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High-purity tellurium dioxide single crystal and preparation method

A technology of tellurium dioxide and single crystal, which is applied in the field of high-purity tellurium dioxide single crystal and its preparation, to achieve the effect of improving the purity

Active Publication Date: 2010-10-06
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0009] Chinese patent ZL03141999.2 has reported the use of crucible drop method to grow high-quality large-size TeO 2 The method of single crystal can reduce the content of impurities such as U and Th to 10 -12 g / g, but still higher than required for double beta decay sources
[0010] However, until the present invention is proposed, there has not been any report about reducing the impurity content and preparing high-purity tellurium dioxide single crystal

Method used

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  • High-purity tellurium dioxide single crystal and preparation method

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Embodiment 1

[0039] (1) TeO prepared by dissolution and neutralization 2 Powder (marked as TeO 2 (1) Powder) was packed into a platinum crucible, calcined at 680° C. for 12 hours, and then rapidly cooled to room temperature. Then put the calcined powder and the oriented seed crystal into a platinum crucible, heat up to 750° C. and keep it warm for 10 hours after sealing. Then control the heating rate to be 2°C per hour, and the crucible's descending rate to be 1.0mm per hour to grow a single crystal. After the growth is completed, the single crystal is lowered to room temperature at 30°C per hour, and then annealed at 680°C for 12 hours to complete the whole process of the first growth.

[0040] (2) Remove the surface 1-2mm of the single crystal obtained in step (1) by coarse grinding, and then dissolve the single crystal into TeCl with 37.5wt% hydrochloric acid 4 solution.

[0041] (3) then join the strong ammoniacal liquor of 28wt% to step (2) gained TeCl 4 solution, a white precipi...

Embodiment 4

[0051] (1) Commercially available TeO 2 Powder is packed in the platinum crucible, feeds oxygen and controls its flow rate to be 750ml per minute. After the powder melts, keep the temperature constant for 4 hours, then gradually lower the oriented seed crystal, adjust the surface temperature of the melt, and make the seed crystal contact the liquid surface when it is close to the solid-liquid equilibrium. After successful inoculation, the pulling rate was controlled to be 1.2 mm per hour, and the seed crystal rotation speed was 30 revolutions per minute to grow a single crystal. After the growth was completed, the single crystal was cooled down to room temperature at 60°C per hour. Finally, after 12 hours of annealing treatment at 680° C., the whole process of the first growth is completed.

[0052] (2) Remove 0.5-0.8mm of the surface of the single crystal obtained in step (1) by coarse grinding, and then dissolve the single crystal into TeCl with 37.5wt% hydrochloric acid ...

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Abstract

The invention relates to a high-purity tellurium dioxide single crystal and a preparation method, which belong to the technical field of the growth of single crystals. The preparation process comprises the following steps of: firstly, growing the single crystal for the first time, then re-dissolving the obtained single crystal, afterwards adding a precipitator for milling, and finally, obtaining the high-purity single crystal after growing the single crystal for the second time at the prepared powder. The purity of the tellurium dioxide single crystal prepared by the invention is high, and especially, the content of the radioactive impurities of U, Th and the like can be lowered to 10 to 13g / g.

Description

technical field [0001] The invention relates to a high-purity tellurium dioxide single crystal and a preparation method thereof, belonging to the technical field of single crystal growth. technical background [0002] In the field of nuclear physics, experiments on neutrinos have always been the scientific frontier of world attention. In 1956, Reines and Kirwan of the United States directly observed neutrinos in experiments, and won the Nobel Prize in Physics in 1995; The neutrinos——Miao neutrinos, won the Nobel Prize in Physics in 1988; in 1968, Davis of the United States discovered the disappearance of solar neutrinos, and he shared the 2002 Year Nobel Prize in Physics. However, so far, the size of the (static) mass of neutrinos and how to transform between different types of neutrinos are still a basic scientific problem to be solved in the field of nuclear physics (Huang Zhixun, Chinese Engineering Science 2002, 4(10 ), 7-10). [0003] In the above research fields, t...

Claims

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Application Information

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IPC IPC(8): C30B29/16C30B29/46C30B11/00C30B15/00C01B19/04
CPCC30B29/46C30B11/00C30B29/16C30B15/00
Inventor 葛增伟朱勇吴国庆殷学技唐林耀赵寒冰顾李臻
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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