Method for preparing rare earth-doped yag nano-powder by partial liquid phase precipitation method

A yttrium aluminum garnet and rare earth doping technology is applied in chemical instruments and methods, rare earth metal compounds, alumina/aluminum hydroxide, etc., and can solve the problems of high cost, poor powder dispersion, and unfavorable large-scale production, etc. Achieve the effect of facilitating washing, high light-to-light conversion efficiency, and avoiding aluminum loss

Active Publication Date: 2008-11-12
SHANDONG UNIV
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Problems solved by technology

[0006] People such as Michael Veith propose sol-gel method (referring to J.Mater.Chem., 1999 (12) 3069-3079), but the preparation process of metal alkoxide is complicated, and cost is high, is unfavorable for 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.
[0007] The combustion method is difficult to control the shape and size of the product due to the violent and explosive nature of the reaction

Method used

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  • Method for preparing rare earth-doped yag nano-powder by partial liquid phase precipitation method
  • Method for preparing rare earth-doped yag nano-powder by partial liquid phase precipitation method
  • Method for preparing rare earth-doped yag nano-powder by partial liquid phase precipitation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: 2%Nd: the ammonium oxalate reverse drip method synthesis of YAG nanopowder

[0035] This batch of Al was measured by thermogravimetric experiment 2 o 3 The aluminum element in the powder is converted into pure Al 2 o 3 95.305%, 5N purity Y 2 o 3 Coarse powder is dissolved in high-purity concentrated nitric acid in a 90°C water bath to prepare 1mol / L Y(NO 3 ) 3 solution, 5N purity Nd 2 o 3 Dissolve in dilute nitric acid to make 0.5mol / L Nd(NO 3 ) 3 .

[0036] 1. Add 0.002g PVP to 40ml of 1mol / L ammonium oxalate (pH=4), mix well, weigh 1.337gAl 2 o 3 Powder. Add it into the mixture, ultrasonically disperse for 30 minutes, and stir in a water bath at 40°C with strong magnetic force to form a uniform suspension.

[0037] 2. Measure 14.7ml of 1mol / L Y(NO 3 ) 3 and 0.6ml of 0.5mol / L Nd(NO 3 ) 3 , diluted to 50ml with deionized water, mixed evenly and added dropwise to the above suspension at a rate of 4ml / min, and then continued to stir and age...

Embodiment 2

[0040] Embodiment 2: 2%Nd: the ammonium oxalate positive drop method synthesis of YAG nanopowder

[0041] 1. Measure 14.7ml of 1mol / L Y(NO 3 ) 3 and 0.6ml of 0.5mol / L Nd(NO 3 ) 3 , diluted to 50ml with deionized water, added 0.01mL oleic acid, mixed well, weighed 1.337gAl 2 o 3 Powder (this batch of Al was measured by thermogravimetric experiment 2 o 3 The aluminum element in the powder is converted into pure Al 2 o 3 is 95.305%). Add it into the mixture, ultrasonically disperse for 30min, and then stir strongly with magnetic force to form a uniform suspension.

[0042] 2. Measure 25ml of 1mol / L ammonium oxalate (PH=4), add it dropwise at a rate of 2ml / min into the above high-intensity stirred suspension, and continue to stir and age for 12 hours.

[0043] 3. After aging, filter and wash with a vacuum filtration device, wash with deionized water for 3 times, and wash with absolute ethanol for 2 times.

[0044] 4. Under normal pressure, dry the precipitate filter cak...

Embodiment 3

[0045] Embodiment 3: 2%Nd: the ammonium bicarbonate back-drop method synthesis of YAG nanopowder

[0046] This batch of Al was measured by thermogravimetric experiment 2 o 3 The aluminum element in the powder is converted into pure Al 2 o 3 95.305%, 5N purity Y 2 o 3 Coarse powder is dissolved in high-purity concentrated nitric acid in a 90°C water bath to prepare 1mol / L Y(NO 3 ) 3 solution, 5N purity Nd 2 o 3 Dissolve in dilute nitric acid to make 0.5mol / L Nd(NO 3 ) 3

[0047] 1. To 60ml of 2mol / L NH 4 HCO 3 Add 0.001g of PVP, mix well, weigh 1.337g of light Al 2 o 3 . Add it into the mixture, ultrasonically disperse for 30 minutes, and stir strongly at room temperature to form a uniform suspension.

[0048] 2. Measure 14.7ml of 1mol / L Y(NO 3 ) 3 and 0.6ml of 0.5mol / L Nd(NO 3 ) 3 , diluted to 50ml with deionized water, mixed evenly and added dropwise to the above suspension at a rate of 4ml / min, and then continued to stir and age for 12 hours.

[0049] 3....

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Abstract

The invention relates to a method for preparing a rare earth doped yttrium aluminum garnet nanometer powder body by a partial liquid phase precipitation method. Y(NO3)3 and Al2O3 are used to synthesize the yttrium aluminum garnet nanometer powder body; and Nd, Yb, Cr and other rare earth elements are used for ion doping. Ammonium oxalate, NH4HCO3 or urea is adopted as a precipitant. Sediment is aged, fully washed, dried and calcined for 15 to 120 minutes at a temperature of between 1000 and 1600 DEG C under the aerobic condition, thereby acquiring the rare earth doped YAG powder body with a grain diameter between 80 to 200 nm. The method can realize the uniform doping of the rare earth elements, also avoid forming a colloidal substance which is unfavorable for washing, and prepare the rare earth doped YAG nanometer powder body material in high efficiency.

Description

Technical field [0001] The present invention relates to a method for preparing rare earth-doped YAG nanopowder, in particular to a partial liquid phase precipitation method that combines a suspension method and a precipitation method, and belongs to the technical field of laser ceramic preparation. Background technique [0002] YAG is the abbreviation of yttrium aluminum garnet, its chemical formula is Y 3 Al 5 O 12 , is determined by Y 2 O 3 and Al 2 O 3 A complex oxide eutectic solution formed, belonging to the cubic crystal system and having a garnet structure. YAG has excellent optical properties and stable chemical properties. Its rare earth-doped single crystal has been widely used in laser technology and is the most commonly used laser crystal for all-solid-state lasers. However, due to the limitations of doping concentration and growth size limitations of single crystals, with the improvement and application of ceramic technology, YAG ceramic materials have be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/02C01F17/00C04B35/44C04B35/50
Inventor 王继扬桑元华吕耀辉刘宏
Owner SHANDONG UNIV
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