Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes

A polycrystalline transparent, ceramic technology, applied in the field of special optical ceramics manufacturing process, can solve the problems of long growth period, difficult to increase crystal size and doping concentration, and high cost

Inactive Publication Date: 2011-05-18
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the limitation of single crystal growth technology, it is difficult to increase the crystal size and doping concentration
In addition, single crystal growth requires precious metal crucibles, and the growth cycle is long, so the cost is high. Therefore, scientists have been looking forward to finding a new method for preparing YAG laser matrix materials.
In 1995, Japanese scientists A.Ikesue et al. [Ikesue.A, Kinoshita.T, Kamata.K, et al. "Fabrication optical properties of high-performance polycrystalline Nd: YAG ceramics for solid-statelasers", J.Am.Ceram .Soc., 78(4)(1995): 1033-1040] using TEOS as a sintering aid, with sub-micron Al 2 o 3 , Y 2 o 3 and Nd 2 o 3 As raw material, using cold isostatic pressing combined with vacuum sintering process, the highly transparent Nd:YAG ceramics were prepared for the first time, and the laser output was obtained for the first time, but the laser power and efficiency were not high

Method used

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  • Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes
  • Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes
  • Method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017]Put 5.098g of α-Al2O3 powder, 6.7066g of Y2O3 powder, 0.1010g of Nd2O3, 0.0600g of TEOS and 0.0600g of castor oil, 0.3600g of PVB, and 0.1200g of unsaturated fatty acid into a high-purity agate ball mill jar , add 72g of high-purity agate balls, 11.800g of absolute ethanol, mix ball mill for 24h. After ball milling, the slurry was dried in an oven at 80°C, and after drying for 48 hours, it was put into an agate mortar and ground, and the powder was passed through a 200-mesh sieve. Axial one-way pressurization with a pressure of 2-10Mpa to form a Φ15 disc, and then cold isostatic pressing under a pressure of 200Mpa. Put the isostatically pressed green body into a tube furnace and raise the temperature to 700°C at a rate of 1°C / min under an oxygen atmosphere, keep it warm for 2 hours, and the oxygen flow rate is 50-100ml per minute, and cool naturally after the keep warm. The degreased green body is put into a vacuum furnace, and the vacuum degree is 1.5×10 -4 Carry out ...

Embodiment 2

[0019] Weigh the commercially available high-purity powder according to the stoichiometric ratio: Y 2 o 3 : 10.0600g, Al 2 o 3 : 7.6470g, Nd 2 o 3 : 0.1516g, add 0.5at% MgO sintering aid, 0.2wt% dispersant polycarboxylic acid, 0.2wt% binder polyvinyl alcohol, 0.5wt% defoamer n-butanol; Additives were poured into 100 g of deionized water and ball milled for 12 hours and mixed at a ball milling speed of 350 r / m, material: ball = 1:10. Put the slurry mixed by ball milling into a vacuum tank, vacuum treatment until the vacuum degree reaches below -0.1Mpa, and no air bubbles escape from the slurry; inject the slurry after defoaming into the gypsum mold, and wait for the gypsum mold to absorb the slurry , the green body shrinks and the plaster mold is separated, and the mold is removed. The formed green body is first dried in the shade at room temperature for a period of time, and then put into an oven to keep warm at 30°C for 5 hours, 40°C for 3 hours, 60°C for 2 hours, and s...

Embodiment 3

[0021] Weigh the commercially available high-purity powder according to the stoichiometric ratio: Y 2 o 3 : 10.0600g, Al 2 o 3 : 7.6470g, Nd 2 o 3 : 0.1516g, add the MgO sintering aid of 0.5at%, add 0.06wt% dispersant fish oil, add raw material to 60 grams by dehydrated alcohol and xylene in the mixed solvent, material: ball=1: 5, ball mill mixes 5 After ~24 hours, add 10wt% binder polyvinyl butyral to the homogeneously mixed slurry, 5wt% plasticizer is butyl phthalate and 1wt% polyalkylene glycol, 0.5wt% except The foaming agent octanol is then mixed and ball milled for 5 to 24 hours. Put the ball-milled slurry into a vacuum defoaming machine, and stir it under negative pressure until no air bubbles escape from the slurry. Pour the defoamed slurry into the hopper of the casting machine, turn on the mechanical motor, rotate the film belt at a constant speed, spread it evenly on the film belt with a scraper, heat the bottom plate to a suitable temperature and dry the gree...

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Abstract

The invention relates to a method for preparing Re:YAG polycrystalline transparent ceramic by using different molding modes, which adopts commercial high-purity Y2O3, Al2O3 and Re2O3 as raw materials, adopts MgO, CaO or TEOS (tetraethyl orthosilicate) as sintering additive, and prepares a raw blank by a cold isostatic pressing, slip casting or tape casting process to react and sinter the transparent polycrystalline Re:YAG ceramic. The method comprises the following steps: mixing and adding the oxides into a liquid medium; adding a certain amount of dispersant, adhesive, plasticizer, pressing agent and defoaming agent, carrying out ball milling, and mixing; treating the slurry under different conditions in different molding modes to obtain the raw blank; and sintering the degreased raw blank in a vacuum furnace. For the Re:YAG ceramic sintering body with thickness of 1.5mm, the transmission rate of straight light in the wavelength of 1064nm is not lower than 80% after the Re:YAG ceramic sintering body is subjected to double-sided polishing. For the raw blank which is prepared by different molding modes and is sintered for 10 hours at 1750 DEG C, sizes of ceramic grains are different, wherein regarding the raw blank prepared by cold isostatic pressing, the average grain of the ceramic is 13.5mu m; regarding the raw blank prepared by slip casting, the average grain of the ceramic is 3.5mu m; and regarding the raw blank prepared by tape casting, the average grain of the ceramic is 1.5mu m.

Description

technical field [0001] The invention provides a method for preparing Re:YAG polycrystalline transparent ceramics in several different molding methods, and belongs to the technical field of special optical ceramics manufacturing technology. Background technique [0002] Traditional laser host materials are usually single crystal or glass, YAG single crystal is the most important solid laser host material, doped with Nd 3+ 、Er 3+ 、Ho 3+ 、Tm 3+ , Yb 3+ 、Cr 3+ YAG single crystals such as rare earth or transition group ions are laser crystals with excellent performance. They have been widely used in many fields such as scientific research, environmental protection, laser medical treatment, and laser processing. However, due to the limitation of single crystal growth technology, it is difficult to increase the crystal size and doping concentration. In addition, single crystal growth requires precious metal crucibles, and the growth cycle is long, so the cost is high. Therefo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/622C04B35/505
Inventor 郭旺曹永革黄秋凤黄志刘媛
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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