CN109280974A - A kind of preparation method of large scale YAG laser crystal - Google Patents
A kind of preparation method of large scale YAG laser crystal Download PDFInfo
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- CN109280974A CN109280974A CN201811518849.2A CN201811518849A CN109280974A CN 109280974 A CN109280974 A CN 109280974A CN 201811518849 A CN201811518849 A CN 201811518849A CN 109280974 A CN109280974 A CN 109280974A
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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
- 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
Abstract
The present invention provides a kind of preparation method of large scale YAG laser crystal, and the preparation method comprises the following steps: the raw material of the raw material for preparing yttrium-aluminium-garnet and doped chemical being mixed, and mixed raw material is pressed into biscuit, sintering obtains YAG polycrystalline biscuit；Obtained YAG polycrystalline biscuit is heated to melting, progress oxygen diffusion in the mixed atmosphere of oxygen and inert gas is placed in, carries out liquid purifying later；Seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth；After crystal growth, by crystal pull to liquid level, cooling obtains YAG laser crystal.The YAG laser crystal of high quality can be prepared in the preparation method, and diameter can reach 200mm up to Ф 100mm, effective length, and crystal active ion doping even concentration, crystal defect is few, and core is small, crystal effective rate of utilization greatly improves, and is convenient for cutting processing large scale laser slab and disc.The preparation method simplifies processing step simultaneously, and reduces costs.
Description
Technical field
The invention belongs to crystal preparation field, be related to a kind of YAG laser crystal preparation method more particularly to a kind of big ruler
The preparation method of very little YAG laser crystal.
Background technique
As laser crystal mostly important so far, neodymium-doped yttrium-aluminum garnet (Nd:YAG) is had become at present in the world
Most mature, most mainstream laser crystal material occupies highly important status in Solid State Laser application field.Whole world solid swashs
50% or more all uses neodymium-doped YAG laser crystal in light device, and neodymium-doped YAG laser crystal is also the first choice of high power solid state laser
Material.Although YAG laser crystal have developed rapidly, a series of achievement is also obtained, but there are a little problems: such as the small (state of size
Interior main product specification is the crystal bar of Ф 50mm/60mm, and product length longest is only capable of reaching 200mm), product core it is big, brilliant
Volume defect is more, crystal is easy to crack, residual stress is small, and crystal bar utilization rate is low etc., is not able to satisfy the demand of high power laser, seriously
Influence the domestic development in great-power solid laser field.
101338453 A of CN discloses a kind of growing method of large size non-core YAG series laser crystal, this method
The grower and method for using resistance heating molybdenum crucible czochralski method, the YAG series laser for being only capable of obtaining 35-50mm are brilliant
Body, and this method crystal power obtained is low, on most of cosmetic sticks applied to low power requirements, rather than industrial high power
Use stick.201241194 Y of CN discloses a kind of induction heating iridium crucible czochralski method laser crystal growth device, which illustrates
A kind of grower is not directed to specific long crystal method, and also not illustrate can grow mostly large-sized crystalline substance using the device
Body.
Summary of the invention
To solve the technical problems existing in the prior art, the present invention provides a kind of preparation of large scale YAG laser crystal
The YAG laser crystal of high quality can be prepared in method, the preparation method, and diameter can reach up to Ф 100mm, effective length
200mm, and crystal active ion doping even concentration, crystal defect is few, and core is small, and crystal effective rate of utilization greatly improves, just
In cutting processing large scale laser slab and disc.The preparation method simplifies processing step simultaneously, and reduces costs.
In order to achieve the above objectives, the invention adopts the following technical scheme:
The present invention provides a kind of preparation method of large scale YAG laser crystal, which is characterized in that the preparation method includes
Following steps:
(1) raw material for preparing yttrium-aluminium-garnet is mixed, and mixed raw material is pressed into biscuit, it is more that sintering obtains YAG
Brilliant biscuit；
(2) obtained YAG polycrystalline biscuit is heated to melting, is placed in the mixed atmosphere of oxygen and inert gas and carries out
Oxygen diffusion, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth；
(4) after crystal growth, by crystal pull to liquid level, cooling obtains YAG laser crystal.
Crystal cleavage is that have stress due to crystals and there is strain, for YAG crystal, mainly there is 2 kinds of stress: one
The thermal stress as caused by axial-temperature gradient, second is that as uneven chemical components and caused by chemical stress, it is most of
Actinobolia growth YAG crystal be high temperature, atmosphere of inert gases single crystal growing furnace in draw, partial pressure of oxygen is lower in furnace, melt
In oxygen be easily pumped, cause component deviation, easily cause chemical stress concentration of local, so as to cause crystal be easy cracking.This
It, can due to the diffusion of oxygen using the mixed atmosphere of oxygen and inert gas in the preparation process of YAG crystal in invention
Oxygen vacancy is gradually filled up, the source of trapped electron is substantially eliminated, improves lasing efficiency.
As currently preferred technical solution, the raw material of step (1) step (1) described yttrium-aluminium-garnet and doping
Element raw material mixes simultaneously.
Preferably, the raw material of the doped chemical is Nd2O3、CeO2Or Yb2O3In any one or at least two group
It closes.The combination is typical but non-limiting example has: Nd2O3And CeO2Combination, CeO2And Yb2O3Combination, Nd2O3And Yb2O3
Combination or Nd2O3、CeO2And Yb2O3Combination etc..
In the present invention, the additional amount of doped chemical can be adjusted according to the performance requirement to YAG crystal, therefore the present invention
The additional amount of doped chemical raw material is not limited specifically.
In the present invention, the additional amount of the raw material of YAG is prepared according to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Carry out ingredient.
The purity for preparing the raw material of YAG need to be not less than 99.999%.It needs to pre-process the raw material for preparing YAG before preparation, to go out
Water and carbon dioxide in raw material.
As currently preferred technical solution, step (1) pressure that mixed raw material is pressed into biscuit is 100
~200MPa, as 100MPa, 110MPa, 120MPa, 130MPa, 140MPa, 150MPa, 160MPa, 170MPa, 180MPa,
190MPa or 200MPa etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally suitable
With.
As currently preferred technical solution, the temperature of step (1) described sintering is 1000~1400 DEG C, such as 1000
DEG C, 1050 DEG C, 1100 DEG C, 1150 DEG C, 1200 DEG C, 1250 DEG C, 1300 DEG C, 1350 DEG C or 1400 DEG C etc., it is not limited to institute
The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, the time of step (1) described sintering be 10~30h, as 10h, 12h, 15h, 18h, 20h, 22h, 25h,
28h or 30h etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, step (2) the YAG polycrystalline biscuit that will be obtained is heated to the side of melting
Method is mid-frequency induction heating.
Preferably, the heating rate of the mid-frequency induction heating is 250~400 DEG C/h, such as 250 DEG C/h, 260 DEG C/h, 280
DEG C/h, 300 DEG C/h, 320 DEG C/h, 350 DEG C/h, 380 DEG C/h or 400 DEG C/h etc., it is not limited to cited numerical value, the number
It is equally applicable to be worth other unlisted numerical value in range.
In the present invention, by YAG polycrystalline biscuit be heated to melting need under oxygen atmosphere will not in the vessel of high progression into
Row, such as iridium crucible.
As currently preferred technical solution, step (2) inert gas is any in nitrogen, neon or argon gas
It is a kind of or at least two combination.
Preferably, the concentration of the oxygen be 0.2~20%, such as 0.2%, 0.5%, 1%, 2%, 5%, 8%, 10%,
12%, 15%, 18% or 20% etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range
It is equally applicable.
Preferably, the time of step (2) oxygen diffusion is 10~20h, as 10h, 11h, 12h, 13h, 14h, 15h,
16h, 17h, 18h, 19h or 20h etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range
It is equally applicable.
It is volatilizable miscellaneous that low temperature can be generated in the present invention, in step (2) liquid purifying, that is, step (2) heating process
Matter need to uncap and wash off impurity.
As currently preferred technical solution, gaseous mixture of step (3) crystal growth in oxygen and inert gas
It being carried out in atmosphere, the concentration of the oxygen is 0.1~0.4%, such as 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%
Or 0.4% etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
In the present invention, oxygen concentration is to subtract in the mixed atmosphere that crystal growth phase reduces oxygen and inert gas
Deterioration of few oxygen to the vessel for filling melting YAG.
Preferably, the rate of pulling of step (3) described czochralski method be 0.1~3mm/h, as 0.1mm/h, 0.2mm/h,
0.5mm/h, 1mm/h, 1.5mm/h, 2mm/h, 2.5mm/h or 3mm/h etc., it is not limited to cited numerical value, the numerical value
Other unlisted numerical value are equally applicable in range.
Preferably, the crystal rotation of step (3) described czochralski method be 3~20rpm, as 3rpm, 5rpm, 8rpm, 10rpm,
12rpm, 15rpm, 18rpm or 20rpm etc., it is not limited to cited numerical value, other are unlisted in the numberical range
Numerical value is equally applicable.
As currently preferred technical solution, the rate of step (4) described cooling is 20~50 DEG C/min, such as 20 DEG C/
Min, 25 DEG C/min, 30 DEG C/min, 35 DEG C/min, 40 DEG C/min, 45 DEG C/min or 50 DEG C/min etc., it is not limited to listed
The numerical value of act, other interior unlisted numerical value of the numberical range are equally applicable.
In the present invention, YAG crystal is according to the crystal growth program automatic growth set, using pure YAG seed crystal, and seed crystal
Guarantee each uniformity to temperature gradient positioned at center.
As currently preferred technical solution, the size of the YAG laser crystal being prepared is 80~120mm,
Such as 80mm, 85mm, 90mm, 95mm, 100mm, 105mm, 110mm, 115mm or 120mm, it is not limited to cited number
Value, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the preparation method of the large scale YAG laser crystal the following steps are included:
(1) raw material of the raw material for preparing yttrium-aluminium-garnet and doped chemical is mixed, under the pressure of 100~200MPa
And mixed raw material is pressed into biscuit, 1000~1400 DEG C of 10~30h of sintering obtain YAG polycrystalline biscuit；
(2) by obtained YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 250~400 DEG C/h, juxtaposition
Oxygen diffusion is carried out in the mixed atmosphere of oxygen and inert gas, the concentration of oxygen is 0.2~20%, carries out liquid pure later
Change；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, the rate of pulling 0.5
~5mm/h, crystal rotation are 3~20rpm, and the concentration of oxygen is 0.1~0.4% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 20~50 DEG C/min cools down to obtain size
For the YAG laser crystal of 80~120mm.
Compared with prior art, the present invention at least has the advantages that
The present invention provides a kind of preparation method of large scale YAG laser crystal, and the preparation method can be prepared high-quality
The YAG laser crystal of amount, diameter is up to Ф 100mm, and effective length can reach 200mm, and crystal active ion doping concentration is equal
Even, crystal defect is few, and core is small, and crystal effective rate of utilization greatly improves, and is convenient for cutting processing large scale laser slab and disc.
The preparation method simplifies processing step simultaneously, and reduces costs.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in the understanding present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
The present embodiment provides a kind of preparation method of large scale YAG laser crystal the following steps are included:
(1) by Y2O3And Al2O3According to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Carry out ingredient, the original with doped chemical
Expect Nd2O3Mixing, Nd2O3It is 1.1% progress ingredient according to neodymium element mass fraction in product, and it will under the pressure of 100MPa
Mixed raw material is pressed into biscuit, and 1000 DEG C of sintering 30h obtain Nd:YAG polycrystalline biscuit；
(2) by obtained Nd:YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 250 DEG C/h, is placed in
Oxygen diffusion is carried out in the mixed atmosphere of oxygen and helium, the concentration of oxygen is 0.2%, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, and the rate of pulling is
0.1mm/h, crystal rotation 3rpm, the concentration of oxygen is 0.1% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 20 DEG C/min cools down to obtain neodymium-doped YAG
Laser crystal.
The diameter 80mm for the Nd:YAG laser crystal that the present embodiment is prepared, effective length 200mm, after being processed,
The laser bar having a size of D8*145 is obtained, test result is wavefront distortion value WF=0.035 λ/inch；Delustring ratio is
35.23dB；Laser power test result under different electric currents is as shown in table 1, and wherein when electric current 250A, laser power value is reachable
341.2W。
Table 1
Embodiment 2
The present embodiment provides a kind of preparation method of large scale YAG laser crystal the following steps are included:
(1) by Y2O3And Al2O3According to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Ingredient is carried out, in the pressure of 100MPa
Down and mixed raw material is pressed into biscuit, 1400 DEG C of sintering 10h obtain white YAG polycrystalline biscuit；
(2) by obtained white YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 400 DEG C/h, is placed in oxygen
Oxygen diffusion is carried out in the mixed atmosphere of gas and nitrogen, the concentration of oxygen is 20%, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, and the rate of pulling is
1.1mm/h, crystal rotation 20rpm, the concentration of oxygen is 0.1% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 50 DEG C/min cools down to obtain having a size of straight
The white YAG laser crystal of diameter 100mm, effective length 150mm.
The diameter 100mm for the white YAG laser crystal that the present embodiment is prepared, effective length 150mm, after being processed,
The large strip having a size of 40mm*20mm*150mm is obtained, can be applicable on military product.
Embodiment 3
The present embodiment provides a kind of preparation method of large scale YAG laser crystal the following steps are included:
(1) by Y2O3And Al2O3According to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Carry out ingredient, the original with doped chemical
Expect Nd2O3Mixing, Nd2O3It is 1% progress ingredient according to neodymium element mass fraction in product, under the pressure of 150MPa and will mixes
Raw material after conjunction is pressed into biscuit, and 1200 DEG C of sintering 20h obtain YAG polycrystalline biscuit；
(2) by obtained YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 250 DEG C/h, is placed in oxygen
With progress oxygen diffusion in the mixed atmosphere of helium, the concentration of oxygen is 5%, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, rate of pulling 2mm/
H, crystal rotation 10rpm, the concentration of oxygen is 0.2% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 30 DEG C/min cools down to obtain having a size of 80
The YAG laser crystal of~120mm neodymium-doped.
The diameter 100mm for the Nd:YAG laser crystal that the present embodiment is prepared, effective length 120mm, after being processed,
The laser bar having a size of D8*120 is obtained, test result is wavefront distortion value WF=0.025 λ/inch；Delustring ratio is
36.23dB；Laser power test result under different electric currents is as shown in table 2, and wherein when electric current 340A, laser power value is reachable
135W。
Table 2
Embodiment 4
The present embodiment provides a kind of preparation method of large scale YAG laser crystal the following steps are included:
(1) by Y2O3And Al2O3According to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Carry out ingredient, the original with doped chemical
Expect CeO2Mixing, CeO2It is 1% progress ingredient according to Ce elements mass fraction in product, and it will mixing under the pressure of 120MPa
Raw material afterwards is pressed into biscuit, and 1100 DEG C of sintering 25h obtain YAG polycrystalline biscuit；
(2) by obtained YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 300 DEG C/h, is placed in oxygen
With progress oxygen diffusion in the mixed atmosphere of neon, the concentration of oxygen is 10%, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, rate of pulling 3mm/
H, crystal rotation 15rpm, the concentration of oxygen is 0.3% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 40 DEG C/min cools down to obtain having a size of 80
~120mm mixes the YAG laser crystal of cerium.
Embodiment 5
The present embodiment provides a kind of preparation method of large scale YAG laser crystal the following steps are included:
(1) by Y2O3And Al2O3According to the chemical formula Y of yttrium-aluminium-garnet3Al5O12Carry out ingredient, the original with doped chemical
Expect Yb2O3Mixing, Yb2O3It is 1% progress ingredient according to ytterbium element mass fraction in product, under the pressure of 180MPa and will mixes
Raw material after conjunction is pressed into biscuit, and 1300 DEG C of sintering 15h obtain YAG polycrystalline biscuit；
(2) by obtained YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 350 DEG C/h, is placed in oxygen
With progress oxygen diffusion in the mixed atmosphere of argon gas, the concentration of oxygen is 2%, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth, rate of pulling 1mm/
H, crystal rotation 5rpm, the concentration of oxygen is 0.2% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 25 DEG C/min cools down to obtain having a size of 80
~120mm mixes the YAG laser crystal of ytterbium.
Comparative example 1
For this comparative example other than YAG polycrystalline biscuit melts and crystal growth carries out under helium atmosphere, other conditions are equal
It is same as Example 1.
The diameter 80mm for the Nd:YAG laser crystal that this comparative example is prepared, effective length 150mm, crystal bar are sent out when checking
Existing many bubbles, it is unavailable.
Comparative example 2
For this comparative example other than YAG polycrystalline biscuit melts and crystal growth carries out under vacuum conditions, other conditions are equal
It is same as Example 1.
The diameter 80mm for the Nd:YAG laser crystal that this comparative example is prepared, effective length 150mm, after being processed,
The laser bar having a size of D8*145 is obtained, test result is wavefront distortion value WF=0.055 λ/inch；Delustring ratio is
31.53dB；Laser power test result under different electric currents is as shown in table 3, and wherein when electric current 250A, laser power value is reachable
268.2W。
Table 3
From the comparison of embodiment 1 and comparative example 1 and 2 as can be seen that the Nd:YAG that embodiment 1 is prepared in the present invention is sharp
Luminescent crystal wherein electric current 250A when, laser power value is up to 341.2W.And the thawing of YAG polycrystalline biscuit and crystal in comparative example 1
It is grown under helium atmosphere and carries out, participated in without oxygen, the crystal bar being prepared has many bubbles, unavailable.And comparative example 2
Middle YAG polycrystalline biscuit melts and crystal growth carries out under vacuum conditions, and wherein when electric current 250A, laser power value is reachable
268.2W is less than the embodiment of the present invention 1.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (10)
1. a kind of preparation method of large scale YAG laser crystal, which is characterized in that the preparation method comprises the following steps:
(1) raw material for preparing yttrium-aluminium-garnet is mixed, and mixed raw material is pressed into biscuit, sintering obtains YAG polycrystalline cake
Material；
(2) obtained YAG polycrystalline biscuit is heated to melting, is placed in progress oxygen expansion in the mixed atmosphere of oxygen and inert gas
It dissipates, carries out liquid purifying later；
(3) seed crystal is added into the fused raw material after liquid purifying, czochralski method carries out crystal growth；
(4) after crystal growth, by crystal pull to liquid level, cooling obtains YAG laser crystal.
2. preparation method according to claim 1, which is characterized in that the raw material of step (1) described yttrium-aluminium-garnet with mix
Miscellaneous element raw material mixes simultaneously；
Preferably, the raw material of the doped chemical is Nd2O3、CeO2Or Yb2O3In any one or at least two combination.
3. preparation method according to claim 1 or 2, which is characterized in that step (1) is described to be pressed into mixed raw material
The pressure of biscuit is 100~200MPa.
4. preparation method according to claim 1-3, which is characterized in that the temperature of step (1) described sintering is
1000~1400 DEG C；
Preferably, the time of step (1) described sintering is 10~30h.
5. preparation method according to claim 1-4, which is characterized in that step (2) YAG that will be obtained is more
The method that brilliant biscuit is heated to melting is mid-frequency induction heating；
Preferably, the heating rate of the mid-frequency induction heating is 250~400 DEG C/h.
6. preparation method according to claim 1-5, which is characterized in that step (2) inert gas is nitrogen
In gas, neon or argon gas any one or at least two combination；
Preferably, the concentration of the oxygen is 0.2~20%；
Preferably, the time of step (2) the oxygen diffusion is 10~20h.
7. preparation method according to claim 1-6, which is characterized in that step (3) described crystal growth is in oxygen
It is carried out in the mixed atmosphere of gas and inert gas, the concentration of the oxygen is 0.1~0.4%；
Preferably, the rate of pulling of step (3) described czochralski method is 0.1~3mm/h；
Preferably, the crystal rotation of step (3) described czochralski method is 3~20rpm.
8. preparation method according to claim 1-7, which is characterized in that the rate of step (4) described cooling is
20~50 DEG C/min.
9. preparation method according to claim 1-8, which is characterized in that the YAG laser being prepared is brilliant
The size of body is 80~120mm.
10. preparation method according to claim 1-8, which is characterized in that the preparation method includes following step
It is rapid:
(1) raw material of the raw material for preparing yttrium-aluminium-garnet and doped chemical is mixed, and it will under the pressure of 100~200MPa
Mixed raw material is pressed into biscuit, and 1000~1400 DEG C of 10~30h of sintering obtain YAG polycrystalline biscuit；
(2) by obtained YAG polycrystalline biscuit mid-frequency induction heating to melting, heating rate is 250~400 DEG C/h, is placed in oxygen
Oxygen diffusion is carried out in the mixed atmosphere of gas and inert gas, the concentration of oxygen is 0.2~20%, carries out liquid purifying later；
(3) it is added seed crystal into the fused raw material after liquid purifying, czochralski method carries out crystal growth, and the rate of pulling is 0.5~
5mm/h, crystal rotation are 3~20rpm, and the concentration of oxygen is 0.1~0.4% in mixed atmosphere when crystal growth,；
(4) after crystal growth, by crystal pull to liquid level, the rate of temperature fall of 20~50 DEG C/min cools down to obtain having a size of 80
The YAG laser crystal of~120mm.
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| CN101338453A (en) * | 2008-07-16 | 2009-01-07 | 成都东骏激光有限责任公司 | Growth device of large size non-core YAG series laser crystal and growth process thereof |
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