Thulium-doped lithium gadolinium lutetium fluoride middle-infrared laser crystal and preparation method thereof

A technology of thulium lutetium gadolinium lithium fluoride and lutetium gadolinium lithium fluoride, which is applied in the field of thulium-doped lutetium lutetium sodium fluoride laser glass and its preparation, can solve the problems of lack of original formula components, influence on crystal quality, equipment loss, etc., and achieve Improve crystal optical performance and utilization rate, high luminous efficiency, and save electricity cost

Inactive Publication Date: 2014-05-07
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, most fluoride crystals will volatilize during the high-temperature growth process to produce highly corrosive fluoride gas, which will cause damage to the equipment and may cause serious harm to the human body, especially due to the volatilization of the gas, causing the original formula components The lack of, affect the quality of the crystal

Method used

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  • Thulium-doped lithium gadolinium lutetium fluoride middle-infrared laser crystal and preparation method thereof
  • Thulium-doped lithium gadolinium lutetium fluoride middle-infrared laser crystal and preparation method thereof
  • Thulium-doped lithium gadolinium lutetium fluoride middle-infrared laser crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh raw material LiF with a purity greater than 99.99%, LuF with a purity of 99.99% 3 Raw material, 99.99% GdF 3 Raw material with 99.99% TmF 3 The raw materials were mixed according to the mole percentage of 51.5:41.0:7.0:0.5, placed in a mill, and milled and mixed for 5 hours to obtain a uniform powder mixture. Obtain the mixture of uniform powder; put the mixture loosely in the boat-shaped platinum crucible, then install the boat-shaped platinum crucible in the platinum pipeline of the tubular resistance furnace, and then use high-purity N 2 Gas removes the air in the platinum pipe, and conducts leak detection on the platinum pipe; then gradually raises the temperature of the furnace body of the tubular resistance furnace to 760°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...

Embodiment 2

[0024] It is basically the same as Example 1, except that LiF raw material is 51.50mol%, LuF 3 Raw material 40.5mol%, GdF3 raw material 7.0mol%, TmF 3 The raw material is 1.0mol%, the reaction time in the platinum tube is 6 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, Tm 3+ Doped LiLuGdF 4 crystals. Analysis and Detection of Gd in Crystal by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ with Tm 3+ The actual content of rare earth ions, the rare earth Gd in the single crystal 3+ The concentration is 5.61mol%, α=0.0561; Tm 3+ The concentration is 0.995 mol%, β=0.00995. 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. Absorption spectrum see fig...

Embodiment 3

[0026] It is basically the same as Example 1, except that LiF raw material is 51.50mol%, LuF 3 Raw material 39.7mol%, GdF3 raw material 7.0mol%, TmF 3 The raw material is 1.8mol%, the reaction time in the platinum tube is 4.5 hours, the temperature gradient of the solid-liquid interface is 70°C / cm°C / cm, the crystal growth rate is 1.2mm / h, and the furnace temperature drop temperature is 65°C / h, Tm 3+ Doped LiLuGdF 4 crystals. Analysis and Detection of Gd in Crystal by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ with Tm 3+ The actual content of rare earth ions, the rare earth Gd in the single crystal 3+ The concentration is 5.61mol%, α=0.0561; Tm 3+ The concentration is 1.79 mol%, β=0.0179. 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. Absorption spectrum see...

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Abstract

The invention discloses a thulium-doped lithium gadolinium lutetium fluoride middle-infrared laser crystal and a preparation method thereof. Tm<3+> rare earth ions are doped into a LiLuGdF crystal to generate a monocrystal of which the chemical formula is LiLu(1-alpha-beta)GdalphaTmbetaF4. The fluoride monocrystal has the advantages of low growth temperature, uniform distribution of Tm<3+>, high solubility, and favorable thermal, mechanical and chemical stability. The rare earth ions doped in the monocrystal have high luminescence efficiency; and by adopting a water-free oxygen-free sealed crucible descending process and carrying out high-temperature fluoridation treatment on the raw material, the preparation method can be used for preparing the high-quality crystal which is almost free of hydroxide ions and oxides. Under the excitation of an 800nm-wavelength LD, the crystal has strong 1.8 mu m fluorescence emission; and the obtained crystal has long fluorescence lifetime in the 1.8 mu m wave range, and thus, can be used as a middle-infrared laser crystal in a laser unit.

Description

technical field [0001] The invention relates to a special fluoride single crystal, in particular to a thulium-doped lutetium fluoride sodium laser glass and a preparation method thereof. Background technique [0002] by Tm 3+ In the fluoride crystal as the luminescent center, Tm 3+ Due to the strong energy cross-relaxation effect between ions ( 3 h 6 , 3 h 4 → 3 f 4 , 3 f 4 ), the quantum efficiency can reach 200% when excited by light, the rare earth ion Tm 3+ middle 3 f 4 → 3 h 6 The energy level transition of the can produce fluorescence radiation in the ~1.8μm band range. Most fluoride crystals such as LiYF 4 Single crystal, as a matrix, has lower phonon energy (300-500cm -1 ), can effectively inhibit Tm 3+ The radiation-free process greatly improves the Tm 3+ Luminous efficiency in the crystal; In addition, this type of fluoride single crystal as a matrix also has the characteristics of stable physical and chemical properties, good optical properties, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/12C30B11/00H01S3/16
Inventor 夏海平李珊珊符立董艳明唐磊汪沛渊彭江涛张约品
Owner NINGBO UNIV
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