CN112126980A - Crystal growth method for reducing absorption of LBO crystal body and crystal prepared by crystal growth method - Google Patents
Crystal growth method for reducing absorption of LBO crystal body and crystal prepared by crystal growth method Download PDFInfo
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- CN112126980A CN112126980A CN202010950232.9A CN202010950232A CN112126980A CN 112126980 A CN112126980 A CN 112126980A CN 202010950232 A CN202010950232 A CN 202010950232A CN 112126980 A CN112126980 A CN 112126980A
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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
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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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
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Abstract
A crystal growth method for reducing absorption of LBO crystal body and a crystal prepared by the method are characterized in that boric acid and lithium carbonate are used as raw materials, a waist-shaped platinum crucible and a platinum seed crystal rod are used as a growth device, a plurality of parallel platinum sheets which are inclined upwards are arranged on the platinum seed crystal rod, the waist-shaped platinum crucible is small in the middle, large in two ends, and in an axial symmetry structure in the vertical direction and the horizontal direction. According to the invention, a plurality of parallel platinum sheets are arranged on the platinum seed crystal rod to dissipate heat of the platinum rod, so that the absorption value is reduced; the platinum sheet is designed in an inclined upward mode, so that the seeding of seed crystals and the observation of the crystal growth process are not influenced, and volatile matters are prevented from falling into the platinum sheet; the specially designed beam waist-shaped platinum crucible avoids the influence of a specific platinum seed crystal rod on a temperature field by utilizing the special temperature field formed by large two ends and small middle part, and simultaneously keeps accelerating the melt flow, reduces the viscosity of a boric acid system, reduces the crystal envelope and improves the crystal quality.
Description
Technical Field
The invention relates to the field of crystal growth, in particular to a crystal growth method for reducing LBO crystal body absorption and improving crystal growth quality.
Background
The LBO crystal is a nonlinear optical crystal excellent in optical properties, which has a wide transmission range, high optical uniformity, a relatively large effective double frequency coefficient, and a high laser damage threshold. It has important and wide application in photoelectronic technology, and is widely applied in laser frequency conversion, optical parametric oscillation, optical parametric amplification and other fields. With higher and higher laser power, higher requirements are placed on the absorption of the LBO crystal device.
The conventional LBO crystal growing method adopts corundum seed crystal rods, molybdenum and other cosolvent, and the absorption value of the grown crystal reaches more than three-four hundred ppm/cm due to the introduction of molybdenum. In order to reduce the absorption value without introducing new atoms, in the prior art, attempts are made to use boric acid and lithium carbonate as raw materials and boric acid as a cosolvent, and the LBO crystals prepared by the method in combination with some process parameter adjustment, and the bulk absorption value of the LBO crystals prepared by the method can be reduced slightly below three-four hundred ppm/cm and is about 250ppm/cm compared with the prior art.
However, in the existing preparation method of boric acid, the value of reduction of the volume absorption value of LBO crystal is limited, and boric acid is used as a cosolvent system, so that the melt viscosity is very high, the enveloping condition in the growth of the LBO crystal becomes more serious, and the yield of the LBO crystal is influenced.
Therefore, how to further reduce the bulk absorption value of the LBO crystal, and reduce the crystal growth envelope while reducing the absorption value, and improve the crystal quality becomes a technical problem to be solved in the prior art.
Disclosure of Invention
The invention aims to provide a crystal growth method for reducing the absorption of LBO crystal body, reducing the crystal growth envelope and improving the quality of the crystal, and simultaneously obtain the prepared crystal.
In order to achieve the purpose, the invention adopts the following technical scheme:
a crystal growth method for reducing the absorption of LBO crystals, characterized by:
boric acid and lithium carbonate are used as raw materials, the boric acid is used as a cosolvent, a beam waist-shaped platinum crucible and a platinum seed crystal rod are used as a growth device,
the platinum seed crystal rod is provided with a plurality of parallel platinum sheets, the platinum sheets are parallel to each other in the platinum rod direction, the waist-shaped platinum crucible is small in the middle, large in two ends, axially symmetric in the vertical and horizontal directions, and the platinum seed crystal rod is placed in the middle of the waist-shaped platinum crucible.
Optionally, the central line of the platinum seed rod is overlapped with the central line of the crucible.
Optionally, the platinum sheet is inclined upward relative to the platinum seed rod.
Optionally, the inclination angle of the platinum sheet relative to the platinum seed rod is 30-60 degrees, and preferably 45 degrees.
Optionally, the diameter of the platinum rod is 5mm, the thickness of the platinum sheet is 0.2-1.0 mm, the length is 5-10 mm, and the width is 2-5 mm.
Optionally, a plurality of platinum sheets are welded in the platinum seed rod.
Optionally, a plurality of platinum sheets are welded in the platinum seed crystal rod, and the platinum sheets are fully distributed on the whole platinum seed crystal rod.
Optionally, the crystal growth method specifically comprises:
firstly, weighing boric acid and lithium carbonate according to a certain proportion, placing the boric acid and the lithium carbonate in a pvc bottle, uniformly mixing the boric acid and the lithium carbonate by using a material throwing machine for not less than 10 hours, melting and pouring the uniformly mixed raw materials into a waist-shaped platinum crucible for growth by using a sintering furnace, placing the waist-shaped platinum crucible in a sealed furnace shell, heating to 800-850 ℃, stirring for 5 days, taking out a stirring paddle, keeping the temperature for 24 hours, slowly cooling to the crystallization temperature, preparing a processed seed crystal, fixing the seed crystal on a platinum seed crystal rod, slowly penetrating the melt to the liquid level just before contacting, starting the seed crystal to rotate at the rotating speed of 30r/min, then cooling at the speed of 0.1 ℃/d until the growth is finished, and taking out the crystal.
The invention also discloses an LBO crystal which is prepared according to the crystal growth method for reducing the absorption of the LBO crystal body.
The invention has the following advantages:
1. a plurality of parallel platinum sheets are arranged on the platinum seed crystal rod to radiate the platinum rod, so that the absorption value is reduced;
2. the platinum sheet is designed in an inclined upward mode, so that the seeding of seed crystals and the observation of the crystal growth process are not influenced, and volatile matters are prevented from falling into the platinum sheet;
3. the specially designed beam waist-shaped platinum crucible is small in the middle, large in two ends, axially symmetric in the vertical and horizontal directions, and the special temperature field formed by the large two ends and the small middle is utilized, so that the influence of a specific platinum seed crystal rod on the temperature field is avoided, the melt flow is accelerated, the viscosity of a boric acid system is reduced, the crystal envelope is reduced, and the crystal quality is improved.
Drawings
FIG. 1 is a schematic view of an LBO crystal growing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a platinum seed rod in an LBO crystal growth apparatus in accordance with an embodiment of the present invention;
FIG. 3 is a schematic view of a platinum crucible of an LBO crystal growth apparatus according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be further noted that, for the convenience of description, only some of the structures related to the present invention are shown in the drawings, not all of the structures.
The invention is characterized in that: in order to further reduce the bulk absorption of the LBO crystal, a plurality of parallel platinum sheets are arranged on the platinum seed crystal rod to radiate the platinum rod, so that the absorption value is reduced; meanwhile, in order to increase heat dissipation of the platinum rod and influence the crystal growth temperature field, and in order to ensure that the crystal is in a proper growth environment, the invention is favorable for thermal conduction transmission and crystal growth, the invention also designs a specially designed beam waist-shaped platinum crucible which is small in the middle, large at two ends, axially symmetrical up, down, left and right, and utilizes the special temperature field formed by the large at two ends and the small in the middle to accelerate melt flow, reduce the viscosity of a boric acid system, and simultaneously reduce the influence of external temperature fluctuation and the like on the crystal growth.
Referring to fig. 1-3, schematic diagrams of an LBO crystal growth apparatus according to particular embodiments of the present invention are shown.
Accordingly, the crystal growth method of the present invention for reducing the absorption of LBO crystals comprises:
boric acid and lithium carbonate are used as raw materials, the boric acid is used as a cosolvent, a beam waist-shaped platinum crucible and a platinum seed crystal rod are used as a growth device,
the platinum seed crystal rod is provided with a plurality of parallel platinum sheets, the platinum sheets are parallel to each other in the platinum rod direction, the waist-shaped platinum crucible is small in the middle, large in two ends, axially symmetric in the vertical and horizontal directions, and the platinum seed crystal rod is placed in the middle of the waist-shaped platinum crucible.
Particularly, the central line of the platinum seed crystal rod is coincident with the central line of the crucible.
Therefore, the invention uses the air-conditioning radiating fin as a reference, uses a plurality of parallel platinum sheets as radiating fins, and increases the platinum consumption as little as possible while enhancing the radiating. Meanwhile, the beam waist-shaped platinum crucible designed in a specific shape utilizes a special temperature field formed by large two ends and small middle part to accelerate melt flow, reduce the viscosity of a boric acid system and simultaneously reduce the influence of external temperature fluctuation and the like on crystal growth.
In a preferred embodiment, a plurality of the platinum sheets are welded in the platinum seed rods. The number of the platinum sheets is 6-10, but not limited to this, and can be determined according to the required heat dissipation effect, and the platinum sheets can also be distributed over the whole platinum seed crystal rod to achieve a better heat dissipation effect.
Further, the platinum sheet is inclined upward relative to the platinum seed rod. Therefore, on one hand, seeding and crystal growth process observation can be conveniently and not influenced, and on the other hand, volatile matters can be reduced from falling in the crystal preparation process.
The platinum sheet is inclined at an angle of 30-60 degrees relative to the platinum seed crystal rod, and preferably 45 degrees.
Specifically, the diameter of the platinum rod is 5mm, the thickness of the platinum sheet is 0.2-1.0 mm, the length of the platinum sheet is 5-10 mm, and the width of the platinum sheet is 2-5 mm.
The device for LBO crystal growth is arranged in a sealed furnace shell, and in order to ensure that the new device can stably grow the target crystal, the following growth process is determined through a plurality of experimental researches:
firstly, weighing boric acid and lithium carbonate according to a certain proportion, placing the boric acid and the lithium carbonate in a pvc bottle, uniformly mixing the boric acid and the lithium carbonate by using a material throwing machine for not less than 10 hours, melting and pouring the uniformly mixed raw materials into a waist-shaped platinum crucible for growth by using a sintering furnace, placing the waist-shaped platinum crucible in a sealed furnace shell, heating to 800-850 ℃, stirring for 5 days, taking out a stirring paddle, keeping the temperature for 24 hours, slowly cooling to the crystallization temperature, preparing a processed seed crystal, fixing the seed crystal on a platinum seed crystal rod, slowly penetrating the melt to the liquid level just before contacting, starting the seed crystal to rotate at the rotating speed of 30r/min, then cooling at the speed of 0.1 ℃/d until the growth is finished, and taking out the crystal. The absorption of the tested crystal is less than 50 ppm/cm.
It should be noted that the preparation process of the present invention is based on
Example 1: in this embodiment, the platinum seed rod has a plurality of parallel platinum sheets inclined upward by 45 °, and the growth crucible is a common platinum crucible.
Mixing boric acid and lithium carbonate according to a molar ratio of 1:8, placing the mixture in a pvc bottle, uniformly mixing the mixture by using a material throwing machine for not less than 10 hours, melting the uniformly mixed raw materials by using a sintering furnace, pouring the melted raw materials into a cylindrical common growth crucible, placing the growth crucible in a sealed furnace shell, heating to 800 ℃, stirring for 5 days, taking out a stirring paddle, keeping the temperature for 24 hours, slowly cooling to a crystallization temperature to prepare processed seed crystals, fixing the seed crystals on a platinum seed crystal rod, slowly extending into a melt until the seed crystals just contact the liquid level, starting the seed crystal rod to rotate at a rotation speed of 30r/min, then cooling at a speed of 0.1 ℃/d until the growth is finished, taking out the crystals, and testing by using a body absorption tester to obtain a body absorption of 100ppm/cm and simultaneously having a large amount of envelopes in the.
Example 2: in this embodiment, the platinum seed rod has a plurality of parallel platinum sheets inclined upward by 45 °, and the growth crucible is a waist-shaped platinum crucible.
The preparation method comprises the steps of proportioning boric acid and lithium carbonate according to the molar ratio of 1:8, placing the mixture in a pvc bottle, uniformly mixing the mixture by using a material throwing machine for not less than 10 hours, melting the uniformly mixed raw materials by using a sintering furnace, pouring the melted mixture into a specially designed beam waist-shaped growth platinum crucible, placing the beam waist-shaped platinum crucible in a sealed furnace shell, heating to 800 ℃, stirring for 5 days, taking out a stirring paddle, keeping the temperature for 24 hours, slowly cooling to a crystallization temperature to prepare processed seed crystals, fixing the seed crystals on a platinum seed crystal rod, slowly extending the melt until the seed crystals just contact the liquid level, starting the seed crystal rod to rotate at the rotating speed of 30r/min, cooling at the speed of 0.1 ℃/d until the growth is finished, taking out the crystals, testing by using a body absorption tester, wherein the body absorption is 30ppm/cm, the internal envelope of the crystals is small, and.
Comparative example: in this example, a prior art preparation method was employed.
Boric acid, lithium carbonate, molybdenum oxide and the like are used as raw materials, and a fluxing agent Li is adopted2O:MoO3:MF2The molar ratio is 1-2: 1-3: 0.5-1.5, a molten salt furnace is used as a growth device, a cylindrical common growth crucible is used, the prepared materials are placed in a pvc bottle and are uniformly mixed by a material throwing machine for 3-5 hours, the uniformly mixed raw materials are melted by a sintering furnace and poured into the common growth crucible, the growth crucible is placed in the molten salt furnace, the temperature is raised to 800 ℃, the mixture is stirred for 3 days, a stirring paddle is taken out, the temperature is slowly lowered to the crystallization temperature to prepare a processed seed crystal, the seed crystal is fixed on a corundum seed crystal rod and slowly goes deep into a melt, the temperature is lowered at the speed of 0.1-1.0 ℃/day, the crystal is rotated at the speed of 20-40 rpm, the prepared crystal absorbs 200-300 ppm/cm, and the yield is about 70-80 percent
It can be seen from the above examples that when boric acid is used as a flux, a waist-shaped platinum crucible and a platinum seed crystal rod with a heat dissipation platinum sheet are used in combination, so that the absorption of the LBO crystal body is reduced, the yield is kept high, the product cost is not increased, and the quality of the LBO product is further improved.
Furthermore, the invention also discloses an LBO crystal which is prepared by adopting the method.
In summary, the invention has the following advantages:
1. a plurality of parallel platinum sheets are arranged on the platinum seed crystal rod to radiate the platinum rod, so that the absorption value is reduced;
2. the platinum sheet is designed in an inclined upward mode, so that the seeding of seed crystals and the observation of the crystal growth process are not influenced, and volatile matters are prevented from falling into the platinum sheet;
3. the specially designed beam waist-shaped platinum crucible is small in the middle, large in two ends, axially symmetric in the vertical and horizontal directions, and the special temperature field formed by the large two ends and the small middle is utilized, so that the influence of a specific platinum seed crystal rod on the temperature field is avoided, the melt flow is accelerated, the viscosity of a boric acid system is reduced, the crystal envelope is reduced, and the crystal quality is improved.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A crystal growth method for reducing the absorption of LBO crystals, characterized by:
boric acid and lithium carbonate are used as raw materials, the boric acid is used as a fluxing agent, a beam waist-shaped platinum crucible and a platinum seed crystal rod are used as a growth device,
the platinum seed crystal rod is provided with a plurality of parallel platinum sheets, the platinum sheets are parallel to each other in the platinum rod direction, the waist-shaped platinum crucible is small in the middle, large in two ends, axially symmetric in the vertical and horizontal directions, and the platinum seed crystal rod is placed in the middle of the waist-shaped platinum crucible.
2. The crystal growth method of claim 1, wherein:
the platinum sheet is inclined upward relative to the platinum seed rod.
3. A crystal growth method according to claim 1 or 2, characterized in that:
the platinum sheet is inclined at an angle of 30-60 degrees relative to the platinum seed crystal rod, and preferably 45 degrees.
4. A crystal growth method according to claim 3, characterized in that:
the diameter of the platinum rod is 5mm, the thickness of the platinum sheet is 0.2-1.0 mm, the length of the platinum sheet is 5-10 mm, and the width of the platinum sheet is 2-5 mm.
5. A crystal growth method according to claim 3, characterized in that:
and a plurality of platinum sheets are welded in the platinum seed crystal rod.
6. A crystal growth method according to claim 3, characterized in that:
the platinum sheets are welded in the platinum seed crystal rod, and the platinum sheets are fully distributed on the whole platinum seed crystal rod.
7. A crystal growth method according to claim 3, characterized in that:
the central line of the platinum seed rod is superposed with the central line of the crucible.
8. A crystal growth method according to any one of claims 4 to 7, characterized in that:
the crystal growth method specifically comprises the following steps:
firstly, weighing boric acid and lithium carbonate according to a certain proportion, placing the boric acid and the lithium carbonate in a pvc bottle, uniformly mixing the boric acid and the lithium carbonate by using a material throwing machine for not less than 10 hours, melting and pouring the uniformly mixed raw materials into a waist-shaped platinum crucible for growth by using a sintering furnace, placing the waist-shaped platinum crucible in a sealed furnace shell, heating to 800-850 ℃, stirring for 5 days, taking out a stirring paddle, keeping the temperature for 24 hours, slowly cooling to the crystallization temperature, preparing a processed seed crystal, fixing the seed crystal on a platinum seed crystal rod, slowly penetrating the melt to the liquid level just before contacting, starting the seed crystal to rotate at the rotating speed of 30r/min, then cooling at the speed of 0.1 ℃/d until the growth is finished, and taking out the crystal.
9. An LBO crystal, characterized in that:
the crystal is prepared according to the crystal growth method for reducing the absorption of LBO crystal body of any one of claims 1 to 8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186592A (en) * | 2021-04-25 | 2021-07-30 | 合肥庞碲新材料科技有限公司 | Method for increasing growth speed of tellurium-zinc-cadmium crystal ingot |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10287492A (en) * | 1997-04-07 | 1998-10-27 | Nikko Eng Kk | Growth of lithium borate single crystal |
| CN103225107A (en) * | 2013-04-03 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of high-quality BBO crystal |
| CN206368220U (en) * | 2017-01-09 | 2017-08-01 | 福建福晶科技股份有限公司 | A kind of seed rod |
| CN208701250U (en) * | 2018-07-18 | 2019-04-05 | 成都新源汇博光电科技有限公司 | A kind of water-cooled seed rod for crystal growing furnace |
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2020
- 2020-09-11 CN CN202010950232.9A patent/CN112126980B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10287492A (en) * | 1997-04-07 | 1998-10-27 | Nikko Eng Kk | Growth of lithium borate single crystal |
| CN103225107A (en) * | 2013-04-03 | 2013-07-31 | 福建福晶科技股份有限公司 | Method for rapid growth of high-quality BBO crystal |
| CN206368220U (en) * | 2017-01-09 | 2017-08-01 | 福建福晶科技股份有限公司 | A kind of seed rod |
| CN208701250U (en) * | 2018-07-18 | 2019-04-05 | 成都新源汇博光电科技有限公司 | A kind of water-cooled seed rod for crystal growing furnace |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113186592A (en) * | 2021-04-25 | 2021-07-30 | 合肥庞碲新材料科技有限公司 | Method for increasing growth speed of tellurium-zinc-cadmium crystal ingot |
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