Preparation method of yttrium aluminum garnet (YAG) nano-powder

A technology of yttrium aluminum garnet and nano-powder, which is applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of easy powder agglomeration, high equipment requirements, high raw material cost, etc., and achieve high sintering activity, Avoid reunion, low cost effect

Active Publication Date: 2013-07-24
SINOMA SYNTHETIC CRYSTALS CO LTD +1
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Problems solved by technology

The disadvantages of the solid phase reaction method are: impurities are easily introduced during the ball milling process and the raw materials are not easy to mix. At the same time, high-temperature calcination reduces the sintering activity of the powder, and it is impossible to obtain nano-scale powder.
The disadvantages of this method are: due to the difference in precipitation speed between different components, it is easy to cause different ions to precipitate successively, which makes it difficult to control the uniformity of the microscopic composition, and it is difficult to wash and filter the precipitate, and the powder is easy to agglomerate
Disadvantages of this technology are: high equipment requirements
[0007] Michael Veith et al (Michael Veith, et al, Low temperature synthesis of nanocrystalline Y 3 Al 5 o 12 (YAG) and Ce-doped Y 3 Al 5 o 12 via different sol-gel methods.J.Mater.Chem.,1999(12)3069-3079) to prepare YAG nanopowder by sol-gel method. The disadvantages of this method are: the cost of raw materials is high, and the main reason for the high cost is The reason is that the synthesis conditions of Y and other rare earth ion alkoxides are particularly harsh (moisture must be strictly controlled), the process is complex, and the synthesis yield is low; in addition, during the drying process of the gel, if the drying is not done properly, it is easy to cause powder Agglomeration, if not resolved immediately, will eventually evolve into hard agglomeration, thereby reducing the sintering activity of the powder

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[0030] A preparation method of yttrium aluminum garnet nano powder, comprising the following steps:

[0031] 1) Dissolve aluminum salt in isopropanol to obtain an aluminum solution with a mass concentration of 15-35 wt%; dissolve yttrium salt and / or acetate of other rare earth ions in deionized water to prepare a mass concentration of 15-35 wt%. The solution A of 25wt%; Wherein,

[0032] The molar ratio of the aluminum salt to the acetate of yttrium salt and / or other rare earth ions is 3:5, the weight and number ratio of the aluminum salt to isopropanol is 1:2 to 1:6, and the yttrium The weight and number ratio of the acetate of salt and / or other rare earth ions to deionized water is 1:3~1:6;

[0033] 2) Under the condition of vigorous stirring, add the aluminum solution dropwise to the solution A, and stir for 1 to 3 hours under the condition of 30-50°C to obtain the sol; then, under the condition of 60-80°C, continue to Stir for 1 to 3 hours to obtain a gel;

[0034] 3) T...

Embodiment 1

[0039] Take aluminum isopropoxide 102.12 grams and dissolve in 300ml isopropanol to form an aluminum solution, weigh yttrium acetate (molecular formula: Y(CH 3 COO) 3 4H 2 O) 101.43 g was dissolved in 600 ml deionized water to form a solution of yttrium. Under vigorous stirring, the above-mentioned aluminum solution was added dropwise to the yttrium solution, stirred at 40°C for 2 hours to form a sol, raised to 60°C and continued to stir for 3 hours to form a gel. The above gel was transferred to a freeze dryer, pre-frozen at -60°C for 12h, and dried at -60°C and 10Pa for 30h to obtain a loose precursor powder. The precursor powder was calcined at 900 °C for 2 h to obtain the final product. Its XRD spectrum is as figure 1 As shown, compared with the standard card JCPDS33-40, the position and relative intensity of the diffraction peaks are completely consistent, indicating that the product is a pure YAG phase. TEM photos such as figure 2 As shown, the average grain size ...

Embodiment 2

[0041] Take by weighing 102.12 grams of aluminum isopropoxide and dissolve in 600ml of isopropanol to form an aluminum solution, weigh 100.4157 grams of yttrium acetate (molecular formula: the same as Example 1), neodymium acetate (molecular formula: Nd(CH 3 COO) 3 ·H 2 O) 1.0181 g was dissolved in 400 ml of deionized water to form a mixed solution of yttrium and neodymium. Under vigorous stirring, the above-mentioned aluminum solution was added dropwise to the mixed solution of yttrium and neodymium, stirred at 45°C for 2h to form a sol, raised to 70°C and continued to stir for 2h to form a gel. The above gel was transferred to a freeze dryer, pre-frozen at -65°C for 8h, and dried at -65°C and 8Pa for 36h to obtain a loose precursor powder. The precursor powder was calcined at 1000°C for 2 hours, and finally Nd:YAG powder with Nd content of 1.0at% was obtained. Its XRD collection of patterns and TEM picture feature are with embodiment 1. The main technical indicators are ...

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Abstract

The invention relates to a preparation method of yttrium aluminum garnet (YAG) nano-powder. The preparation method comprises the steps of dissolving aluminum salt in isopropanol to prepare an aluminum solution, dissolving acetate of yttrium ions and/or other rare earth ions in deionized water to prepare a solution A, dropwise adding the aluminum solution to the solution A under the condition of vigorous stirring, executing the stages of collosol, gel, freeze drying and the like to form a precursor, and calcinating the precursor at a high temperature to form the YAG nano-powder. With the adoption of the preparation method, the YAG nano-powder which is small in particle size (30-110nm), high in sintering activity and uniform in doping can be prepared at lower cost and lower temperature (900-1100 DEG C).

Description

technical field [0001] The present invention relates to a kind of yttrium aluminum garnet (Y 3 al 5 o 12 , referred to as YAG) nano-powder preparation method, in particular to a combination of sol-gel and freeze-drying method for preparing YAG nano-powder, which belongs to the technical field of transparent ceramic preparation. Background technique [0002] YAG has the advantages of excellent optical properties and stable chemical properties, and is widely used as window materials and functional materials. Rare earth ion-doped YAG single crystal is an ideal laser material, which has been widely used in the field of laser technology and is an important matrix of all solid-state lasers. Compared with single crystals, YAG transparent ceramics have the advantages of simple preparation process, low cost, high-concentration doping, large-scale production, and multi-layer multifunctional composite structures, etc., and have become a research hotspot in recent years. Among them,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C04B35/44
Inventor 王海丽蒲瑞满沈德忠
Owner SINOMA SYNTHETIC CRYSTALS CO LTD
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