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Spray granulation preparation method for YAG-based transparent ceramic powder

A technology of spray granulation and transparent ceramics, which is applied in the field of spray granulation preparation of YAG-based transparent ceramic powder, which can solve the problems of poor sphericity, low density of ceramic green bodies, general fluidity and filling properties, etc., and achieve loose High packing density and filling density, reasonable particle size distribution, good fluidity and filling effect

Active Publication Date: 2015-02-18
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Document 1 (W.B.Liu, W.X.Zhang, J.Li, etc. Ceram Int, 38 (2012) 259-264.) in the solid content of 46.43wt.%, adding PVB binders under the conditions of 2.0wt.%, respectively, The granulated particles with a central particle diameter of about 5 μm were produced, but the surface had many depressions and poor sphericity, and the transmittance of the final fired YAG transparent ceramics at 1064 nm was less than 80%.
Document 6 (L.Esposito, A.Piancastelli, A.L.Costa, etc, Opt Mater, 33 (2011) 713-721.) As a research before the spray granulation process of Document 3 was not optimized, the highest transmittance of YAG ceramics is only 78% , but the remaining pores in the ceramic sintered body are still significantly less than those directly dried in an oven
And document 7 (E.Cavalli, L.Esposito, J.Hostasa, etc. J Eur Ceram Soc, 33 (2013) 1425-1434.) Er: YAG ceramics prepared by the process of document 3 has a higher transmittance at 1064nm Less than 78%, Er / Yb:YAG ceramics less than 68%
In addition, the output of the spray granulation process in Documents 3 to 7 is very low, only about 30g / h
[0008] In the above patents and documents, the YAG transparent ceramic powder produced by the spray granulation process generally has irregular particle shape, poor sphericity, more surface depressions, mostly "apple" shape, and dispersed particles. Poor performance, mutual adhesion, small particle size (center particle diameter is mostly below 10 μm), and deviates from normal distribution, low yield (all Lab grade), and this kind of granules are in the process of forming between particles and between particles The friction between the abrasive tools is still relatively large, the fluidity and filling properties are average, the density of the ceramic green body is not high, and the transmittance of the final transparent ceramics needs to be improved, which cannot meet the preparation of high optical quality YAG-based transparent ceramics, especially It is its application in high power, large size and composite structure

Method used

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  • Spray granulation preparation method for YAG-based transparent ceramic powder
  • Spray granulation preparation method for YAG-based transparent ceramic powder
  • Spray granulation preparation method for YAG-based transparent ceramic powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 # (undoped, Y 3 al 5 o 12 ):

[0037] Composition as in Table 1 1 # Shown, specific preparation method comprises the following steps:

[0038] ① Weigh the raw materials according to the composition in Table 1. First, put the oxide raw material powder into a high-purity alumina ball mill tank, add 2800g of high-purity alumina balls, and add sintering aids, dispersants, and absolute ethanol to prepare slurry Material; Ball milling and mixing on planetary ball mill for 10 hours, the rotating speed is 160r / min, then add binder, continue ball milling and mixing for 2 hours to obtain the slurry used for spray granulation;

[0039] ② Use a centrifugal spray dryer to spray and granulate the slurry obtained in step ①. The spray drying conditions are: the inlet temperature of hot air is 70°C, the outlet temperature is 60°C, and the inlet air volume is 200m 3 / h, outlet air volume 300m 3 / h; the rotational speed of the centrifugal atomizer is 8000r / min; the pumpi...

Embodiment 2

[0042] Example 2 # (1mol%Nd:YAG,(Y 0.99 Nd 0.01 ) 3 al 5 o 12 ):

[0043] Composition as in Table 1 2 # Shown, specific preparation method comprises the following steps:

[0044] ①Weigh the raw materials according to the composition in Table 1, first put the oxide raw material powder into the high-purity alumina ball mill tank, add 1400g high-purity alumina balls, and add sintering aids, dispersants, and absolute ethanol to prepare the slurry Material; ball milling and mixing on a planetary ball mill for 8 hours, the rotating speed is 300r / min, then add binder, continue ball milling and mixing for 1.5 hours to obtain the slurry used for spray granulation;

[0045] ② Use a centrifugal spray dryer to spray and granulate the slurry obtained in step ①. The spray drying conditions are: the inlet temperature of hot air is 65°C, the outlet temperature is 50°C, and the inlet air volume is 250m 3 / h, outlet air volume 350m 3 / h; the rotational speed of the centrifugal atomize...

Embodiment 3

[0048] Example 3 # (30.0mol%Yb:YAG,Y 0.7 Yb 0.3 ) 3 al 5 o 12 ):

[0049] Composition as in Table 1 3 # Shown, specific preparation method comprises the following steps:

[0050] ①Weigh the raw materials according to the composition in Table 1, first put the oxide raw material powder into the high-purity alumina ball mill tank, add 5600g of high-purity alumina balls, and add sintering aids, dispersants, and absolute ethanol to prepare the slurry Material; ball milling and mixing on a planetary ball mill for 12 hours, the rotating speed is 100r / min, then add binder, continue ball milling and mixing for 1 hour to obtain the slurry used for spray granulation;

[0051] ② Use a centrifugal spray dryer to spray and granulate the slurry obtained in step ①. The spray drying conditions are: the inlet temperature of hot air is 80°C, the outlet temperature is 65°C, and the inlet air volume is 150m 3 / h, outlet air volume 250m 3 / h; centrifugal atomizer speed is 6000r / min; slurry...

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Abstract

The invention relates to a spray granulation preparation method for YAG-based transparent ceramic powder. The preparation method particularly comprises the following steps: weighting raw material powder according to the molar ratio of metallic elements needed to compose (Y1-xREx)3Al5O12; adding in a sintering additive, a dispersing agent and a solvent to prepare a sizing agent; mixedly adding in a binder in an upper ball mill of a planetary ball mill; continuously conducting ball milling and mixing to obtain a sizing agent for pray granulation; selecting a centrifugal spray dryer to conducting pray granulation on the sizing agent; sieving granulation powder obtained by collecting to obtain the YAG-based transparent ceramic powder. The prepared YAG-based transparent ceramic powder is high in chemical purity, good in uniformity, good in degree of sphericity, good in liquidity, high in yield and high in productive rate, drying of the sizing agent can be completed in short time, the experimental period is shortened, and the preparation cost is reduced.

Description

technical field [0001] The present invention relates to a method for preparing YAG-based transparent ceramic powder by spray granulation, more precisely to a method using polyvinyl butyral (PVB) and polymer DS005 as binder and strong dispersant respectively, using The method of centrifugal atomization to prepare solid monodisperse YAG granulated powder with high chemical purity, good uniformity, high sphericity and good fluidity belongs to the field of advanced ceramics. Background technique [0002] Since Japanese scientist Ikesue realized the continuous laser output of Nd:YAG transparent ceramics by solid state reaction sintering method in 1995, laser ceramics are characterized by short preparation cycle, easy realization of uniform (gradient) and high concentration doping, easy realization of large size and design Due to the advantages of flexibility and other advantages, various new laser transparent ceramic materials emerge in an endless stream, such as Yb / Nd:YSAG, Nd:Y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/44C04B35/505C04B35/626
Inventor 张乐章健杨浩乔学斌唐定远沈德元周天元周刊
Owner XUZHOU NORMAL UNIVERSITY
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