 1 , the transmission electron microscope photo see figure 2 .

[0027] Put 3.0000g of self-made 2at% Nd:YAG powder, 0.0150g of TEOS and 0.0300g of PVB into a high-purity agate ball mill jar, add 12g of high-purity agate balls, 6g of absolute ethanol, and mix for...

Embodiment 2

[0030] According to Nd 0.06 Y 2.94 al 5 o 12 Molecular formula, weigh 11.5629g of Al(NO3)3, 6.8190g of Y(NO3)3, and 0.1510g of Nd(NO3)3 respectively, and prepare a metal mother solution with a total metal ion concentration of 0.2mol / L. , was added dropwise to 1.0mol / L excessive ammonium bicarbonate solution at a speed of 5ml / min, wherein the two solvents were aged in ethylene glycol-water system for 24 hours, filtered with suction, washed with deionized water for 3 times, and washed with alcohol for 2 The second time, the obtained filter cake was dried at 55°C for 48 hours, crushed and sieved, and the obtained precursor was calcined at 1100°C for 3 hours to obtain 2at% Nd:YAG powder.

[0031] Put 3.0000g of homemade 2at% Nd:YAG powder, 0.0150g of TEOS and 0.0450g of PVB into a high-purity agate ball mill jar, add 12g of high-purity agate balls, 9g of absolute ethanol, and mix for 20 hours with a planetary ball mill. The resulting slurry was spray-dried with an inlet temper...

Embodiment 3

[0033] According to Nd 0.06 Y 2.94 al5 o 12 Molecular formula, respectively weigh 11.5629g of Al(NO3)3, 6.8190g of Y(NO3)3, 0.1510g of Nd(NO3)3, and prepare a metal mother solution with a total metal ion concentration of 0.5mol / L, under stirring , was added dropwise at a speed of 10ml / min to 2.0mol / L excessive ammonium bicarbonate solution, wherein the two solvents were isopropanol-water system and aged for 12 hours, filtered with suction, washed with deionized water for 5 times, and washed with alcohol for 2 The second time, the obtained filter cake was dried at 60°C for 24 hours, crushed and sieved, and the obtained precursor was calcined at 1200°C for 3 hours to obtain 2at% Nd:YAG powder.

[0034] Put 3.0000g of homemade 2at% Nd:YAG powder, 0.0150g of TEOS and 0.0450g of PVB into a high-purity agate ball mill jar, add 12g of high-purity agate balls, 7.5g of absolute ethanol, and mix for 20 hours using a planetary ball mill . The resulting slurry was spray-dried with an ...

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Abstract

The invention relates to a method for preparing rare earth doped yttrium aluminum garnet transparent ceramics by utilizing spray granulation modified powder. The method is characterized in that an alcohol-water system is adopted as a solvent and comprises the following steps: preparing rare earth doped Re to yttrium aluminum garnet(YAG) powder through a coprecipitation method; modifying the powder by adopting a spray granulation process; carrying out the molding through the mode combining dry pressing and cold isostatic pressing; preparing the rare earth doped Re to YAG transparent ceramics through degreasing, vacuum sintering, annealing treatment, plane grinding and polishing; modifying the powder through a spray granulation process, namely carrying out the ball grinding on the prepared Re to YAG transparent ceramics, a ball grinding medium and surfactants such as a sintering auxiliary, an adhesive, a plasticizer, a dispersant and the like; carrying out the twice granulation on the slurry obtained by the ball grinding through a spray drying method, and preparing powder after being modified into solid spherical granules or similar spherical granules. The modified powder has good dispersity, enhances the fluidity of the powder, is easy to mold, has the granule-stage proportion, greatly enhances the density of the biscuit and is beneficial to sintering at the later stage..

Description

technical field [0001] The invention relates to a method for preparing rare earth-doped yttrium aluminum garnet transparent ceramics by spraying and granulating modified powder, and belongs to the field of laser ceramic materials. Background technique [0002] Yttrium aluminum garnet (Y 3 al 5 o 12 , yttrium aluminum garnet, YAG) belongs to the cubic crystal system, has a garnet structure, and the space group is O h (10)-I a 3d, each unit cell contains 8 compounds, which has the characteristics of optical isotropy, no birefringence effect, low temperature creep, good chemical stability, etc., and the cubic structure of YAG is also conducive to the generation of narrow fluorescence spectrum , so as to achieve high-gain, low-threshold laser operation, after doping trivalent rare earth ions, no charge compensation is required, so Nd:YAG is currently the only practical solid working substance that can work continuously at room temperature. At present, the YAG laser material...

Claims

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Application Information

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IPC IPC(8): C04B35/44C04B35/50C04B35/622
Inventor 刘媛曹永革郭旺黄秋凤黄志
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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