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Gel burning synthetic method for preparing reodymium doped gadolinium-gallium garnet nano powder

A technology of combustion synthesis and garnet, applied in the field of preparation of artificial crystals and ceramic materials, can solve the problems of difficult to pioneer powder, particle agglomeration, difficult to control pH value, etc., and achieve narrow particle size distribution, uniform dispersion, raw material cost and operation. low cost effect

Inactive Publication Date: 2006-11-08
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of polycrystalline Nd:GGG powder by co-precipitation method also has some disadvantages: (1) due to the difference in solubility product and sedimentation rate, it is difficult to form a precursor powder with precise stoichiometric ratio and uniform composition; (2) it is difficult to control the appropriate The pH makes Gd +3 , Ga +3 、Nd +3 Complete precipitation at the same time; (3) The rinsing and drying process of the powder obtained by the co-precipitation method may lead to the formation of particle agglomeration

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] When x=0.09, according to the chemical formula Nd 0.09 Gd 2.91 Ga 5 o 12 , take 2.500g gallium nitrate (or take 0.682g metal gallium and dissolve in 29.3ml of dilute nitric acid solution with a concentration of 1.0mol / L), 1.953g gadolinium nitrate (or get 0.895g metal gadolinium and dissolve in 17.1ml with a concentration of 1.0mol / L dilute nitric acid solution), 0.058g neodymium nitrate, 6.574g citric acid, dissolved in 80ml deionized water, and stirred to form a uniform solution. Put it in a constant temperature water bath, keep the temperature of the water bath at 80°C and keep stirring, a yellow transparent viscous gel will be formed after several hours. Put the gel into a drying oven with the temperature controlled at 200°C, and finally form a black, fluffy precursor through combustion and heat release. The precursor was repeatedly ground in an agate mortar, then loaded into a quartz crucible, and calcined at 900°C for two hours to obtain white neodymium-doped ...

Embodiment 2

[0019] When x=0.12, according to the chemical formula Nd 0.12 Gd 2.88 Ga 5 o 12 , Take 5.000g gallium nitrate, 3.865g gadolinium nitrate, 0.118g neodymium chloride, 5.350g carbohydrazide, dissolve in 120ml isopropanol, stir to form a uniform solution. Put it in a constant temperature water bath, keep the temperature of the water bath at 60°C and keep stirring, a yellow transparent viscous gel will be formed after several hours. Put the gel into a drying oven with the temperature controlled at 220°C, and finally form a black, fluffy precursor through combustion and heat release. The precursor was repeatedly ground in an agate mortar, then loaded into a quartz crucible, and calcined at 900°C for two hours to obtain white neodymium-doped gadolinium-gallium garnet nanopowder with an average particle size of 30 nm. In this embodiment, the ratio of the molar ratio of the added organic fuel carbohydrazide to the sum of the moles of metal ions contained in the mixed solution is 1....

Embodiment 3

[0021] When x=0.18, according to the chemical formula Nd 0.18 Gd 2.82 Ga 5 o 12 , get 6.209g gallium nitrate (or get 2.276g digallium trioxide dissolved in 14.5ml concentration of dilute nitric acid solution of 5.0mol / L), 4.700g gadolinium nitrate (or get 3.330g digadolinium trioxide dissolved in 11.0ml concentration of 5.0mol / L dilute nitric acid solution), 0.289g neodymium nitrate, 6.410g glycine, dissolved in 200ml absolute ethanol, and stirred to form a uniform solution. Put it in a constant temperature water bath, keep the temperature of the water bath at 60°C and keep stirring, a yellow transparent viscous gel will be formed after several hours. Put the gel into a drying oven with the temperature controlled at 200°C, and finally form a black, fluffy precursor through combustion and heat release. The precursor was repeatedly ground in an agate mortar, then loaded into a quartz crucible, and calcined at 1100°C for two hours to obtain white neodymium-doped gadolinium-ga...

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Abstract

The gel burning synthesis process of preparing neodymium doped gadolinium-gallium garnet includes the following steps: mixing Nd compound, Gd compound and Ga compound in the molar ratio of Nd, Gd and Ga in X to 3-X to 5, where X is 0-0.3 to form mixture solution; adding organic fuel citric acid, amino acid, urea, tartaric acid and / or hydrazine carbonate to the mixture solution; evaporating to dewater the solution at 60-80 deg.c in a water bath to obtain viscose gel; burning the viscose gel to produce exothermal reaction at 160-220 deg.c and normal pressure to obtain black puffy precursor; grinding; and calcining at 900-1100 deg.c to obtain the neodymium doped gadolinium-gallium garnet powder. The present invention has the advantages of ion level homogeneous mixing, short preparing process, low temperature, superfine product granularity, homogeneous dispersivity and homogeneous chemical components.

Description

technical field [0001] The invention belongs to the field of preparation of artificial crystals and ceramic materials, in particular to a gel combustion synthesis method for preparing neodymium-doped gadolinium-gallium garnet nanopowder. Background technique [0002] GGG is the abbreviation of gadolinium gallium garnet, its chemical formula is Gd 3 Ga 5 o 12 , by Gd 2 o 3 with Ga 2 o 3 A complex oxide formed, belonging to the cubic crystal system, with a garnet structure. The density of GGG crystals is 7.09g / cm 3 , the melting point is 1720°C, the Mohs hardness is 7.5, the lattice constant is 12.383 Ȧ, and the thermal expansion coefficient is 9.03×10 -6 / °C. The most important use of GGG crystals is as a laser matrix material. Nd-doped GGG (Nd:GGG) crystals and Nd:GGG transparent ceramics are key materials for all-solid-state high-efficiency high-power heat capacity lasers. [0003] Polycrystalline Nd:GGG powder is the initial raw material for Nd:GGG single crystal...

Claims

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Application Information

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IPC IPC(8): C04B35/50C04B35/65
Inventor 胡章贵李先学李江涛
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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