Ho<3+>/Yb<3+> double doped Alpha-NaYF4 laser crystal and preparation method thereof

A laser crystal and double-doping technology, applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems that limit the development of infrared laser crystals and devices, and it is difficult to mature LED lasers, so as to facilitate large-scale industrialization Production, single crystal with high purity and good quality

Active Publication Date: 2015-03-04
安徽靖芮精工技术有限公司
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Thanks to Ho 3+ The main absorption band is in the ultraviolet band, so it is difficult to have a matching mature LED laser as its pump source
thus limiting the Ho 3+ Development of single-doped mid-infrared laser crystals and devices

Method used

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  • Ho&lt;3+&gt;/Yb&lt;3+&gt; double doped Alpha-NaYF4 laser crystal and preparation method thereof
  • Ho&lt;3+&gt;/Yb&lt;3+&gt; double doped Alpha-NaYF4 laser crystal and preparation method thereof
  • Ho&lt;3+&gt;/Yb&lt;3+&gt; double doped Alpha-NaYF4 laser crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh NaF, KF, YF with a purity greater than 99.99% 3 、HoF 3 , YbF 3 Raw materials, by molar ratio NaF: KF: (YF 3 +HoF 3 +YbF 3 )=1.3:1:2.8, and HoF 3 : YbF 3 =1:2, YF 3 :HoF 3 =1:0.01, YF 3 : YbF 3 =1:0.02 Put the raw materials in a mill, grind and mix for 5.5 hours to obtain a uniform powder mixture; put the mixture in a boat-shaped platinum crucible, and then install the boat-shaped platinum crucible in a tubular resistance furnace in the platinum pipeline, 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 790°C, passes HF gas, and reacts for 2 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...

Embodiment 2

[0031] Substantially the same as Example 1, the difference is only in molar ratio NaF: KF: (YF 3 +HoF 3 +YbF 3 )=1.3:1:2.8, HoF 3 : YbF 3 =1:4, YF 3 :HoF 3 =1:0.01, YF 3 : YbF 3 =1:0.04 Place the raw materials in a mill, grind and mix for 5 hours to obtain a mixture of uniform powder; place the raw materials in the mill after mixing, and then gradually increase the temperature of the furnace body of the tubular resistance furnace to 780 ℃, with HF gas flowing, the reaction time is 3 hours, the furnace temperature is 980°C, the inoculation temperature is 860°C, the temperature gradient of the solid-liquid interface is 60°C / cm, the crystal growth rate is 0.2mm / h, and the furnace temperature drop temperature is 80°C / h, to transparent crystals. Analysis and Detection of Ho in Crystals by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ , Yb 3+ The actual molar content of rare earth ions, x = 0.99, y = 3.96, and the crystal chemical formula is α-NaY 0.950...

Embodiment 3

[0033] Substantially the same as Example 1, the difference is only in molar ratio NaF: KF: (YF 3 +HoF 3 +YbF 3 )=1.3:1:2.8, HoF 3 : YbF 3 =1:6, YF 3 :HoF 3 =1:0.01, YF 3 : YbF 3 =1:0.06 Place the raw materials in a mill, grind and mix for 5 hours to obtain a mixture of uniform powder; place the raw materials in the mill after mixing, and then gradually increase the furnace temperature of the tubular resistance furnace to 770 ℃, with HF gas flowing, the reaction time is 4 hours, the furnace temperature is 950℃, the inoculation temperature is 810℃, the temperature gradient of the solid-liquid interface is 65℃ / cm, the crystal growth rate is 0.2mm / h, and the furnace temperature drop temperature is 80°C / h, to transparent crystals. Analysis and Detection of Ho in Crystals by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ , Yb 3+ The actual molar content of rare earth ions is x=0.97, y=5.97, and the obtained crystal chemical formula is α-NaY 0.9306 Ho 0....

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Abstract

The invention discloses an Ho<3+>/Yb<3+> double doped Alpha-NaYF4 laser crystal and a preparation method thereof. The preparation method is characterized in that KF is taken as a fluxing agent, and is added in the raw materials of NaF, YF3, HoF3 and YbF3 to generate the Ho<3+>/Yb<3+> double doped Alpha-NaYF4 laser crystal. The preparation method has the advantages that because a certain quantity of KF (of which the melting point is 858 DEG C) is added in the initial raw materials as the fluxing agent, the fluxing agent KF reduces the melting point of the Alpha-NaYF4 laser crystal, and changes the phase equilibrium relation in the melt; when primary crystallization is begun in the melt, only solid phase of the Alpha-NaYF4 and other liquid phase are separated; the Alpha-NaYF4 laser crystal with a relatively large size is obtained eventually along with nucleus formation and growth of the Alpha-NaYF4 crystal; the NaYF4 monocrystal is high in solvability to rare earth, and has good thermal, mechanical and chemical stability; rare earth ions doped in the monocrystal are high in luminous efficiency.

Description

technical field [0001] The invention relates to a special fluoride single crystal, in particular to a Ho 3+ / Yb 3+ Double doped α-NaYF 4 Laser crystal and its preparation method. Background technique [0002] Solid-state lasers in the ~2.0μm band that are safe for human eyes have important applications in the fields of radar, remote sensing, ranging, environmental detection, bioengineering, and medical treatment. Rare earth ion Ho 3+ middle 5 I 7 → 5 I 8 The energy level transition can produce fluorescence radiation in the ~2μm band range, Ho 3+ Doped materials are expected to be developed into laser materials in the 2μm band. [0003] Currently as Ho 3+ Ion-doped mid-infrared host materials mainly include non-oxide glasses and crystals such as fluorides and chalcogenides with low phonon energy. Lower phonon energy, which can effectively suppress Ho 3+ The radiation-free process greatly improves the Ho 3+ luminous efficiency. For non-oxide glasses such as fluor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01F17/00
Inventor 杨硕夏海平姜永章张加忠符立董艳明李珊珊张约品
Owner 安徽靖芮精工技术有限公司
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