CN103074685A - High concentration Nd-doped YAG laser crystal growth method - Google Patents
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- 239000013078 crystal Substances 0.000 claims abstract description 168
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- 230000006698 induction Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 14
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- 229910052741 iridium Inorganic materials 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
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- 239000000155 melt Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
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- 229910052786 argon Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
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- 229920000126 latex Polymers 0.000 claims description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 5
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- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
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Abstract
本发明公开一种高浓度Nd掺杂YAG激光晶体生长方法，该方法基于中频感应激光晶体炉，该方法涉及掺钕钇铝石榴石工艺领域，包括七个步骤4个阶段的生长方法。本发明所提供的高浓度Nd掺杂YAG激光晶体生长方法可获得直径Ф25～45mm、掺钕浓度1.17～1.41at%、浓度梯度小、散射颗粒少、质量较高的Nd:YAG激光晶体，工艺稳定，晶体成炉率较高，具有很好的应用前景。
The invention discloses a high-concentration Nd-doped YAG laser crystal growth method. The method is based on an intermediate-frequency induction laser crystal furnace. The method relates to the field of neodymium-doped yttrium aluminum garnet technology, and includes seven steps and four stages of growth methods. The high-concentration Nd-doped YAG laser crystal growth method provided by the present invention can obtain Nd:YAG laser crystals with a diameter of 25-45mm, a neodymium-doped concentration of 1.17-1.41at%, a small concentration gradient, few scattering particles, and high quality. It is stable, has a high crystal formation rate, and has a good application prospect.
Description
Technical field
The present invention relates to neodymium-doped yttrium-aluminum garnet technology field (abbreviation Nd:YAG), particularly a kind of high density Nd doping YAG laser crystal growth method.
Background technology
The Nd:YAG laser crystals has the advantages such as optical homogeneity is good, high gain, good mechanical property, is one of best, the most frequently used at present solid laser material.Because the application popularization of solid high power pulse laser welding technique and equipment, accelerated solid statelaser towards superpower, high-level efficiency, the future development of high light velocity quality, demand to high quality YAG series laser crystal increases rapidly, the used Nd:YAG laser crystal material of high power laser is by the Medium frequency induction Czochralski grown at present, the highest 1.1at% that is no more than of its neodymium-doped concentration, cause it by using large size Nd:YAG laser crystal bar or lath-shaped dual-tripler to obtain high-power output, and the use of large size Nd:YAG laser crystals can strengthen the difficulty of cooling, again because the little defective of quantum benefit of himself, be easy to produce thermal lensing effect when working long hours, can make the Laser output Efficiency Decreasing.Investigators had carried out the research of high neodymium-doped Nd:YAG laserable material and substitute in the last few years, such as the terraced method growth of temperature high density, large size Nd:YAG laser crystals, the Nd:YAG transparent laser ceramic that the development doping content is high etc., but because defective is more or also in the stage of fumbling, application all is very limited.
Summary of the invention
Based on this, for above-mentioned problems of the prior art, the object of the present invention is to provide the high density Nd doping YAG laser crystal growth method that a kind of neodymium-doped concentration is high, concentration gradient is little, scattering particles are few, quality is higher.
For achieving the above object, technical solution of the present invention is:
A kind of high density Nd doping YAG laser crystal growth method, the method comprises step based on the Medium frequency induction laser crystal growth furnace:
S1. with purity more than or equal to 99.999% yttrium oxide Y
2O
3, aluminium oxide Al
2O
3, Neodymium trioxide Nd
2O
3600 ~ 800 ℃ of lower calcinations 4 ~ 8 hours, again by default neodymium-doped concentration calculate, weighing is configured to bed material;
S2. the bed material for preparing among the step S1 is packed in the Plastic Bottle, be fixed on the mixer and fully mixed 24 ~ 48 hours;
S3. the powder that mixes among the step S2 is put into the latex mould, pass through again 200 ~ 300MPa isostatic pressing after the sealing;
S4. seed crystal is put into the iridium crucible seed rod of required employing;
S5. the raw material of moulding is put into the iridium crucible of diameter 60～120mm, vacuumized after adjusting the concentricity of coil, heat-insulation system, seed crystal, iridium crucible, when body of heater vacuum tightness reaches 3.5 ~ 4.5Pa, pour argon gas;
S6. starting the Medium frequency induction laser crystal growth furnace heats up the heating system in the burner hearth, after raw material in iridium crucible described in the step S5 all melts, the melt liquid fluid line begins slowly to descend seed crystal when steady and audible, contact liquid level elapsed-time standards is about 1～2 hour from lower seed crystal to seed crystal, and constant temperature was 1 ~ 2 hour when the adjusting melt temperature made seed crystal reduced 1 ~ 2mm;
S7. lift seed crystal, the growth of beginning crystal, its direction of growth is＜111 〉, the crystal growth comprises 4 stages:
In the shouldering stage, brilliant raising speed rate is 0.6～0.7mm/h during shouldering, and brilliant rotational speed rate is 16～18 rev/mins, and the shouldering angle is controlled at 40
O~ 50
O, at crystal shouldering growth later stage brilliant raising speed rate to the 0.5～0.55mm/h that will progressively slow down, reducing brilliant rotational speed rate to 14～15 rev/min, it is mild that temperature rate is wanted, and when shouldering place diameter and crystal target diameter differ 2 ~ 4mm, begins constant temperature;
Deng through growth phase, the growth of crystal constant temperature entered the isodiametric growth stage after 15～48 hours, brilliant raising speed rate slows to 0.4～0.45mm/h along with the length increase of isodiametric growth of crystal, brilliant rotational speed rate slowly is decreased to 12～13 rev/mins, crystal growth temperature control speed span can not be excessive, makes the crystal diameter deviation control within 1 ~ 2mm;
The ending stage, the crystal growth begins the ending that heats up after reaching predetermined length, along with diminishing of crystal diameter slowly improved brilliant raising speed rate to 0.6～0.65mm/h, brilliant rotational speed rate also will progressively slow to 9～11 rev/mins, when crystal diameter is reduced to 4～6mm left and right sides, carried out isodiametric growth 8～10 hours, at last cooling makes the crystal diameter change expand into greatly " lid " type again, to prevent crystal cleavage and protection crucible;
Temperature-fall period, crystal growth finish rear temperature with vitellarium in the rate reduction iridium crucible of 10～80 ℃/h, until room temperature.
The high density Nd doping YAG laser crystal growth method that this programme provides can obtain diameter Ф 25～45mm, neodymium-doped concentration 1.17～1.41 at%, concentration gradient is little, scattering particles are few, quality is higher Nd:YAG laser crystals, process stabilizing, crystal become the stove rate higher.This product is made when laser apparatus uses has the advantages that the Output of laser energy is high, service efficiency is high, is suitable for superpower continuous wave laser or pulsed laser; Also can satisfy the miniature laser application demand of some needs output high-powers, have good application prospect.
Further, in one embodiment, the vision slit outer end of described Medium frequency induction laser crystal growth furnace is equipped with YAG polishing eyeglass.In order to reduce radially heat dissipation capacity of crystal, reduce radially thermal stresses, further promote crystal quality.
Further, in one embodiment, the zirconium white annulus is equipped with in the shielding at described Medium frequency induction laser crystal growth furnace top upper end.Axial-temperature gradient when lifting to cold zone in order to reduce crystal further promotes crystal quality.
Further, in one embodiment, the purity of argon that pours among the described step S5 is more than or equal to 99.9999%.Effectively reduce the crucible loss, promote the quality of crystal, prolong pot life.
Compared with prior art, the present invention has following beneficial effect: high density Nd doping YAG laser crystal growth method provided by the present invention can obtain diameter Ф 25～45mm, neodymium-doped concentration 1.17～1.41 at%, concentration gradient is little, scattering particles are few, quality is higher Nd:YAG laser crystals, process stabilizing, crystal becomes the stove rate higher, has good application prospect.
Description of drawings
Fig. 1 is embodiment of the invention Medium frequency induction laser crystal growth furnace structural representation.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment one
A kind of high density Nd doping YAG laser crystal growth method, the method is based on the Medium frequency induction laser crystal growth furnace, and it comprises step:
S1. with purity more than or equal to 99.999% yttrium oxide Y
2O
3, aluminium oxide Al
2O
3, Neodymium trioxide Nd
2O
3600 ℃ of lower calcinations 8 hours, again by default neodymium-doped concentration calculate, weighing is configured to bed material;
S2. the bed material for preparing among the step S1 is packed in the Plastic Bottle, be fixed on the mixer and fully mixed 48 hours;
S3. the powder that mixes among the step S2 is put into the latex mould, pass through again the 300MPa isostatic pressing after the sealing;
S4. seed crystal is put into the iridium crucible seed rod of required employing;
S5. the raw material of moulding is put into the iridium crucible of diameter 60～120mm, vacuumized after adjusting the concentricity of coil, heat-insulation system, seed crystal, iridium crucible, when body of heater vacuum tightness reaches the 4.5Pa left and right sides, pour purity greater than 99.9999% argon gas;
S6. starting the Medium frequency induction laser crystal growth furnace heats up the heating system in the burner hearth, after raw material in iridium crucible described in the step S5 all melts, the melt liquid fluid line begins slowly to descend seed crystal when steady and audible, contact liquid level elapsed-time standards is about 2 hours from lower seed crystal to seed crystal, and constant temperature was 2 hours when the adjusting melt temperature made seed crystal reduced 2mm;
S7. lift seed crystal, the growth of beginning crystal, its direction of growth is＜111 〉, the crystal growth comprises 4 stages:
In the shouldering stage, brilliant raising speed rate is 0.7mm/h during shouldering, and brilliant rotational speed rate is 18 rev/mins, and the shouldering angle is controlled at 50
O, the later stage to progressively slow down brilliant raising speed rate to 0.55mm/h in crystal shouldering growth, reduce brilliant rotational speed rate to 15 rev/min, it is mild that rate of temperature fall is wanted, and when shouldering place diameter and crystal target diameter differ 4mm, begins constant temperature;
Deng through growth phase, the growth of crystal constant temperature entered the isodiametric growth stage after 48 hours, brilliant raising speed rate slows to 0.45mm/h along with the length increase of isodiametric growth of crystal, brilliant rotational speed rate slowly is decreased to 13 rev/mins, crystal growth temperature control speed span can not be excessive, makes the crystal diameter deviation control within 2mm;
The ending stage, the crystal growth begins the ending that heats up after reaching predetermined length, along with diminishing of crystal diameter slowly improved brilliant raising speed rate to 0.65mm/h, brilliant rotational speed rate also will progressively slow to 11 rev/mins, when crystal diameter is reduced to the 6mm left and right sides, carried out isodiametric growth 10 hours, at last cooling makes the crystal diameter change expand into greatly " lid " type again, to prevent crystal cleavage and protection crucible;
Temperature-fall period, crystal growth finish rear temperature with vitellarium in the rate reduction iridium crucible of 70 ℃/h, until room temperature.
The vision slit outer end of described Medium frequency induction laser crystal growth furnace is equipped with YAG polishing eyeglass.In order to reduce radially heat dissipation capacity of crystal, reduce radially thermal stresses, further promote crystal quality
The zirconium white annulus is equipped with in the shielding upper end at described Medium frequency induction laser crystal growth furnace top.Axial-temperature gradient when lifting to cold zone in order to reduce crystal further promotes crystal quality.
Embodiment two
A kind of high density Nd doping YAG laser crystal growth method, the method is based on the Medium frequency induction laser crystal growth furnace, and it comprises step:
S1. with purity more than or equal to 99.999% yttrium oxide Y
2O
3, aluminium oxide Al
2O
3, Neodymium trioxide Nd
2O
3700 ℃ of lower calcinations 5 hours, again by default neodymium-doped concentration calculate, weighing is configured to bed material;
S2. the bed material for preparing among the step S1 is packed in the Plastic Bottle, be fixed on the mixer and fully mixed 30 hours;
S3. the powder that mixes among the step S2 is put into the latex mould, pass through again the 250MPa isostatic pressing after the sealing;
S4. seed crystal is put into the iridium crucible seed rod of required employing;
S5. the raw material of moulding is put into the iridium crucible of diameter 60～120mm, vacuumized after adjusting the concentricity of coil, heat-insulation system, seed crystal, iridium crucible, when body of heater vacuum tightness reaches the 4Pa left and right sides, pour purity greater than 99.9999% argon gas;
S6. starting the Medium frequency induction laser crystal growth furnace heats up the heating system in the burner hearth, after raw material in iridium crucible described in the step S5 all melts, the melt liquid fluid line begins slowly to descend seed crystal when steady and audible, contact liquid level elapsed-time standards is about 1.5 hours from lower seed crystal to seed crystal, and constant temperature was 1.5 hours when the adjusting melt temperature made seed crystal reduced 1.5mm;
S7. lift seed crystal, the growth of beginning crystal, its direction of growth is＜111 〉, the crystal growth comprises 4 stages:
In the shouldering stage, brilliant raising speed rate is 0.65mm/h during shouldering, and brilliant rotational speed rate is 17 rev/mins, and the shouldering angle is controlled at 45
O, the later stage to progressively slow down brilliant raising speed rate to 0.52mm/h in crystal shouldering growth, reduce brilliant rotational speed rate to 14.5 rev/min, it is mild that temperature rate is wanted, and when shouldering place diameter and crystal target diameter differ 3mm, begins constant temperature;
Deng through growth phase, the growth of crystal constant temperature entered the isodiametric growth stage after 23 hours, brilliant raising speed rate slows to 0.42mm/h along with the length increase of isodiametric growth of crystal, brilliant rotational speed rate slowly is decreased to 12 rev/mins, crystal growth temperature control speed span can not be excessive, makes the crystal diameter deviation control within 1.5mm;
The ending stage, the crystal growth begins the ending that heats up after reaching predetermined length, along with diminishing of crystal diameter slowly improved brilliant raising speed rate to 0.62mm/h, brilliant rotational speed rate also will progressively slow to 10 rev/mins, when crystal diameter is reduced to the 5mm left and right sides, carried out isodiametric growth 9 hours, at last cooling makes the crystal diameter change expand into greatly " lid " type again, to prevent crystal cleavage and protection crucible;
Temperature-fall period, crystal growth finish rear temperature with vitellarium in the rate reduction iridium crucible of 30 ℃/h, until room temperature.
The vision slit outer end of described Medium frequency induction laser crystal growth furnace is equipped with YAG polishing eyeglass.In order to reduce radially heat dissipation capacity of crystal, reduce radially thermal stresses, further promote crystal quality
The zirconium white annulus is equipped with in the shielding upper end at described Medium frequency induction laser crystal growth furnace top.Axial-temperature gradient when lifting to cold zone in order to reduce crystal further promotes crystal quality.
Embodiment three
A kind of high density Nd doping YAG laser crystal growth method, the method is based on the Medium frequency induction laser crystal growth furnace, and it comprises step:
S1. with purity more than or equal to 99.999% yttrium oxide Y
2O
3, aluminium oxide Al
2O
3, Neodymium trioxide Nd
2O
3800 ℃ of lower calcinations 4 hours, again by default neodymium-doped concentration calculate, weighing is configured to bed material;
S2. the bed material for preparing among the step S1 is packed in the Plastic Bottle, be fixed on the mixer and fully mixed 24 hours;
S3. the powder that mixes among the step S2 is put into the latex mould, pass through again isostatic pressing after the sealing;
S4. seed crystal is put into the iridium crucible seed rod of required employing;
S5. the raw material of moulding is put into the iridium crucible of diameter 60～120mm, vacuumized after adjusting the concentricity of coil, heat-insulation system, seed crystal, iridium crucible, when body of heater vacuum tightness reaches the 3.5Pa left and right sides, pour purity greater than 99.9999% argon gas;
S6. starting the Medium frequency induction laser crystal growth furnace heats up the heating system in the burner hearth, after raw material in iridium crucible described in the step S5 all melts, the melt liquid fluid line begins slowly to descend seed crystal when steady and audible, contact liquid level elapsed-time standards is about 1 hour from lower seed crystal to seed crystal, and constant temperature was 1 hour when the adjusting melt temperature made seed crystal reduced 1mm;
S7. lift seed crystal, the growth of beginning crystal, its direction of growth is＜111 〉, the crystal growth comprises 4 stages:
In the shouldering stage, brilliant raising speed rate is 0.6mm/h during shouldering, and brilliant rotational speed rate is 16 rev/mins,, the shouldering angle is controlled at 40
O, the later stage to progressively slow down brilliant raising speed rate to 0.5mm/h in crystal shouldering growth, reduce brilliant rotational speed rate to 14 rev/min, it is mild that temperature rate is wanted, and when shouldering place diameter and crystal target diameter differ 2mm, begins constant temperature;
Deng through growth phase, the growth of crystal constant temperature entered the isodiametric growth stage after 15 hours, brilliant raising speed rate slows to 0.4mm/h along with the length increase of isodiametric growth of crystal, brilliant rotational speed rate slowly is decreased to 12 rev/mins, crystal growth temperature control speed span can not be excessive, makes the crystal diameter deviation control within 1mm;
The ending stage, the crystal growth begins the ending that heats up after reaching predetermined length, along with diminishing of crystal diameter slowly improved brilliant raising speed rate to 0.6mm/h, brilliant rotational speed rate also will progressively slow to 9 rev/mins, when crystal diameter is reduced to the 4mm left and right sides, carried out isodiametric growth 8 hours, at last cooling makes the crystal diameter change expand into greatly " lid " type again, to prevent crystal cleavage and protection crucible;
Temperature-fall period, crystal growth finish rear temperature with vitellarium in the rate reduction iridium crucible of 10 ℃/h, until room temperature.
The vision slit outer end of described Medium frequency induction laser crystal growth furnace is equipped with YAG polishing eyeglass.In order to reduce radially heat dissipation capacity of crystal, reduce radially thermal stresses, further promote crystal quality
The zirconium white annulus is equipped with in the shielding upper end at described Medium frequency induction laser crystal growth furnace top.Axial-temperature gradient when lifting to cold zone in order to reduce crystal further promotes crystal quality.
As shown in Figure 1, the Medium frequency induction laser crystal growth furnace that relates in the various embodiments described above comprises:
Only be the preferred embodiments of the present invention below, but design concept of the present invention is not limited to this, all insubstantial modifications of utilizing this design that the present invention is made also all fall within protection scope of the present invention.
Claims (4)
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| CN103422173A (en) * | 2013-08-08 | 2013-12-04 | 巢湖市环宇光学技术有限公司 | Growth method of yttrium aluminum garnet crystal doped with high-concentration neodymium |
| CN103436962A (en) * | 2013-08-08 | 2013-12-11 | 巢湖市环宇光学技术有限公司 | Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof |
| CN103436952A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Neodymium-doped yttrium aluminum garnet and pure yttrium aluminum garnet bonded growth method |
| CN104357899A (en) * | 2014-11-21 | 2015-02-18 | 中国电子科技集团公司第二十六研究所 | Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals |
| CN104746135A (en) * | 2013-12-27 | 2015-07-01 | 成都晶九科技有限公司 | Growth method of induction furnace planar-interface large-sized neodymium-doped yttrium aluminium garnet crystal |
| CN106119965A (en) * | 2016-08-25 | 2016-11-16 | 广州半导体材料研究所 | The preparation method of Er doping LuAG crystal |
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| CN107653487A (en) * | 2017-10-23 | 2018-02-02 | 安徽中晶光技术股份有限公司 | A kind of recycling bin for being used in crystal growing process reclaim iridium powder |
| CN109338472A (en) * | 2018-12-06 | 2019-02-15 | 上海超硅半导体有限公司 | A method of eliminating YAG laser crystal tail portion cracking |
| CN109868507A (en) * | 2017-12-05 | 2019-06-11 | 长春理工大学 | A kind of New Type Magneto crystal Tb2YGa5O12(TYGG) preparation method |
| US10844514B1 (en) | 2019-08-21 | 2020-11-24 | Meishan Boya Advanced Materials Co., Ltd. | Open Czochralski furnace for single crystal growth |
| WO2021031139A1 (en) * | 2019-08-21 | 2021-02-25 | 眉山博雅新材料有限公司 | Multi-component garnet-structured scintillation crystal growth method and equipment |
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| CN103422173A (en) * | 2013-08-08 | 2013-12-04 | 巢湖市环宇光学技术有限公司 | Growth method of yttrium aluminum garnet crystal doped with high-concentration neodymium |
| CN103436962A (en) * | 2013-08-08 | 2013-12-11 | 巢湖市环宇光学技术有限公司 | Large-volume neodymium-doped yttrium vanadate crystal and preparation method thereof |
| CN103436952A (en) * | 2013-08-13 | 2013-12-11 | 安徽环巢光电科技有限公司 | Neodymium-doped yttrium aluminum garnet and pure yttrium aluminum garnet bonded growth method |
| CN104746135A (en) * | 2013-12-27 | 2015-07-01 | 成都晶九科技有限公司 | Growth method of induction furnace planar-interface large-sized neodymium-doped yttrium aluminium garnet crystal |
| CN104746135B (en) * | 2013-12-27 | 2017-04-19 | 成都晶九科技有限公司 | Growth method of induction furnace planar-interface large-sized neodymium-doped yttrium aluminium garnet crystal |
| CN104357899A (en) * | 2014-11-21 | 2015-02-18 | 中国电子科技集团公司第二十六研究所 | Kyropoulos method-based preparation method of large-size Yb-YAG laser crystals |
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