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Prepn process of Ce-doped lanthanum oxide scintillation crystal

A scintillation crystal, lanthanum chloride technology, applied in chemical instruments and methods, crystal growth, single crystal growth and other directions, can solve the problems of moisture absorption or heating of raw materials, quality degradation, crystal defects increase, etc.

Inactive Publication Date: 2006-10-18
北京工物科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Prior art growth of Ce:LaCl 3 Scintillation crystals have the following disadvantages: Anhydrous LaCl 3 , CeCl 3 The surface activity of the raw material powder is very high, and the hygroscopicity is extremely strong. Therefore, the process of mixing raw materials and sealing the tubes must be carried out in an ultra-dry atmosphere, especially in the process of vacuum sealing the tubes. Due to the long operation time, The material tube must be heated, and a little carelessness can easily cause the raw material to absorb moisture or heat to cause LaCl 3 The hydrolysis reaction generates LaOCl impurities, and LaOCl becomes infusible La in the subsequent high-temperature melting process 2 o 3 , mixed with a trace amount of La 2 o 3 LaCl 3 The crystals grown from the melt are prone to cracking, which will at least cause more crystal defects and lower quality
In order to obtain high-quality LaCl 3 Crystal, the impurity content in the raw material is required to be less than 0.1%. See U.S. Pat. No: 20040238747A1. For this reason, the raw material needs to be purified by vacuum evaporation, which greatly increases the complexity of the process and the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of LaCl3 (3% CeCl3) cerium-doped lanthanum chloride scintillation crystal

[0034] The specific preparation process steps are as follows:

[0035] La with purity greater than 99.98% 2 O 3 , Into the vacuum drying oven at 200 ℃ -250 ℃ roasting for 10-30 hours.

[0036] According to the above chemical equation (1), the molar amount of the two components on the left side is NH 4 Ingredients with a large excess of Cl: The specific molar ratio is as follows:

[0037] La 2 O 3 : NH 4 Cl=1: (15)

[0038] Put the ingredients in step into a roasting furnace at a temperature of 150°C-300°C, in air, preferably in a nitrogen stream, for 20-60 hours. The firing container is a covered quartz cup or alumina ceramic cup, preferably alumina ceramic cup.

[0039] CeCl 3 ·6H 2 O and NH 4 Cl is prepared in the following proportions, and the specific molar ratio is as follows:

[0040] CeCl 3 ·6H 2 O: NH 4 Cl=1: (8)

[0041] The above ingredients are put into a quartz b...

Embodiment 2

[0046] Example 2: Preparation of LaCl3 (10% CeCl3) cerium-doped lanthanum chloride scintillation crystal

[0047] The specific preparation process steps are as follows:

[0048] La with purity greater than 99.98% 2 O 3 , Into the vacuum drying oven at 200 ℃ -250 ℃ roasting 10-30 hours.

[0049] According to the above chemical equation the molar amount of the two components on the left side is NH 4 Ingredients with a large excess of Cl: The specific molar ratio is as follows:

[0050] La 2 O 3 : NH 4 Cl=1: (19)

[0051] Put the ingredients in step into a roasting furnace at a temperature of 150°C-300°C, in air, preferably in a nitrogen stream, for 20-60 hours. The firing container is a covered quartz cup or alumina ceramic cup, preferably alumina ceramic cup.

[0052] CeCl 3 ·6H 2 O and NH 4 Cl is prepared in the following proportions, and the specific molar ratio is as follows:

[0053] CeCl 3 ·6H 2 O: NH 4 Cl=1: (10)

[0054] Put the above ingredients into a quartz boat and v...

Embodiment 3

[0059] Example 3: Preparation of LaCl3 (3% CeCl3) cerium-doped lanthanum chloride scintillation crystal

[0060] The specific preparation process steps are as follows:

[0061] La with purity greater than 99.98% 2 O 3 , Into the vacuum drying oven at 200 ℃ -250 ℃ roasting 10-30 hours.

[0062] Describe the chemical equation The molar amount of the two components on the left side is NH 4 Ingredients with a large excess of Cl:

[0063] The specific molar ratio is as follows:

[0064] La 2 O 3 : NH 4 Cl=1: (22)

[0065] Put the ingredients in step into a roasting furnace at a temperature of 150°C-300°C, in air, preferably in a nitrogen stream, for 20-60 hours. The firing container is a covered quartz cup or alumina ceramic cup, preferably alumina ceramic cup.

[0066] CeCl 3 ·6H 2 O and NH 4 Cl is prepared in the following proportions, and the specific molar ratio is as follows:

[0067] CeCl 3 ·6H 2 O: NH 4 Cl=1: (15)

[0068] Put the above ingredients into a quartz boat and vacu...

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PUM

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Abstract

The present invention is preparation process of Ce-doped lanthanum chloride scintillation crystal. The scintillation crystal has the chemical composition of La(1-x)CexCl3, where x is 0.01-0.2, and features that La2O3, anhydrous NH4Cl, CeCl3 .7H2O and other facile chemical materials are pretreated, converted and molten to form ingot and the ingot is set quartz ampoule bottle for growing Ce-doped lanthanum chloride scintillation crystal through a falling crucible process. The present invention has common industrial material adopted and simple production process, and the prepared crystal has relatively low oxygen impurity and relatively high optical quality.

Description

Technical field: [0001] The present invention relates to the field of crystal growth, in particular to a cerium-doped lanthanum chloride scintillation single crystal whose chemical composition is La 1-χ Ce χ Cl 3 (0.01≤χ≤0.3) and its growth method. Specifically involving the use of La as the initial raw material 2 O 3 , Anhydrous NH 4 Cl and CeCl 3 ·6H 2 Common chemical raw materials such as O, which are easily obtained, are pre-processed, transformed and melted into a block, and then put into a quartz ampoule, and the cerium-doped lanthanum chloride scintillation crystal is grown by the crucible descending method. Background technique: [0002] Scintillation crystals are widely used to detect high-energy particles such as gamma rays, X-rays, cosmic rays, electrons, and neutrons. The scintillation crystal emits light pulses under the action of radiation or particles. After the light pulses pass through the crystals, they are received by photomultiplier tubes, avalanche photodiode...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B15/04
Inventor 郝佳李端堂
Owner 北京工物科技有限责任公司
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