Preparation method of gadolinium oxysulfide scintillation ceramic
A technology of scintillating ceramics and gadolinium oxysulfide, which is applied in chemical instruments and methods, instruments, radiation measurement, etc., and can solve problems such as expensive, difficult to obtain, and high hot-pressing pressure
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[0019] In order to overcome one or more defects of the prior art, the invention provides a preparation method of GOS scintillation ceramics, which comprises the following steps:
[0020] 1) To Gd with a median particle size of 5-9μm 2 o 2 S: Pr, Ce scintillation ceramic powder with sintering aid added. Preferably, the powder is commercially available, and its purity is not less than 99.995%, preferably not less than 99.999%; it is also preferred that the doping amount of Pr ions is 500-800ppm in mass content, and the doping amount of Ce ions is The amount is 10-50ppm in mass content. In addition, preferably wherein the sintering aid is LiF and / or Li 2 GeF 6 ; The addition of the sintering aid is 0.02-1%, preferably 0.1-1%, based on the mass of the scintillation ceramic powder. The mixed powder is ball milled to make it uniformly mixed, and optionally refined to obtain a powder containing a sintering aid. Preferably said ball milling is carried out on a planetary ball mil...
Embodiment 1-5
[0041] Weigh 100 g of commercial Gd with a particle size of 4.0 μm for d(0.1), 6.8 μm for d(0.5) and 10.1 μm for d(0.9) with a purity of 99.999% 2 o 2 S:Pr, Ce scintillation ceramic powder, add 0.2g Li 2 GeF 6 As a sintering aid, put a polyurethane ball mill tank with an inner diameter of 100 mm and a height of 100 mm in an argon gas box, add 500 g of high-density yttrium oxide reinforced zirconia grinding balls with graded sizes, add 300 mL of MOS grade high-purity absolute ethanol, and place In the planetary ball mill, at a speed of 500 rpm, the ball mill was mixed for 1 hour, and the forward and reverse directions were run for 0.5 hours each.
[0042] The polyurethane ball mill jar and zirconia balls need to be pre-cleaned. The specific method is as follows: Put 500g of high-density yttria-strengthened zirconia balls into the ball mill jar, including 35g of balls with a diameter of 10mm, 105g of balls with a diameter of 6mm, and 360g of balls with a diameter of 3mm. , ad...
Embodiment 6、7
[0047] The scintillation powder was ball milled and mixed in the same manner as in Examples 1-5 to obtain powders with the same particle size distribution. Put the powder into a carbon fiber composite material mold with an inner diameter of 50 mm, and perform vacuum hot pressing for one-time sintering. The temperature is at 1500 and 1550°C respectively, the pressure is 200MPa, and the vacuum is 5×10 -2 Pa, heat preservation and pressure for 2 hours. After the heat preservation is over, execute the cooling program, the cooling rate is 5°C / min, and take it out after it is completely cooled to room temperature, which is the GOS primary sintered body. The same annealing and hot isostatic pressing methods as in Examples 1-5 were used for secondary sintering and post-treatment to obtain GOS:Pr, Ce, F scintillation ceramics.
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