Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying

A technology of spray freeze-drying and yttrium aluminum garnet, which is applied in the direction of drying solid materials, drying solid materials without heating, drying, etc., can solve the problems of high cost, poor powder dispersibility, and difficult washing of precursor gel. Achieve the effect of avoiding tediousness, simple steps, and achieving uniform doping

Inactive Publication Date: 2011-09-07
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Michael Veith and others proposed the sol-gel method (see J. Mater. Chem., 1999(12) 3069-3079), but the preparation process of metal alkoxide is complicated and costly, which is not conducive to large-scale production
The reaction process is not easy to control, and the prepared YAG precursor gel is difficult to wash, and it is easy to form secondary particles during drying. The precursor will produce hard agglomeration during heat treatment, which makes the dispersibility of the final prepared powder poor and the sintering activity is not ideal.
[0008] The combustion method is an improved type of the sol-gel method. Due to the violent and explosive nature of the reaction, the shape and size of the product are difficult to control.

Method used

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  • Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying
  • Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying
  • Method for preparing neodymium-doped yttrium aluminum garnet micro/nano powder by spray freeze-drying

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Nd:YAG powder was prepared by spray freeze-drying using nitrate as raw material.

[0027] (1) Dissolve aluminum nitrate, yttrium nitrate and neodymium nitrate in deionized water, the cation concentration is 1mol / L, and the ion ratio can be used to obtain the compound Nd 0.03 Y 2.97 Al 5 o 12 , adjust the pH value of the mixed ionic liquid to about 4 with ammonia water.

[0028] (2) Spray the uniformly mixed solution into a refrigerant mixed with liquid nitrogen and liquid ethane at a ratio of 1:2 to produce a frozen product, and vacuum freeze-dry the frozen product at -20°C for more than 20 hours to sublimate the water in the product Disappears, powder looks fluffy due to less sublimation of moisture.

[0029] (3) The fluffy powder obtained in step (2) was quickly put into a tube furnace with an initial temperature of 80°C, and calcined at 800°C for 2 hours under an oxygen atmosphere.

[0030] (4) Through XRD test, the powder is amorphous phase.

Embodiment 2

[0031] Embodiment 2: Same as Embodiment 1, except that the calcination condition is calcination at 850° C. for 2 hours.

[0032] The results of XRD prove that the Nd:YAG powder obtained under this condition is a pure phase with good crystallinity! SEM showed particles smaller than 20nm (see figure 2 ).

Embodiment 3

[0033] Embodiment 3: Same as Embodiment 1, except that the calcination condition is calcination at 900° C. for 2 hours.

[0034] The results of XRD prove that the Nd:YAG powder obtained under this condition is a pure phase, and the crystallinity is higher than that of the powder calcined at 850°C!

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Abstract

The invention discloses a method for preparing neodymium-doped yttrium aluminum garnet micro / nano powder by spray freeze-drying, which comprises the following steps: dissolving soluble salts of yttrium, aluminum and neodymium, which are used as raw materials; mixing the raw materials according to the stoichiometric proportion; and by using ammonia water or acetic acid as a pH regulator and the mixture of liquid nitrogen and liquid ethane as a freezing agent, granulating by spray freeze-drying, and calcining to obtain the uniform neodymium-doped yttrium aluminum garnet micro / nano powder. The method disclosed by the invention is simple, has the advantage of low cost, and can be used for scale-up production of the raw material of rare-earth-doped transparent ceramics.

Description

technical field [0001] The invention relates to a method for preparing YAG (yttrium aluminum garnet) micronano powder, in particular to a method for preparing neodymium-doped yttrium aluminum garnet micronano powder by spray freeze drying, which belongs to the preparation of transparent laser ceramics technology field. Background technique [0002] YAG is the abbreviation of yttrium aluminum garnet, its chemical formula is Y 3 Al 5 o 12 , by Y 2 o 3 and Al 2 o 3 A complex oxide co-solution is formed, which belongs to the cubic crystal system and has a garnet structure. YAG has excellent optical properties and stable chemical properties. Its rare earth-doped single crystal crystal has been widely used in laser technology, and it is the most widely used laser crystal in all solid-state lasers. However, due to the shortcomings of single crystals such as doping concentration limitations and growth size limitations, with the improvement and application of ceramic technolo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/44C04B35/50C04B35/626F26B5/06
Inventor 刘宏桑元华秦海明吕耀辉王继扬
Owner SHANDONG UNIV
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