Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof

A technology of compound crystal and doping concentration, applied in the direction of crystal growth, polycrystalline material growth, 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: 2014-11-05
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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  • Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof
  • Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Embodiment 1: Five sections of Nd:Y 3 al 5 o 12 Concentration Gradient Composite Crystal

[0052] Preparation (Nd x Y 1-x ) 3 al 5 o 12 (x=x 1 , x 2 , x 3 , x 4 , x 5 )

[0053] The specific chemical formula is: 3xNd 2 o 3 +3(1-x)Y 2 o 3 +5Al 2 o 3 =2(Nd x Y 1-x ) 3 al 5 o 12

[0054] The raw material that present embodiment adopts is Nd 2 o 3 , Y 2 o 3 and Al 2 o 3, five different doping concentration x values ​​are taken in the proportioning, which are respectively x=0.1at%, 0.3at%, 0.5at%, 0.7at%, 0.9at%, and Nd 2 o 3 (4N), Y 2 o 3 (5N), and Al 2 o 3 (4N) The raw material is properly dried in the air, and then five parts of the material are strictly weighed according to five different stoichiometric ratios, and the five parts of the material are fully mixed respectively, and then put into a Pt crucible and sintered at 1000 ° C for 8 hours, the obtained polycrystalline material was ground with agate mortar and mortar to grind into f...

Embodiment 2

[0059] Embodiment 2: Five sections of Nd:Gd 3 Ga 5 o 12 Concentration Gradient Composite Crystal

[0060] Preparation (Nd x Gd 1-x ) 3 Ga 5 o 12 (x=x 1 , x 2 , x 3 , x 4 , x 5 ),

[0061] The specific chemical formula is: 3xNd 2 o 3 +3(1-x)Gd 2 o 3 +5Ga 2 o 3 =2(Nd x Gd 1-x ) 3 Ga 5 o 12

[0062] The raw material that present embodiment adopts is Nd 2 o 3 , Gd 2 o 3 and Ga 2 o 3 , five different doping concentration x values ​​are taken in the proportioning, which are respectively x=0.1at%, 0.3at%, 0.5at%, 0.7at%, 0.9at%, and Nd 2 o 3 (4N), Gd 2 o 3 (5N), and Ga 2 o 3 (4N) Raw materials were strictly weighed according to five different stoichiometric ratios, fully mixed, put into Pt crucibles and sintered at 1000-1100°C for 8 hours, and the obtained polycrystalline materials were ground into fine powders with an average particle size of 4 μm. Polycrystalline material rods were prepared according to the method of Example 1, wherein the length...

Embodiment 3

[0064] Embodiment 3: five sections of Nd:Lu 3 Ga 5 o 12 Concentration Gradient Composite Crystal

[0065] Preparation (Nd x Lu 1-x ) 3 Ga 5 o 12 (x=x 1 , x 2 , x 3 , x 4 , x 5 ),

[0066] The specific chemical formula is: 3xNd 2 o 3 +3(1-x)Lu 2 o 3 +5Ga 2 o 3 =2(Nd x Lu 1-x ) 3 Ga 5 o 12

[0067] The raw material that present embodiment adopts is Nd 2 o 3 , Lu 2 o 3 and Ga 2 o 3 , take five different numerical values ​​of doping concentration x in the proportioning, which are respectively x=0.1%, 0.3%, 0.5%, 0.75%, and 1%. The segment lengths are 15mm, 8mm, 8mm, 8mm and 15mm in sequence. The crystal growth period is one day, and five segments of Nd:Lu are obtained 3 Ga 5 o 12 The concentration gradient composite crystal has a total length of 44mm, and the lengths of each segment are 10mm, 8mm, 8mm, 8mm, and 10mm. The next five paragraphs Nd:Gd 3 Ga 5 o 12 The annealing and processing of the concentration gradient composite crystal are the ...

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Abstract

The invention relates to a garnet composite crystal with a multi-segment doping concentration gradient and a growing method thereof. The garnet composite crystal has the following structural general formula: (Lnx1Re1-x1) 3B2C3O12 / (Lnx2Re1-x2) 3B2C3O12 / (Lnx3Re1-x3) 3B2C3O12 / ... / (LnxnRe1-xn) 3B2C3O12, wherein Ln is equal to Nd or Yb or Tm or Ho, x1 is more than 0 and less than 1, x2 is more than 0 and less than 1, x3 is more than 0 and less than 1, xn is more than 0 and less than 1, and n is more than 3; Re is equal to Lu, Y or Gd; B is equal to Sc, Al or Ga; and C is equal to Al or Ga; and the garnet composite crystal has a garnet structure. 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, obvious gradient concentration segments and relatively simple process. The growing crystals have high transparency and few cracks and are suitable for growing of the garnet composite crystals with the concentration gradients.

Description

technical field [0001] The invention relates to a multi-segment doping concentration gradient garnet composite crystal and a growth 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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Patent Type & Authority Patents(China)
IPC IPC(8): H01S3/06H01S3/16C30B29/28C30B13/00
Inventor 张怀金武奎于浩海王继扬
Owner SHANDONG UNIV
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