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Laser-activated vanadate composite crystal with ion doping concentration gradient and preparation method thereof

A gradient vanadate, composite crystal technology, applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve the problems of uncontrollable growth process of liquid phase epitaxy, a large number of bubbles and inclusions, and laser loss.

Active Publication Date: 2014-10-22
SHANDONG UNIV
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Problems solved by technology

However, these growth methods have their own shortcomings: the growth process of the hydrothermal method is complex and difficult to grow large sizes, the quality of the composite crystal grown by the pulling method is poor, there are a large number of defects such as bubbles and inclusions at the interface, and the growth process of the liquid phase epitaxy method is uncontrollable. It is difficult to achieve a high thickness of the composite layer. The thermal bonding method has relatively high requirements on the process, the production process has high requirements on the environment, and the conditions are relatively harsh. The bonded crystal interface is lossy to the laser.
The disadvantage of this method is that during the crystal growth process, the crystal needs to be cooled and taken out, and the three-stage YVO can be obtained by secondary growth. 4 / Nd 3+ :YVO 4 / YVO 4
Cannot grow target crystals at once

Method used

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  • Laser-activated vanadate composite crystal with ion doping concentration gradient and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1: Five sections of Nd: YVO 4 Concentration Gradient Composite Crystal

[0052] Preparation of Nd x Y 1-x VO 4 (x=x 1 , x 2 , x 3 , x 4 , x 5 ), the chemical equation is:

[0053] wxya 2 o 3 +(1-x)Y 2 o 3 +V 2 o 5 =2Nd x Y 1-x VO 4 ;

[0054] The raw material is Nd 2 o 3 , Y 2 o 3 and V 2 o 5 , five different values ​​of doping concentration x are taken in the ratio, which are respectively x 1 = 0.1at%, x 2 = 0.3at%, x 3 = 0.5at%, x 4 = 0.7at%, x 5 =0.9at%, the Nd 2 o 3 (4N), Y 2 o 3 (5N), and V 2 o 5 (4N) Raw material, dry properly in the air, and then strictly weigh five parts according to five different stoichiometric ratios, and mix the five parts fully, and put them into a Pt crucible in turn at 1000-1100 °C Sintering for 8 hours, the obtained polycrystalline material was ground with agate mortar and pestle respectively, and ground into fine powder, which was ground into fine powder with an average particle size of 4 μm...

Embodiment 2

[0057] Embodiment 2: Five sections of Nd:GdVO 4 Concentration Gradient Composite Crystal

[0058] Preparation of Nd x Gd 1-x VO 4 (x=x 1 , x 2 , x 3 , x 4 , x 5 ), the chemical equation is:

[0059] wxya 2 o 3 +(1-x)Gd 2 o 3 +V 2 o 5 =2Nd x Gd 1-x VO 4 ;

[0060] The raw material used is Nd 2 o 3 , Gd 2 o 3 and V 2 o 5 , take five different values ​​of doping concentration x in the ratio, which are 0.1at%, 0.3at%, 0.5at%, 0.7at%, 0.9at%, and Nd 2 o 3 (4N), Gd 2 o 3 (5N), and V 2 o 5 (4N) Raw materials, weighed according to five different stoichiometric ratios, fully mixed, put into Pt crucibles and sintered at 1000-1100°C for 8 hours to obtain five polycrystalline materials with different ratios, ground into fine powder and averaged The particle size is 4 μm, and the polycrystalline rod prepared by the method of Example 1 is loaded into a floating zone growth furnace for crystal growth. All the other operations are the same as in Example 1.

Embodiment 3

[0061] Embodiment 3: five sections of Nd:LuVO 4 Concentration Gradient Composite Crystal

[0062] Preparation of Nd x Lu 1-x VO 4 (x=x 1 , x 2 , x 3 , x 4 , x 5 ), the chemical equation is:

[0063] wxya 2 o 3 +(1-x)Lu 2 o 3 +V 2 o 5 =2Nd x Lu 1-x VO 4 ;

[0064] The raw material used is Nd 2 o 3 , Lu 2 o 3 and V 2 o 5 , the doping concentrations are x=0.1at%, 0.3at%, 0.5at%, 0.7at%, 0.9at%, respectively. Thereafter, the preparation of raw materials, preparation of polycrystalline rods, and crystal growth, annealing, and processing are the same as in Example 1.

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Abstract

The invention relates to a vanadate composite crystal with a laser active ion doping concentration gradient and a preparation method thereof. The vanadate composite crystal has the following structural general formula: Lnx1Re1-x1VO4 / Lnx2Re1-x2VO4 / Lnx3Re1-x3VO4 / ... / Lnx (n-1) Re1-x (n-1) VO4 / LnxnRe1-xnVO4, wherein n is more than 3; Ln is equal to Nd, Yb or Tm or Ho; and Re is equal to Lu, Y or Gd. The growing method comprises the following steps of: making the composite crystal grow by an optical float-zone method; proportioning the raw materials according to chemometry in the general formula; preparing polycrystal charge bars according to the predesigned segments and length; and loading the polycrystal charge bars into an optical float-zone furnace for growing. The method has the advantages of high speed, short cycle, no crucible in the process crystal growth, less pollution on crystals, and obvious gradient concentration segments. The growing crystals have high transparency and few cracks and are used for manufacturing laser devices.

Description

technical field [0001] The invention relates to a multi-segment concentration gradient vanadate composite crystal and a preparation method thereof, in particular to the field of application to high-power laser devices. Background technique [0002] Laser diode (LD)-pumped solid-state lasers have the advantages of compact structure, high efficiency, good stability, and long life, and have broad application prospects in scientific research, medical treatment, communication, military and other fields. As a key part of solid-state lasers, gain media doped with rare earth ions or transition metal ions have been studied and applied a lot, among which garnet and vanadate crystals are widely used. The traditional gain medium usually adopts a crystal structure with a single doping concentration. This kind of gain medium depends on the pump power density and the concentration of dopant ions in the crystal due to the increase of temperature under higher pump power. In general, when th...

Claims

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Application Information

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IPC IPC(8): C30B29/30C30B13/00
Inventor 张怀金武奎于浩海王继扬
Owner SHANDONG UNIV
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