CN1292107C - Growth method of neodymium-doped gadolinium gallium garnet laser crystal - Google Patents
Growth method of neodymium-doped gadolinium gallium garnet laser crystal Download PDFInfo
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- CN1292107C CN1292107C CN 200410067129 CN200410067129A CN1292107C CN 1292107 C CN1292107 C CN 1292107C CN 200410067129 CN200410067129 CN 200410067129 CN 200410067129 A CN200410067129 A CN 200410067129A CN 1292107 C CN1292107 C CN 1292107C
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- neodymium
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Abstract
The present invention relates to a growth method of laser crystals of neodymium-doped gadolinium gallium garnet. Gadolinium oxide, gallium oxide, neodymium oxide and cerium oxide are primarily used as raw materials which are prepared by a two-step synthesis method according to a proportion, and the growth of laser crystals is realized by a crystal pulling method under the condition of 98% of nitrogen and 2% of oxygen. The present invention solves the problem of lattice distortion caused by O<2-> introduction due to doped Nd2O3 existing in the prior art, enhances the irradiation preventing capability of crystals and improves the spectral performance and the laser performance of crystals of Nd and GGG.
Description
Technical field
The present invention relates to Nd-Gd-Ga garnet (Nd
3+: Gd
3Ga
5O
12Laser crystals, hereinafter to be referred as: the growth method of Nd:GGG, particularly a kind of neodymium-doped gadolinium gallium garnet laser crystal.
Background technology
High power solid state laser has the requirement of a series of strictnesses to laser crystals: big absorption cross and emission cross section, little Stokes shift, long fluorescence lifetime, high thermomechanical property and the crystal that can grow into the large size high optical quality.The subject matter that faces of high power solid state laser is the heat collapse in the pumping process.Even the use diode pumping also has very considerable a part of heat and absorbed by laser medium, thereby the thermal lensing effect of causing, mechanical stress and other effect.
Nd:GGG grows under smooth solid-liquid interface easily, there are not other impurity and center of stress, whole cross section all can effectively utilize, obtain being applied to the large size lath and the fuel plate of superpower laser easily, and Nd:GGG has good mechanics and chemical stability, high thermal conductivity, wide pump absorption band, long fluorescence lifetime, the absorption of pump light and energy storage are all better, can realize the running of continous way or pulse type laser.Nd:GGG has become one of preferred material of high average power solid laser device.
Because the Nd:GGG crystal is mainly used in the high average power solid laser device, will have powerful energy stream in the course of the work, be the emphasis that people study so how to increase the anti-irradiation ability of crystalline.
Summary of the invention
The problem of the problem to be solved in the present invention is to overcome the defective of above-mentioned prior art, solves because of mixing Nd
2O
3And the lattice distortion problem that causes provides a kind of method of the Nd:GGG of preparation laser crystals, reduces Nd:GGG crystalline defective dislocation, improves the anti-irradiation ability of Nd:GGG.
Reaction equation in the process of growth of the present invention:
Technical solution of the present invention is as follows:
A kind of growth method of neodymium-doped gadolinium gallium garnet laser crystal mainly is to mix CeO simultaneously in GGG crystal growth prescription
2, because Ce
3+Can be effectively the energetic ray of irradiation be converted into fluorescence, so can effectively improve the anti-irradiation ability of Nd:GGG.
The growth method of neodymium-doped gadolinium gallium garnet laser crystal of the present invention is characterized in that may further comprise the steps:
1. by following mole proportioning weighing following raw materials:
Raw material mol
Gd
2O
3 3(1-x-y)
Ga
2O
3 5.1
Nd
2O
3 y
CeO
2 6x
The span of x: 0.001mol≤X≤0.005mol wherein
The span of y: 0.005mol≤y≤0.1mol;
2. with above-mentioned raw materials behind thorough mixing, use the hydropress briquetting, 1200 ℃ of following sintering 12 hours;
3. the crystal pulling method single crystal growing furnace of packing into vacuumizes, and charges into 98% nitrogen+2% oxygen, and the significant parameter of crystal growth is: pull rate=2-5mm/h, speed of rotation=10-15rpm;
4. crystal growth finishes, and adopts the method for in-situ annealing slowly to reduce to room temperature, takes out crystal.
Crystal pulling method (Czochralski) growth of Nd that the present invention is used: GGG crystalline device is common Frequency Induction Heating single crystal growing furnace.It comprises parts such as iridium crucible, vacuum system, Medium frequency induction generator power and temperature control system.
Technique effect of the present invention:
The neodymium-doped gadolinium gallium garnet laser crystal of present method growth, after tested, Nd
3+The concentration uniform distribution, dislocation desity obviously reduces, and anti-irradiation ability is significantly strengthened, the also corresponding raising of spectrum property.
Mix CeO in the GGG crystal growth prescription
2, because Ce
3+Can be effectively the energetic ray of irradiation be converted into fluorescence, so can effectively improve the anti-irradiation ability of Nd:GGG, method is simple.
Embodiment
The invention will be further described below by embodiment, but should not limit protection scope of the present invention with this.
Embodiment 1:
With above-mentioned proportioning raw materials and technical process growth of Nd: the GGG crystal, get x=0.001 in the proportioning raw materials, Y=0.005.At first with Gd
2O
3, Ga
2O
3, Nd
2O
3And CeO
2Weigh by said ratio, after mechanically mixing is even, 1400 ℃ of sintering in retort furnace, the growing single-crystal stove of packing into vacuumizes, and charges into 98% nitrogen+2% oxygen, pull rate: 2mm/h, speed of rotation: 15rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal.After tested, Nd
3+The concentration uniform distribution detects and spectrum test through dislocation, and the result bits dislocation density obviously reduces, and anti-irradiation ability is effectively improved.The also corresponding raising of spectrum property.
Embodiment 2:
With above-mentioned proportioning raw materials and technical process growth of Nd: the GGG crystal, get x=0.002 in the proportioning raw materials, Y=0.1.At first with Gd
2O
3, Ga
2O
3, Nd
2O
3And CeO
2Weigh by said ratio, after mechanically mixing was even, with 1500 ℃ of sintering, the growing single-crystal stove of packing into vacuumized in retort furnace, charges into 98% nitrogen+2% oxygen, pull rate: 2.5mm/h, speed of rotation: 14rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal, Nd
3+The concentration uniform distribution detects and spectrum test through dislocation, and the result bits dislocation density obviously reduces, and anti-irradiation ability is effectively improved.The also corresponding raising of spectrum property.
Embodiment 3:
With above-mentioned proportioning raw materials and technical process growth of Nd: the GGG crystal, get x=0.003 in the proportioning raw materials, Y=0.6.At first with Gd
2O
3, Ga
2O
3, Nd
2O
3And CeO
2Weigh by said ratio, mechanically mixing evenly after, in retort furnace with 1100 ℃ of sintering, the growing single-crystal stove of packing into, vacuumize, charge into 98% nitrogen+2% oxygen, pull rate: 3mm/h, speed of rotation: 16rpm, behind the growing crystal, slowly reduce to room temperature, take out crystal.After tested, Nd
3+The concentration uniform distribution detects and spectrum test through dislocation, and the result bits dislocation density obviously reduces, and anti-irradiation ability is effectively improved.The also corresponding raising of spectrum property.
Embodiment 4:
With above-mentioned proportioning raw materials and technical process growth of Nd: the GGG crystal, get x=0.005 in the proportioning raw materials, Y=0.04.At first with Gd
2O
3, Ga
2O
3, Nd
2O
3And CeO
2Weigh by said ratio, after mechanically mixing was even, with 1200 ℃ of sintering, the growing single-crystal stove of packing into vacuumized in retort furnace, charges into 98% nitrogen+2% oxygen, pull rate: 2.5mm/h, speed of rotation: 10rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal, Nd
3+The concentration uniform distribution detects and spectrum test through dislocation, and the result bits dislocation density obviously reduces, and anti-irradiation ability is effectively improved.The also corresponding raising of spectrum property.
Embodiment 5:
With above-mentioned proportioning raw materials and technical process growth of Nd: the GGG crystal, get x=0.005 in the proportioning raw materials, Y=0.003.At first with Gd
2O
3, Ga
2O
3, Nd
2O
3And CeO
2Weigh by said ratio, after mechanically mixing was even, with 1600 ℃ of sintering, the growing single-crystal stove of packing into vacuumized in retort furnace, charges into 98% nitrogen+2% oxygen. pull rate: 2.5mm/h, speed of rotation: 16rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal.Nd after tested
3+The concentration uniform distribution detects and spectrum test through dislocation, and the result bits dislocation density obviously reduces, and anti-irradiation ability is effectively improved.The also corresponding raising of spectrum property.
Claims (1)
1, a kind of growth method of neodymium-doped gadolinium gallium garnet laser crystal is characterized in that may further comprise the steps:
1. by following mole proportioning weighing following raw materials:
Raw material mol
Gd
2O
3 3(1-x-y)
Ga
2O
3 5.1
Nd
2O
3 y
CeO
2 6x
The span of x: 0.001mol≤X≤0.005mol wherein
The span of y: 0.005mol≤y≤0.1mol;
2. with above-mentioned raw materials behind thorough mixing, use the hydropress briquetting, 1200 ℃ of following sintering 12 hours;
3. the Czochralski grown single crystal growing furnace of packing into vacuumizes, and charges into 98% nitrogen+2% oxygen, and the significant parameter of crystal growth is: pull rate=2-5mm/h, speed of rotation=10-15rpm;
4. crystal growth finishes, and adopts the method for in-situ annealing slowly to reduce to room temperature, takes out crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067129 CN1292107C (en) | 2004-10-13 | 2004-10-13 | Growth method of neodymium-doped gadolinium gallium garnet laser crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410067129 CN1292107C (en) | 2004-10-13 | 2004-10-13 | Growth method of neodymium-doped gadolinium gallium garnet laser crystal |
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|---|---|
| CN1621576A CN1621576A (en) | 2005-06-01 |
| CN1292107C true CN1292107C (en) | 2006-12-27 |
Family
ID=34765004
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|---|---|---|---|
| CN 200410067129 Expired - Fee Related CN1292107C (en) | 2004-10-13 | 2004-10-13 | Growth method of neodymium-doped gadolinium gallium garnet laser crystal |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319389B (en) * | 2008-05-22 | 2011-05-11 | 成都东骏激光股份有限公司 | Preparation method of gadolinium gallium garnet planar interface crystal |
| CN102134749A (en) * | 2010-01-22 | 2011-07-27 | 中国科学院福建物质结构研究所 | Dysprosium ion activated gadolinium gallium garnet novel laser crystal |
| CN110453284A (en) * | 2018-05-08 | 2019-11-15 | 安徽科瑞思创晶体材料有限责任公司 | A kind of GAGG scintillation crystal manufacturing method |
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2004
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Granted publication date: 20061227 Termination date: 20111013 |