Process for preparing lead tungstate-doped crystal

A lead tungstate and crystal technology, applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve problems such as impossibility of doping, uneven distribution of doping concentration, difficulties, etc.

Inactive Publication Date: 2007-05-16
JIAXING UNIV +1
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  • Abstract
  • Description
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Problems solved by technology

[0002] The existing technology is relatively successful in growing lead tungstate and some oxides with relatively high melting point doping modified lead tungstate crystals, but it encounters difficulties in growing dopant doping with low melting point and strong volatility, because in these When growing crystals in the device, it is usually necessary to reserve a part of the upper part of the crystal raw material in the crucible to accommodate the oxygen required for crystal growth. The temperature distribution in the crystal growth furnace is shown in Figure 1. The upper part has a higher temperature, and the crystal growth raw materials and dopants In the molten state, doped with non-volatile doping substances such as La 2 o 3 The effect of the reserved space on crystal growth is not very obvious, but in the growth of low melting point and high volatility such as PbF 2 When doping substances, the severe volatilization of doping substances will make doping almost impossible
[0003] In order to solve this problem, Chinese applicatio

Method used

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  • Process for preparing lead tungstate-doped crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] a PbF 2 :PbWO 4 Crystal preparation method, comprises the steps:

[0019] (1) PbO and WO with a purity of 99.99% 3 and dopant PbF 2 After the solid powder is dried at about 150 °C, PbO and WO 3 Weighing according to the stoichiometric ratio, the dopant PbF 2 The molar concentration is 0.01%, and the weighed solid powder is pressed into a dense block solid under a pressure of 10Kpa, sintered in an oxidizing atmosphere at 750°C, and kept at a constant temperature of 1130°C for half an hour in a closed platinum crucible filled with oxygen to make it completely melt;

[0020] (2) Introduce the melted raw material into a growth crucible with a seed crystal to form a dense polycrystalline ingot, and place the growth crucible in a temperature-gradient method crystal growth furnace for inoculation and growth to obtain the finished product PbF 2 :PbWO 4 Crystal; the temperature distribution curve in the temperature gradient method crystal growth furnace is divided into fo...

Embodiment 2

[0022] a Yb 2 o 3 :PbWO 4 Crystal preparation method, comprises the steps:

[0023] (1) PbO and WO with a purity of 99.99% 3 and dopant Yb 2 o 3 After the solid powder is dried at about 180 °C, PbO and WO 3 Weighing according to the stoichiometric ratio, the dopant Yb 2 o 3 The molar concentration is 0.05%, and the weighed solid powder is pressed into a dense block solid under a pressure of 30Kpa, sintered in an oxidizing atmosphere at 900°C, and kept at 1160°C for half an hour in a closed platinum crucible filled with oxygen to make it completely melt;

[0024] (2) Introduce the melted raw material into a growth crucible with a seed crystal to form a dense polycrystalline ingot, and place the growth crucible in a temperature-gradient method crystal growth furnace for inoculation and growth to obtain the finished product Yb 2 o 3 :PbWO 4 Crystal; the temperature distribution curve in the temperature gradient method crystal growth furnace is divided into four section...

Embodiment 3

[0026] a BaF 2 :PbWO 4 Crystal preparation method, comprises the steps:

[0027] (1) PbO and WO with a purity of 99.99% 3 and dopant BaF 2 After the solid powder is dried at about 200 °C, PbO and WO 3 Weighing according to the stoichiometric ratio, the dopant BaF 2 The molar concentration is 0.1%, and the weighed solid powder is pressed into a dense block solid under a pressure of 50Kpa, sintered in an oxidizing atmosphere at 1000°C, and kept at a constant temperature of 1200°C for half an hour in a closed platinum crucible filled with oxygen to make it completely melt.

[0028] (2) Introduce the melted raw material into a growth crucible with a seed crystal to form a dense polycrystalline ingot, and place the growth crucible in a temperature-gradient method crystal growth furnace for inoculation and growth to obtain the finished product BaF 2 :PbWO 4 Crystal; the temperature distribution curve in the temperature gradient method crystal growth furnace is divided into fo...

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Abstract

The invention discloses a preparing method of doped lead tungstate crystal, which comprises the following steps: (1) drying PbO, WO3 with purity at 99.99% and solid powder of doping agent under 150-200 Deg C; weighing the PbO and WO3 according to chemical weight; setting the molar rate density of doping agent at 0.01-0.1%; pressing weighted solid powder into dense solid under 10-50Kpa; sintering in the oxidizing environment at 750-1000Deg C; aerating oxygen in the sealed platinum copple; insulating at 1130-1200 Deg C to fuse the solid; (2) introducing fused raw material into growing copple with seed to form dense multi-crystal ingot; placing the growing copple in the temperature-gradient crystal growing furnace to inoculate and grow with introducing speed at 1.0mm/h. The invention is fit for effumable doping agent, which is also fit for doping agent without effumability.

Description

technical field [0001] The invention relates to the field of crystal growth, in particular to a method for preparing doped lead tungstate crystals. Background technique [0002] The existing technology is relatively successful in growing lead tungstate and some oxides with relatively high melting point doping modified lead tungstate crystals, but it encounters difficulties in growing dopant doping with low melting point and strong volatility, because in these When growing crystals in the device, it is usually necessary to reserve a part of the upper part of the crystal raw material in the crucible to accommodate the oxygen required for crystal growth. The temperature distribution in the crystal growth furnace is shown in Figure 1. The upper part has a higher temperature, and the crystal growth raw materials and dopants In the molten state, doped with non-volatile doping substances such as La 2 o 3 The effect of the reserved space on crystal growth is not very obvious, but ...

Claims

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Application Information

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IPC IPC(8): C30B29/32C30B11/00
Inventor 万尤宝刘俊星
Owner JIAXING UNIV
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