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Ce<3+> doped gadolinium lithium fluoride ultraviolet laser crystal and preparation method thereof

A technology of lithium gadolinium fluoride and ultraviolet laser, applied in chemical instruments and methods, crystal growth, single crystal growth, etc., can solve problems affecting crystal utilization and quality, ion radius mismatch, and crystal cracking easily, etc. Achieve the effects of overcoming extremely uneven concentration distribution, preventing volatilization, and small crystal stress

Inactive Publication Date: 2014-05-28
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, in growing Ce 3+ :LiYF 4 Crystals have the following key technical issues: 1) Ce 3+ Doping is achieved by substituting Y 3+ Enter LiYF 4 Lattice, Ce 3+ (1.034 ) and Y 3+ (0.893 ); the ionic radius is very mismatched, the crystal stress obtained by growth is large, and the crystal is prone to cracking, due to Ce 3+ In LiYF 4 The segregation coefficient in the crystal is small and the distribution is extremely uneven, which affects the utilization rate and quality of the crystal; 2) LiYF 4 Fluoride crystals will volatilize and produce highly corrosive fluoride gas during the high-temperature growth process, which will cause loss to equipment, and may cause serious harm to the human body, especially due to the volatilization of the gas, resulting in the loss of the original formula components. missing, affecting the quality of the crystal

Method used

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  • Ce&lt;3+&gt; doped gadolinium lithium fluoride ultraviolet laser crystal and preparation method thereof
  • Ce&lt;3+&gt; doped gadolinium lithium fluoride ultraviolet laser crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh raw material LiF with a purity greater than 99.99%, GdF with a purity of 99.99% 3 Raw material with 99.99% CeF 3 The raw materials are mixed according to the molar percentage of 62.0:37.35:0.65, placed in a mill, and ground and mixed for 5 hours to obtain a uniform powder mixture; the mixture is fluffy placed in a boat-shaped platinum crucible, and then the boat-shaped platinum crucible is installed In the platinum tube of the tube resistance furnace, then use high-purity N 2 Gas removes the air in the platinum pipeline, and conducts leak detection on the platinum pipeline; then gradually raises the furnace body temperature of the tubular resistance furnace to 720°C, passes HF gas, and reacts for 3 hours to remove possible H 2 O and oxyfluoride, during the reaction process, use NaOH solution to absorb HF gas in the tail gas. After the reaction, stop passing HF gas, close the tube resistance furnace, and finally use high-purity N 2 The gas removes the residual HF...

Embodiment 2

[0026] It is basically the same as Example 1, except that LiF raw material is 62.0mol%, GdF 3 Raw material 36mol%, CeF 3 The raw material is 2.0mol%, the reaction time in the platinum tube is 5 hours, the temperature gradient of the solid-liquid interface is 65°C / cm, the crystal growth rate is 0.2mm / h, and the furnace temperature drop temperature is 80°C / h to obtain Ce 3+ Doped LiGdF 4 crystals. Cutting and sampling, the X-ray diffraction pattern of the sample is similar to that of Example 1. The rare earth Ce in the single crystal 3+ The concentration is 0.63 mol%, α=0.0063. The obtained sample was polished into the same 2 mm thick sheet as in Example 1, and the same optical test conditions as in Example 1 were maintained, and the obtained fluorescence intensity was comparable to that of the sample in Example 1. Under the light excitation of 296nm, the test of fluorescence spectrum is carried out, and the ultraviolet fluorescence emission in the band of 300-345nm is prod...

Embodiment 3

[0028] It is basically the same as Example 1, except that LiF raw material is 62.0mol%, GdF 3 Raw material 34.8mol%, CeF 3 The raw material is 3.2mol%, the reaction time in the platinum tube is 4.5 hours, the temperature gradient of the solid-liquid interface is 70°C / cm, the crystal growth rate is 1.2mm / h, and the furnace temperature drop temperature is 65°C / h to obtain Ce 3+ Doped LiGdF 4 crystals. Cutting and sampling, the X-ray diffraction pattern of the sample is similar to that of Example 1. The rare earth Ce in the single crystal 3+ The concentration is 1.01 mol%, α=0.0101. The obtained sample was polished into the same 2 mm thick sheet as in Example 1, and the same optical test conditions as in Example 1 were maintained, and the obtained fluorescence intensity was comparable to that of the sample in Example 1. Under the light excitation of 296nm, the test of fluorescence spectrum is carried out, and the ultraviolet fluorescence emission in the band of 300-345nm is ...

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Abstract

The invention discloses a Ce<3+> doped gadolinium lithium fluoride ultraviolet laser crystal and a preparation method thereof. Ce<3+> rare earth ions are doped into LiGdF4 crystals to generate monocrystals with the chemical formula of LiGd(1-alpha)CealphaF4. The fluoride monocrystals have the characteristics of low growth temperature, uniform distribution of Ce<3+>, small stress, and good calorimetric, mechanical and chemical stability. The preparation method adopts a water and oxygen insulation sealed crucible descent technology and allows raw materials to undergo high temperature fluorination treatment in order to obtain high-quality crystals containing almost no hydroxide ions. The crystals emit strong 300-345nm ultraviolet fluorescence under the excitation of light with the wavelength of 296nm, and can be expected to be applied in the laser medicine field, the material processing field, the laser spectroscopy field, the laser chemistry field and the like.

Description

technical field [0001] The invention relates to a special fluoride single crystal, in particular to a Ce 3+ Ion-doped gadolinium fluoride lithium ultraviolet laser crystal and its preparation method. Background technique [0002] Tunable short-wavelength ultraviolet lasers have important applications in laser medicine, material processing, laser spectroscopy, and laser chemistry. The short-wavelength tunable dye lasers currently used are subject to certain limitations because the dyes are prone to photodecomposition under the action of ultraviolet light; and color center and terminal phonon lasers are difficult to achieve continuous output in the ultraviolet band. [0003] Among all rare earth luminescent ions, due to Ce 3+ Ionic 4 f- 5 The d energy level transition can emit ultraviolet light with the shortest wavelength. Since 1980, some Ce-based 3+ Ion-doped various solid-state laser materials, but some of these materials quench the ultraviolet emission due to their ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/12C30B11/00
Inventor 夏海平董艳明符立李珊珊唐磊汪沛渊彭江涛张约品
Owner NINGBO UNIV
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