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Preparation method of yttrium aluminium garnet doped transparent laser ceramics

A technology of yttrium aluminum garnet and transparent ceramics, which is applied in the field of preparation of transparent laser ceramics doped with yttrium aluminum garnet, can solve the problems of poor sintering activity of powder, high sintering temperature of transparent ceramics, and high preparation cost, and achieve high sintering activity and dispersibility, overcome the dependence on raw materials, and reduce production costs

Active Publication Date: 2013-02-06
北京雷生强式科技有限责任公司
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  • Abstract
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Problems solved by technology

[0008] ① This method uses commercially available high-purity (above 4N) Y 2 o 3 、Al 2 o 3 and other rare earth (Re) oxide powders as raw materials, although the cost is relatively low, it is highly dependent on the particle size, particle distribution, sintering activity, purity and other properties of commercially available raw materials, and commercially available commercial powders are mainly calcined Preparation method, the sintering activity of the powder is poor, resulting in high sintering temperature of transparent ceramics, it is difficult to sinter high optical quality transparent ceramics;
[0012] This method uses commercial oxide powder as raw material, and there is a problem of great dependence on raw materials
However, the preparation of Re:YAG powder by wet chemistry also has the problems of complex process, difficult control, and difficulty in large-scale production.
Moreover, this method requires expensive hot isostatic pressing equipment, and the preparation cost is relatively high

Method used

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  • Preparation method of yttrium aluminium garnet doped transparent laser ceramics
  • Preparation method of yttrium aluminium garnet doped transparent laser ceramics
  • Preparation method of yttrium aluminium garnet doped transparent laser ceramics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Weigh 78.62g of Y (NO 3 ) 3 ·6H 2 O, dissolved in deionized water to form 0.1mol L -1 Y(NO 3 ) 3 solution. Take 118.58g of ammonium bicarbonate with a purity better than 99.9%, dissolve it in a mixed solution composed of deionized water and absolute ethanol at a volume ratio of 1:1, and form a concentration of 0.2mol L -1 Ammonium bicarbonate alcoholic aqueous solution, add (NH 4 ) 2 SO 4 (ammonium sulfate and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 1:2) as a dispersant to obtain NH 4 HCO 3 mixture. After stirring evenly, Y(NO 3 ) 3 The solution was added dropwise to NH at a rate of 5ml / min 4 HCO 3 in the mixed solution. Meanwhile, the ammonium bicarbonate mixed solution was constantly stirred with a stirrer, and the pH value of the mixed solution was monitored with an acidity meter, and the pH value of the solution was adjusted between 7.0 and 7.5 with ammonia water and nitric acid. After the titration, the solution was aged for 24 hours. The preci...

Embodiment 2

[0079] Weigh 60.68g of YCl with a purity of 4N with a balance 3 ·6H 2 O, dissolved in deionized water to form 0.1mol L -1 YCl 3 solution. Take 118.58g of ammonium bicarbonate with a purity better than 99%, and dissolve it in a mixed solution composed of deionized water and absolute ethanol at a volume ratio of 2:1 to form a concentration of 2mol L -1 Ammonium bicarbonate alcoholic aqueous solution, add (NH 4 ) 2 SO 4 ((NH 4 ) 2 SO 4 with YCl 3 ·6H 2 The molar ratio of O is 2:1) as a dispersant to obtain a mixed solution of ammonium bicarbonate. After stirring well, the YCl 3 The solution was added dropwise to NH at a rate of 0.5ml / min 4 HCO 3in the mixed solution. Meanwhile, the mixed solution was continuously stirred with a stirrer, and the pH value of the mixed solution was monitored with an acidity meter, and the pH value of the solution was adjusted between 7.5 and 8.0 with ammonia water and nitric acid. After the titration, the solution was aged for 48 hou...

Embodiment 3

[0087] Use a balance to weigh 22.58g of Y with a purity of 5N 2 o 3 Powder, dissolved in CMOS Ⅱ grade concentrated nitric acid, and prepared with deionized water to make 0.5mol L -1 Y(NO 3 ) 3 solution. Take 158.1g of ammonium bicarbonate with a purity better than 99.9%, dissolve it in a mixed solution composed of deionized water and absolute ethanol at a volume ratio of 1:1, and form a concentration of 0.5mol L -1 Ammonium bicarbonate alcoholic aqueous solution, add appropriate amount (NH 4 ) 2 SO 4 As a dispersant ((NH 4 ) 2 SO 4 with Y 3+ ions in a molar ratio of 1:1), resulting in NH 4 HCO 3 Mix alcohol water solution. After stirring evenly, Y(NO 3 ) 3 The solution was added dropwise to NH at a rate of 10ml / min 4 HCO 3in the mixed solution. Meanwhile, the mixed solution was continuously stirred with a stirrer, and the pH value of the mixed solution was monitored with an acidity meter, and the pH value of the mixed solution was adjusted between 9.5 and 10....

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Abstract

The invention discloses a preparation method of yttrium aluminium garnet doped transparent laser ceramics. The method includes using an alcohol-aqueous system stepping chemical co-precipitation method to firstly prepare high-dispersity and high-activity nanometer Y2O3 oxide powders, Al2O3 oxide powders and rare earth (Re) oxide powders, weighing raw materials of the powders according to a stoichiometric ratio of Y<3-x>RexAl5O12 when the powders are prepared, placing the powders, sintering aids, dispersing agents and absolute ethyl alcohol into a ball-milling tank for ball milling, drying ball-milling mixing slurries into powders, forming the powders into green bodies with certain shapes by dry pressing, and then subjecting the green bodies to isostatic cool pressing to obtain ceramic biscuits. The ceramic biscuits are subjected to binder removing, vacuum sintering, powder-burying hot-pressing post-processing, annealing and optical polishing to obtain Re:YAG transparent ceramics. The preparation method has the advantages of being controllable, high in repeatability, low in cost and high in transmittance.

Description

technical field [0001] The invention belongs to the field of preparation of transparent ceramics, in particular to a method for preparing transparent laser ceramics doped with yttrium aluminum garnet. Background technique [0002] With the development of modern technology and industry, solid-state lasers have been used more and more widely in many fields. The laser working medium material is the heart of the solid-state laser, and its performance directly determines the performance and technical level of the solid-state laser. Traditional solid-state laser materials are mainly doped with rare earth ions on yttrium aluminum garnet (molecular formula is Re x Y 3-x AlO 12 , abbreviated as Re:YAG, the most important of which is neodymium-doped yttrium aluminum garnet, whose molecular formula is Nd x Y 3-x al 5 o 12 , referred to as Nd:YAG) single crystal as the representative laser crystal material and neodymium glass (Nd:Glass) as the representative laser glass material....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/44C04B35/505C04B35/622
Inventor 李兴旺张月娟杜秀红郑东阳陈文博
Owner 北京雷生强式科技有限责任公司
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