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Preparation method of rare earth ion-doped large lead tungstate crystal

A technology of rare earth ions and lead tungstate, which is applied in the field of preparation of large single crystals of lead tungstate, can solve problems such as easy cracking, large stress of PWO crystals, and crystal size that cannot meet the requirements for use, so that it is not easy to crack and the preparation process is simple. Effect

Active Publication Date: 2012-05-09
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the PWO crystals prepared by the high-temperature melting method often have relatively high stress, are prone to cracking during mechanical processing, and the crystal size cannot meet the requirements for use.

Method used

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  • Preparation method of rare earth ion-doped large lead tungstate crystal
  • Preparation method of rare earth ion-doped large lead tungstate crystal
  • Preparation method of rare earth ion-doped large lead tungstate crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a) Made of platinum with a thickness of 0.14mm figure 1 A crucible with the structure shown and a size of Φ40×200mm, wherein: the shoulder angle at the seed crystal end α=30 degrees;

[0026] b) Using a PWO single crystal with an orientation of and a size of Φ20×50mm as a seed crystal;

[0027] c) Nd with a purity of 99.99% 2 o 3 Incorporated into PWO polycrystalline ingot, Nd 3+ The doping amount is 0.5at%;

[0028] d) will be doped with Nd 2 o 3 Put the PWO polycrystalline ingot into the platinum crucible, then put the seed crystal and close the crucible, and use the descending method for crystal growth: put the seed crystal end of the platinum crucible down into the ceramic downtube, and use alumina powder in the gap Fill, then place the downcomer on the lowering platform, raise the temperature of the furnace to 1250°C after 12 hours, and then keep it warm for 6 hours; then gradually lift the downcomer to gradually melt the raw materials in the crucible until ...

Embodiment 2

[0031] a) Made of platinum with a thickness of 0.14mm figure 1 A crucible with the structure shown and a size of Φ50×300mm, wherein: the shoulder angle at the seed crystal end α=45 degrees;

[0032] b) Using a PWO single crystal with an orientation of and a size of Φ25×60mm as the seed crystal;

[0033] c) Nd with a purity of 99.99% 2 o 3 Incorporated into PWO polycrystalline ingot, Nd 3+ The doping amount is 1.0at%;

[0034] d) will be doped with Nd 2 o 3 Put the PWO polycrystalline ingot into the platinum crucible, then put the seed crystal and close the crucible, and use the descending method for crystal growth: put the seed crystal end of the platinum crucible down into the ceramic downtube, and use alumina powder in the gap Fill, then place the downcomer on the descending platform, raise the furnace temperature to 1280°C after 15 hours, and then keep it warm for 4 hours; then gradually raise the downcomer to gradually melt the raw materials in the crucible until th...

Embodiment 3

[0036] a) Made of platinum with a thickness of 0.14mm figure 1 A crucible with the structure shown and a size of 40×40×200 mm, wherein: the shoulder angle at the seed crystal end α=30 degrees;

[0037] b) Using a PWO single crystal with an orientation of and a size of 15×15×50 mm as a seed crystal;

[0038] c) Er with a purity of 99.99% 2 o 3 Incorporated into PWO polycrystalline ingot, Er 3+ The doping amount is 0.5at%;

[0039] d) will be doped with Er 2 o 3Put the PWO polycrystalline ingot into the platinum crucible, then put the seed crystal and close the crucible, and use the descending method for crystal growth: put the seed crystal end of the platinum crucible down into the ceramic downtube, and use alumina powder in the gap Fill, then place the downcomer on the lowering platform, raise the temperature of the furnace to 1250°C after 12 hours, and then keep it warm for 6 hours; then gradually lift the downcomer to gradually melt the raw materials in the crucible u...

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Abstract

The invention discloses a preparation method of a rare earth ion-doped large lead tungstate crystal. By the adoption of a crucible descent method, the preparation method is characterized in that the seed crystal is a round or square lead tungstate crystal with its radial dimension being 10-25mm; the crucible comprises a conical-form seed crystal end and the shoulder angle of the seed crystal end is 30-45 degrees; when the crystal grows, the maximum descent rate during the shoulder phase needs to be controlled within 0.4-0.8mm / h, and the maximum descent rate during the crystal growth phase is 0.8-1.2mm / h. By the adoption of the crucible descent method, the rare earth ion-dope PWO large crystal with its diameter being 50mm can be obtained from the growth of a minor-diameter seed crystal, and the prepared large crystal is not easy to crack during the machining process and can satisfy the application requirement of a luminescent material. In addition, the preparation technology provided by the invention is simple, and the grown crystal can satisfy the machining requirement without complex post-annealing, and the preparation method has industrial application values.

Description

technical field [0001] The invention relates to a method for preparing a large single crystal of lead tungstate doped with rare earth ions, and belongs to the technical field of crystal growth. Background technique [0002] Lead tungstate (PbWO 4 , referred to as PWO) crystals are not only widely used in high-energy physics, nuclear medicine and other fields due to their characteristics of fast luminescence, high density and low cost, but also have a wide range of light transmission, stable physical and chemical properties, high thermal conductivity and damage threshold The advanced characteristics make it a new type of semiconductor and optical functional host material. Therefore, the research on the luminescence of different doped PWO crystal materials is gradually attracting widespread attention. Due to the high segregation coefficient of rare earth ions in PWO crystals, it is conducive to high-concentration doping and uniform distribution of ion concentration, and the d...

Claims

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Application Information

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IPC IPC(8): C30B29/32C30B11/00
Inventor 熊巍袁晖周尧陈良
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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