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Indirect sulfur source preparation method of gadolinium oxysulfide scintillation ceramic powder

A technology of gadolinium oxysulfide and scintillation ceramics, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc.

Inactive Publication Date: 2016-07-27
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims to overcome the defects of the existing preparation method of gadolinium oxysulfide scintillation ceramic powder, and the present invention provides an indirect sulfur source preparation method of scintillation ceramic powder scintillation ceramic powder

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  • Indirect sulfur source preparation method of gadolinium oxysulfide scintillation ceramic powder
  • Indirect sulfur source preparation method of gadolinium oxysulfide scintillation ceramic powder
  • Indirect sulfur source preparation method of gadolinium oxysulfide scintillation ceramic powder

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preparation example Construction

[0030] The invention discloses a method for preparing an indirect sulfur source of scintillation ceramic powder, comprising:

[0031] Weigh carbon, sodium sulfate and gadolinium oxide powder in a ratio of 1:1:0.05 to 1:6:2, add rare earth active ions that are 1% to 0.0001% of the mass of gadolinium oxide powder, and the obtained raw materials are ball milled, dried, Gd can be obtained by sieving, calcining and washing 2 o 2 S: X powder.

[0032] The rare earth activating ion X includes Ce, Tb, Nd and other rare earth elements, which can be one of them or a mixture of several of them in different proportions. It can be introduced in the form of oxides, and also includes sulfates, nitrates, carbonates, etc. of such rare earth elements.

[0033] The mixture is put into an alumina crucible after dry pressing, and calcined in a muffle furnace at a high temperature of 600-1400°C, and the holding time is 10min-10h.

[0034] After the calcined powder is taken out and crushed, it i...

Embodiment 1

[0055] Weigh 20g of high-purity sodium sulfate and 3g of high-purity activated carbon, add 1.2g of gadolinium oxide and 0.002g of hexapraseodymium oxide, pour it into an agate ball mill jar, add 150g of alumina balls and 25ml of alcohol, and mill on a planetary ball mill After 4 hours, the mixed powder was dried in an oven at 100°C, passed through a 200-mesh sieve, put into a double crucible, and filled with activated carbon to form a protective atmosphere. Cover it with an alumina plate, put it in a muffle furnace for 180 minutes and raise the temperature to 900°C, keep it at this temperature for 3 hours, and then cool it down naturally. Take out the powder and add 5% dilute nitric acid, soak for 30min, filter, add 500ml of water to wash 3 times, and finally wash once with alcohol. Put it in a glass petri dish and dry it in an oven at 70°C to get high-quality Gd 2 o 2 S: Pr phosphor. figure 2 Indicates that Gd is generated 2 o 2 S, and has good crystallinity. image 3 ...

Embodiment 2

[0057] Weigh 150g of high-purity sodium sulfate and 23g of high-purity activated carbon, add 50g of gadolinium oxide and 0.004g of hexapraseodymium oxide, pour it into an agate ball mill jar, add 345g of alumina balls and 120ml of alcohol, and mill on a planetary ball mill for 4 hours The mixed powder is dried in an oven at 100°C, then passed through a 200-mesh sieve, put into a crucible, covered with an alumina plate, placed in a muffle furnace that can pass through an inert atmosphere and heated to 1000°C for 200 minutes, and then The temperature was kept for 3 hours and then cooled naturally. Take out the powder and add 5% dilute nitric acid, soak for 30min (Gd 2 o 2 S is insoluble in dilute nitric acid solution, this process can remove excess gadolinium oxide), filter, then pour off the supernatant, add 1000ml of water to wash twice, and finally wash with alcohol. Put it in a glass petri dish and dry it in an oven at 70°C to get high-quality Gd 2 o 2 S: Pr phosphor. ...

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Abstract

The invention provides an indirect sulfur source preparation method of gadolinium oxysulfide scintillation ceramic powder. The method comprises weighing carbon, sodium sulfate and gadolinium oxide powder, blending the powder, calcining the mixed powder at a temperature of 600-1400 DEG C in an inert atmosphere and removing impurities to obtain gadolinium oxysulfide. A sulfur source is sodium sulfide prepared from carbon and sodium sulfate and the sulfur source and gadolinium oxide undergo a reaction to produce gadolinium oxysulfide. A mass ratio of the carbon, sodium sulfate to gadolinium oxide powder is 1: 1: 0.05 to 1: 7: 2, preferably, the mass ratio is 1: 1: 0.05 to 1: 6: 2 and more preferably, the mass ratio is 1: 5.875: 0.05 to 1: 7: 2.

Description

technical field [0001] The invention relates to an indirect sulfur source preparation method for gadolinium oxysulfide scintillating ceramic powder. High-luminescence fluorescent powder such as gadolinium oxysulfide can be used for sintering scintillation ceramics and as materials for X-ray intensifying screens. Background technique [0002] Rare earth oxysulfides are wide bandgap semiconductors with many excellent properties, such as good chemical stability, environmental friendliness, and high luminous efficiency. Therefore, they are widely used in fluorescent matrix materials, such as high-efficiency red phosphors Applied to color picture tube, X-ray computed tomography, laser materials. Among a series of oxysulfides, gadolinium oxysulfide belongs to the hexagonal system, Has a very high density (7.34g / cm 3 ), the atomic number of Gd is 60, which has a high resistance to X-rays, especially after being prepared into ceramics, gadolinium oxysulfide ceramics have good sci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C04B35/50
Inventor 王伟寇华敏刘秉龙李超宇刘书萍潘裕柏郭景坤石云李江冯锡琪
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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