CN105696073A - Self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal and growth method thereof - Google Patents
Self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal and growth method thereof Download PDFInfo
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- CN105696073A CN105696073A CN201610087488.5A CN201610087488A CN105696073A CN 105696073 A CN105696073 A CN 105696073A CN 201610087488 A CN201610087488 A CN 201610087488A CN 105696073 A CN105696073 A CN 105696073A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
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- H01S3/164—Solid materials characterised by a crystal matrix garnet
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Abstract
The invention discloses a self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal consisting of chemical formula V5xNd3yY3(1-y)Al5(1-x)O12, wherein x is more than 0 and not more than 0.02, and y is more than 0 and not more than 0.015.The invention further discloses a growth method of the self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal.The growth method includes the steps of mixing a vanadium compound, a neodymium compound, an yttrium compound and an aluminum compound uniformly and pressing a mixture to obtain a crystal growth initial raw material with the chemical formula V5xNd3yY3(1-y)Al5(1-x)O12; heating the crystal growth initial raw material with the chemical formula V5xNd3yY3(1-y)Al5(1-x)O12 to a molten state to obtain a crystal growth melt, and then growing by a crystal growth from melt method so as to obtain the self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal.The self-saturated absorption type Q-switching yttrium aluminum garnet laser crystal has Q-switching and laser gain functions.
Description
Technical field
The present invention relates to laser crystal and technical field of crystal growth, particularly relate to a kind of self-saturation and absorb tune Q Yttrium aluminium garnet laser crystal and growing method thereof。
Background technology
Nd:YAG laser instrument is one of most widely used all solid state laser, and it all has a wide range of applications in fiber-optic transfer, miniature manufacture, remote sensing, information storage etc. the nanosecond order pulse of 1.3～1.4 μm。In addition, l.3～1.4 mu m wavebands are human eye safe waveband districts, simultaneously with the low dispersion of silicon optical fiber and low-loss consistent wavelength, therefore the laser of this wave band can be widely applied to the fields such as the pumping source of laser medicine, fiber optic communication, light sensing location and mid-infrared parametric oscillation。1.3～1.4 μm of laser instrument at Nd:YAG are inserted into V3+: YAG or Co2+:LaMgAl11O19Adjusting Q pulse laser output can be realized, it is thus achieved that therefore high pulse power laser as saturated absorbing body。In this fashion, V3+: YAG and Nd:YAG needs to prepare respectively monocrystalline, is processed into two devices, V3+: YAG element is as saturated absorbing body, and Nd:YAG is then as laser work gain media。Recently, Czech is existing by V3 +: YAG and Nd:YAG is bonded together the report as composite crystal element。In this fashion, it is still necessary to grow V respectively3+: YAG and Nd:YAG crystal, respectively it is carried out Precision Machining, again through light adhesive process, the two is realized combination geometrically, after the high-temperature heatings of 1000～1500 DEG C, allow V3+: the component phase counterdiffusion between YAG and YAG, it is achieved the bonding between two crystal, thus forming geometry V3+: the composite crystal element of YAG and YAG。It can be seen that this preparation method is not only loaded down with trivial details consuming time, bonding and sintering diffusion couple technique, firing equipment also have significantly high requirement。
Summary of the invention
The present invention proposes a kind of self-saturation and absorbs tune Q Yttrium aluminium garnet laser crystal and growing method thereof, and gained self-saturation absorbs adjusts Q Yttrium aluminium garnet laser crystal to have tune Q and laser gain dual-use function, has important application prospect in all solid state laser。
A kind of self-saturation that the present invention proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal, has below formula composition: V5xNd3yY3(1-y)Al5(1-x)O12, wherein 0 < x≤0.02,0 < y≤0.015。
The above-mentioned self-saturation that the present invention also proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal growing method, comprises the steps:
S1, by vanadium-containing compound, containing neodymium compound, containing after yttrium compound, aluminum contained compound mix homogeneously, carrying out compacting, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed；
S2, it is V by chemical formula5xNd3yY3(1-y)Al5(1-x)O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt crystal growth method by melt method to carry out growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal。
Preferably, the operating procedure of S1 is: by vanadium-containing compound, containing neodymium compound, containing after yttrium compound, aluminum contained compound mix homogeneously, suppress, and then carrying out synthetic reaction, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed。
Preferably, in S1, synthetic reaction is high temperature solid state reaction, liquid phase synthesis or vapor-phase synthesis。
Preferably, the concrete operation step of S1 is: by molar part by 2.5x part V2O5, 1.5y part Nd2O3, 1.5 (1-y) part Y2O3With 2.5 (1-x) part Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed, calcining heat is 900～1300 DEG C, and calcination time is 48～200h；
Its reaction equation is as follows:
Preferably, when self-saturation absorbs, to adjust the segregation coefficient of certain element in Q Yttrium aluminium garnet laser crystal be k, k=0.01～1, thenWherein m is the quality in S1 containing this element compound, and n is that this element is at V5xNd3yY3(1-y)Al5(1-x)O12The amount of middle contained substance, M is the molal weight containing this element compound。
Preferably, in the crystal growth method by melt method of S2, crystal growth atmosphere is the one in air atmosphere, oxygen atmosphere, argon gas atmosphere, nitrogen atmosphere, carbon dioxide atmosphere, carbon monoxide atmosphere。
Preferably, in S2, crystal growth method by melt method is the one in czochralski method, Bridgman-Stockbarger method, temperature ladder method, heat-exchanging method, kyropoulos, top-seeded solution growth, flux growing method。
Preferably, in S2, when crystal growth method by melt method is czochralski method, Bridgman-Stockbarger method or top-seeded solution growth, adopting seed crystal oriented growth, seed crystal is Y3Al5O12、Nd:Y3Al5O12、V:Y3Al5O12Or V5xNd3yY3(1-y)Al5(1-x)O12。
Preferably, seed crystal direction is<111>,<100>,<010>or<001>direction。
This invention takes the method innovated completely, by V3+、Nd3+Ion mixes in YAG substrate together, forms V5xNd3yY3(1-y)Al5(1-x)O12, just prepare tune Q and working-laser material element by a crystal growth, adjust Q and laser output only can realize with one piece of crystal, have great importance for improving the stability of Laser Devices, improving crystal preparation efficiency。
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail。
Embodiment 1
The above-mentioned self-saturation that the present invention proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal growing method, comprises the steps:
S1, by molar part by 0.0375 part of V2O5, 0.375 part of Nd2O3, 1.425 parts of Y2O3With 2.4625 parts of Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V0.075Nd0.15Y2.85Al4.925O12Crystal growth initial feed, calcining heat is 1000 DEG C, and calcination time is 200h, and wherein the segregation coefficient of neodymium element is 0.2；
Its reaction equation is as follows:
S2, it is V by chemical formula0.075Nd0.15Y2.85Al4.925O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt czochralski method to carry out seed crystal oriented growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal；Wherein seed crystal is the Y in<111>direction3Al5O12, crystal growth atmosphere is argon gas atmosphere。
Embodiment 2
The above-mentioned self-saturation that the present invention proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal growing method, comprises the steps:
S1, by molar part by 0.1 part of V2O5, 0.225 part of Nd2O3, 1.275 parts of Y2O3With 2.45 parts of Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V0.1Nd0.45Y2.55Al4.9O12Crystal growth initial feed, calcining heat is 1250 DEG C, and calcination time is 50h, and wherein the segregation coefficient of v element is 0.5；
Its reaction equation is as follows:
S2, it is V by chemical formula0.1Nd0.45Y2.55Al4.9O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt Bridgman-Stockbarger method to carry out seed crystal oriented growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal；Wherein seed crystal is the Nd:Y in<100>direction3Al5O12, crystal growth atmosphere is air atmosphere。
Embodiment 3
The above-mentioned self-saturation that the present invention proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal growing method, comprises the steps:
S1, by molar part by 0.025 part of V2O5, 0.15 part of Nd2O3, 1.35 parts of Y2O3With 2.475 parts of Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V0.05Nd0.3Y2.7Al4.95O12Crystal growth initial feed, calcining heat is 1100 DEG C, and calcination time is 150h；
Its reaction equation is as follows:
S2, it is V by chemical formula0.05Nd0.3Y2.7Al4.95O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt heat-exchanging method to carry out growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal。
Embodiment 4
The above-mentioned self-saturation that the present invention proposes absorbs adjusts Q Yttrium aluminium garnet laser crystal growing method, comprises the steps:
S1, by molar part by 0.125 part of V2O5, 0.075 part of Nd2O3, 1.425 parts of Y2O3With 2.375 parts of Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V0.25Nd0.15Y2.85Al4.75O12Crystal growth initial feed, calcining heat is 1200 DEG C, and calcination time is 100h；
Its reaction equation is as follows:
S2, it is V by chemical formula0.25Nd0.15Y2.85Al4.75O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt Bridgman-Stockbarger method to carry out seed crystal oriented growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal；Wherein seed crystal is the V in<001>direction5xNd3yY3(1-y)Al5(1-x)O12, crystal growth atmosphere is nitrogen atmosphere。
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; it is equal to replacement according to technical scheme and inventive concept thereof or is changed, all should be encompassed within protection scope of the present invention。
Claims (10)
1. a self-saturation absorbs and adjusts Q Yttrium aluminium garnet laser crystal, it is characterised in that have below formula composition: V5xNd3yY3(1-y)Al5(1-x)O12, wherein 0 < x≤0.02,0 < y≤0.015。
2. a self-saturation as claimed in claim 1 absorbs and adjusts Q Yttrium aluminium garnet laser crystal growing method, it is characterised in that comprise the steps:
S1, by vanadium-containing compound, containing neodymium compound, containing after yttrium compound, aluminum contained compound mix homogeneously, carrying out compacting, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed；
S2, it is V by chemical formula5xNd3yY3(1-y)Al5(1-x)O12The heating of crystal growth initial feed obtain crystal growth melt to molten condition, then adopt crystal growth method by melt method to carry out growth and obtain self-saturation and absorb and adjust Q Yttrium aluminium garnet laser crystal。
3. self-saturation absorbs tune Q Yttrium aluminium garnet laser crystal growing method according to claim 2, it is characterized in that, the operating procedure of S1 is: by vanadium-containing compound, containing neodymium compound, containing after yttrium compound, aluminum contained compound mix homogeneously, suppressing, then carrying out synthetic reaction, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed。
4. self-saturation absorbs tune Q Yttrium aluminium garnet laser crystal growing method according to claim 3, it is characterised in that in S1, synthetic reaction is high temperature solid state reaction, liquid phase synthesis or vapor-phase synthesis。
5. self-saturation according to claim 3 or 4 absorbs and adjusts Q Yttrium aluminium garnet laser crystal growing method, it is characterised in that the concrete operation step of S1 is: by molar part by 2.5x part V2O5, 1.5y part Nd2O3, 1.5 (1-y) part Y2O3With 2.5 (1-x) part Al2O3After mix homogeneously, carrying out calcining, to obtain chemical formula be V5xNd3yY3(1-y)Al5(1-x)O12Crystal growth initial feed, calcining heat is 900～1300 DEG C, and calcination time is 48～200h。
6. self-saturation according to any one of claim 2-5 absorbs and adjusts Q Yttrium aluminium garnet laser crystal growing method, it is characterised in that when self-saturation absorbs, to adjust the segregation coefficient of certain element in Q Yttrium aluminium garnet laser crystal be k, k=0.01～1, thenWherein m is the quality in S1 containing this element compound, and n is that this element is at V5xNd3yY3(1-y)Al5(1-x)O12The amount of middle contained substance, M is the molal weight containing this element compound。
7. self-saturation according to any one of claim 2-6 absorbs and adjusts Q Yttrium aluminium garnet laser crystal growing method, it is characterized in that, in the crystal growth method by melt method of S2, crystal growth atmosphere is the one in air atmosphere, oxygen atmosphere, argon gas atmosphere, nitrogen atmosphere, carbon dioxide atmosphere, carbon monoxide atmosphere。
8. self-saturation according to any one of claim 2-7 absorbs and adjusts Q Yttrium aluminium garnet laser crystal growing method, it is characterized in that, in S2, crystal growth method by melt method is the one in czochralski method, Bridgman-Stockbarger method, temperature ladder method, heat-exchanging method, kyropoulos, top-seeded solution growth, flux growing method。
9. self-saturation absorbs tune Q Yttrium aluminium garnet laser crystal growing method according to claim 8, it is characterised in that in S2, when crystal growth method by melt method is czochralski method, Bridgman-Stockbarger method or top-seeded solution growth, adopts seed crystal oriented growth, and seed crystal is Y3Al5O12、Nd:Y3Al5O12、V:Y3Al5O12Or V5xNd3yY3(1-y)Al5(1-x)O12。
10. self-saturation absorbs tune Q Yttrium aluminium garnet laser crystal growing method according to claim 9, it is characterised in that seed crystal direction is<111>,<100>,<010>or<001>direction。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010022794A1 (en) * | 2000-02-10 | 2001-09-20 | Yoshiharu Urata | Laser device |
| CN1645691A (en) * | 2005-02-02 | 2005-07-27 | 中国科学院物理研究所 | Active and passive Q-adjusted single longitudinal mode laser |
| CN1912195A (en) * | 2006-07-28 | 2007-02-14 | 中国科学院上海光学精密机械研究所 | Growth method of vanadium-doped yttrium aluminum garnet crystal |
| CN103710755A (en) * | 2013-12-27 | 2014-04-09 | 中国科学院合肥物质科学研究院 | Rare earth co-doping activated yttrium-aluminum-scandium garnet luminescent material and melt crystal growth method thereof |
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- 2016-02-16 CN CN201610087488.5A patent/CN105696073A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010022794A1 (en) * | 2000-02-10 | 2001-09-20 | Yoshiharu Urata | Laser device |
| CN1645691A (en) * | 2005-02-02 | 2005-07-27 | 中国科学院物理研究所 | Active and passive Q-adjusted single longitudinal mode laser |
| CN1912195A (en) * | 2006-07-28 | 2007-02-14 | 中国科学院上海光学精密机械研究所 | Growth method of vanadium-doped yttrium aluminum garnet crystal |
| CN103710755A (en) * | 2013-12-27 | 2014-04-09 | 中国科学院合肥物质科学研究院 | Rare earth co-doping activated yttrium-aluminum-scandium garnet luminescent material and melt crystal growth method thereof |
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Application publication date: 20160622 |