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Preparation method of gadolinium oxysulfide powder and sparkling ceramics

A technology of gadolinium oxysulfide and powder, which is applied in the field of ceramics, can solve the problems of large-scale commercial application limitation, complex process, deviation of firing effect, etc., to achieve easy batch production, uniform powder particle size and avoid adverse effects Effect

Active Publication Date: 2019-09-06
上海御光新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This production method requires the particle size of the scintillating powder to be small and the surface sintering activity to be good. The process of making such a powder is relatively complicated.
The patent US 8,025,817 of Philips adopts a method of preparing GOS scintillating ceramics by using a commercial scintillating powder with a larger particle size through a vacuum hot pressing method. The method is characterized in that the scintillating powder with a larger particle size is used, but in The hot pressing pressure is required to be as high as about 200-250MPa during hot pressing, which requires high requirements on hot pressing molds. The cost of such hot pressing molds is very high, and there are few suppliers, which restricts large-scale commercial applications.
[0005] Hot pressing sintering can be fired into large size according to the needs, the cost is relatively low, and the preparation efficiency is high. The quality determines the quality of subsequent sintered ceramics
Spark plasma sintering is a new sintering technology that has emerged in recent years. It has the advantages of fast heating, short sintering time, and high sintering efficiency. Secondary sintering using hot isostatic pressing sintering method requires the use of a large amount of high-purity gas, the overall process is complex, equipment investment is large, and the cost is high

Method used

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  • Preparation method of gadolinium oxysulfide powder and sparkling ceramics
  • Preparation method of gadolinium oxysulfide powder and sparkling ceramics
  • Preparation method of gadolinium oxysulfide powder and sparkling ceramics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Take analytically pure concentrated sulfuric acid H 2 SO 4 26g, diluted with 400g deionized water to obtain dilute sulfuric acid solution; add high-purity Gd 2 o 3 95.72g, Pr 6 o 11 0.899g, use a magnetic stirrer to stir evenly to make the reaction fully, filter the solution after 2 hours, dry the precipitate to obtain the precursor powder 1;

[0046] Heat the precursor powder 1 to 350°C for 1 hour, then continue to heat up to 750°C for 2 hours to obtain the precursor powder 2; add the reducing agent activated carbon to the calcined precursor powder 2 in a proportion of 0.005wt% After ball milling and mixing, continue to pass the mixed powder through H 2 Carry out reduction, pass high-purity nitrogen gas after reduction, cool down to room temperature, and obtain Gd 2 o 2 S: Pr powder;

[0047] Will Gd 2 o 2 S: Add MOS grade high-purity absolute ethanol to Pr powder, stir evenly, and then granulate through a granulator to obtain 95% of Gd with a particle size ...

Embodiment 2

[0052] Take analytically pure concentrated sulfuric acid H 2 SO 4 26g, diluted with 400g deionized water to obtain dilute sulfuric acid solution; add high-purity Gd 2 o 3 96g, Tb 2 o 3 0.97g, use a magnetic stirrer to stir evenly to make the reaction fully, filter the solution after 2 hours, dry the precipitate to obtain the precursor powder 1;

[0053] Heat the precursor powder 1 to 350°C for 1 hour, then continue to heat up to 750°C for 2 hours to obtain the precursor powder 2; add the reducing agent activated carbon to the calcined precursor powder 2 in a proportion of 0.005wt% After ball milling and mixing, continue to pass the mixed powder through H 2 Carry out reduction, pass high-purity nitrogen gas after reduction, cool down to room temperature, and obtain Gd 2 o 2 S: Tb ​​powder;

[0054] Will Gd 2 o 2 S: Add MOS grade high-purity absolute ethanol to Tb powder, stir evenly, and then granulate through a granulator to obtain 95% Gd with a particle size of 3....

Embodiment 3

[0059] Gd 2 o 3 , sulfuric acid and CeO 2 According to the molar ratio of 0.995:1:0.01, use a magnetic stirrer to stir evenly to make the reaction fully, filter the solution after the reaction, and dry the precipitate to obtain the precursor powder 1; the sulfuric acid described in this embodiment is dilute sulfuric acid, and its mass fraction 65%;

[0060] Calcining the precursor powder 1 at 700°C for 2.5 hours to obtain the precursor powder 2; adding the reducing agent graphene to the calcined precursor powder 2 according to the ratio of 0.005wt% of its mass, and then ball milling and mixing. The powder continues to pass through H 2 Carry out reduction, pass high-purity nitrogen gas after reduction, cool down to room temperature, and obtain Gd 2 o 2 S: Ce powder;

[0061] Will Gd 2 o 2 S: Add MOS grade high-purity absolute ethanol to Ce powder, stir evenly, and then granulate through a granulator to obtain 95% of Gd with a particle size of 3.5-7 μm 2 o 2 S: Ce powd...

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Abstract

The invention provides a preparation method of gadolinium oxysulfide powder and sparkling ceramics. The preparation method of Gd2O2S powder includes the following steps that Gd2O3, sulfuric acid and rare earth oxides are mixed and stirred to obtain precursor powder; the precursor powder is calcined at 700-800 DEG C; the well calcined precursor powder and a solid reducing agent are subjected to ball milling and mixed; the mixed powder is reduced in a reducing atmosphere, and (Gd1-XBX)2O2S powder is obtained, wherein B refers to one or more of Pr, Tb, Ce and Eu and X=0.005-0.15; ethyl alcohol isadded into the (Gd1-XBX)2O2S powder, pelleting is performed through a pelletizer after stirring, and the (Gd1-XBX)2O2S powder with the particle size more than 95% is obtained. A commercially feasiblecomplete method for preparing Gd2O2S powders, pre-pressing powders and sintering ceramics is provided, and the method has the advantages that the cost is low, batch manufacture is easy and stabilityand reliability are achieved.

Description

technical field [0001] The invention relates to the field of ceramics, in particular to gadolinium oxysulfide ceramics. Background technique [0002] The detector component is mainly composed of photodiodes and scintillators, and is an important part of radiation detection devices such as security inspection machines and computed tomography scanners. The scintillator in the detector emits visible light after absorbing high-energy rays, and its performance greatly affects the overall performance index and detection effect of the radiation detection device. The current scintillators are mainly artificial crystals and transparent ceramics. Compared with ceramics, they are not easy to deliquescence, the production cycle is short, the preparation cost is lower than that of artificial crystals, the doping of rare earth ions is more uniform, and there is no segregation coefficient. It needs to be prepared into various shapes and other outstanding advantages, and its application in...

Claims

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Application Information

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IPC IPC(8): C04B35/50C04B35/622C04B35/626C09K11/77
CPCC04B35/50C04B35/622C04B35/62605C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/662C04B2235/9646C09K11/7771
Inventor 唐华纯李中波
Owner 上海御光新材料科技股份有限公司
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