CN111485283A - Crystal growth device and method - Google Patents
Crystal growth device and method Download PDFInfo
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- CN111485283A CN111485283A CN202010417703.XA CN202010417703A CN111485283A CN 111485283 A CN111485283 A CN 111485283A CN 202010417703 A CN202010417703 A CN 202010417703A CN 111485283 A CN111485283 A CN 111485283A
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- crucible
- crystal
- melt
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- inner crucible
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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
- C30B15/10—Crucibles or containers for supporting the melt
- C30B15/12—Double crucible methods
-
- 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
- C30B29/30—Niobates; Vanadates; Tantalates
-
- 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
- C30B29/34—Silicates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a crystal growing device, which comprises an outer crucible and an inner crucible which are mutually independent, wherein the diameter of the inner crucible is smaller than that of the outer crucible; the bottom of the inner crucible is provided with a small hole for enabling melt to flow in or out, the top of the inner crucible is provided with a crucible cover, an inner crucible fixing rod is arranged on the crucible cover, the bottom of the inner crucible fixing rod is fixed on the crucible cover, and the top of the inner crucible fixing rod is connected with a furnace body; and a crucible supporting rod for controlling the outer crucible to lift is arranged at the bottom of the outer crucible. Meanwhile, the invention also discloses a method for growing crystals by using the device. The crystal prepared by the growth device and the growth method has no defects of cracking, bubbles, inclusion, scattering and the like.
Description
Technical Field
The invention relates to the field of crystal preparation, in particular to a crystal growth device and a crystal growth method.
Background
The Czochralski method is a method for growing crystals from a melt, has the advantages of high growth speed, easy observation, high crystal quality and the like, and is widely applied to the growth of silicon, germanium, sapphire, laser crystals and scintillation crystals.
After the raw materials are melted in the crucible, impurities in the raw materials and the thermal field can float on the surface of the crucible and gather in the middle of the melt, so that seeding and crystal growth are influenced, polycrystal and stress can be caused seriously, and finally, the crystal is cracked or the utilization rate is reduced. In addition, in the conventional pulling device and the crystal growth method, as the crystal growth is carried out, the melt in the crucible is gradually reduced, the exposed surface of the crucible is gradually increased, the heat radiation effect of the crucible on the crystal is gradually enhanced, the temperature gradient near the crystal growth surface is gradually reduced, and the defects of over-cooling of components, interface inversion, wrapping, cloud layer and the like are easily caused.
Therefore, it is necessary to design a new crystal growth apparatus and a new crystal growth method to solve the above-mentioned problems.
Disclosure of Invention
Based on this, the invention aims to overcome the defects of the prior art and provide a crystal growing device and a crystal growing method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a crystal growing apparatus comprises an outer crucible and an inner crucible which are independent from each other, wherein the diameter of the inner crucible is smaller than that of the outer crucible; the bottom of the inner crucible is provided with a small hole for enabling melt to flow in or out, the top of the inner crucible is provided with a crucible cover, an inner crucible fixing rod is arranged on the crucible cover, the bottom of the inner crucible fixing rod is fixed on the crucible cover, and the top of the inner crucible fixing rod is connected with a furnace body; and a crucible supporting rod for controlling the outer crucible to lift is arranged at the bottom of the outer crucible.
Preferably, the diameter of the small holes is 2-5 mm. The hole with the diameter of 2-5mm can effectively prevent impurities in the melt from entering the inner crucible and enable the melt to pass through.
Preferably, outer crucible bottom is equipped with heat preservation device, heat preservation device's bottom is equipped with the crucible and holds in the palm, the crucible bracing piece is located the crucible holds in the palm the bottom.
Meanwhile, the invention also provides a crystal growth method, and the crystal is grown by adopting the growth device.
Preferably, the crystal growth method comprises the following steps:
s1, material melting stage: sleeving the outer crucible outside the inner crucible; lowering the outer crucible so that the bottom of the inner crucible is higher than the top of the outer crucible; then placing the raw materials in an outer crucible, and heating to melt the raw materials until the melt is stable;
s2, crystal growth stage: slowly raising the outer crucible to ensure that the melt in the outer crucible enters the inner crucible through a small hole at the bottom of the inner crucible; after the melt is stabilized, crystal growth is completed in the inner crucible.
More preferably, in step S2, after the crystal growth is finished, the outer crucible is slowly lowered, the melt is made to flow into the outer crucible through the small hole at the bottom of the inner crucible and the bottom of the inner crucible is made higher than the top of the outer crucible, and then the melt is cooled.
When the bottom of the inner crucible is contacted with the melt, floating impurities at the center of the melt of the outer crucible are collected on the melt between the inner crucible and the outer crucible and finally adhered to the outer wall of the inner crucible. After the melt is stabilized, crystal growth is finished in the inner crucible, and after the crystal growth is finished, the outer crucible is slowly descended, so that the melt flows into the outer crucible through the small hole at the bottom of the inner crucible, and the bottom of the inner crucible is higher than the top of the outer crucible. After the melt is cooled, the tail material without crystallization is in the outer crucible, so that the cleaning is convenient.
Preferably, in step S2, the lowering rate of the outer crucible after the crystal growth is finished is 0.5-2 mm/h. In the descending process of the outer crucible, the crystal is gradually far away from the high-temperature melt and the outer crucible, the temperature field of the crystal is changed, and the crystal is gradually cooled. The descending speed of the outer crucible is kept to be 0.5-2mm/h, so that the thermal stress caused by the temperature field change of the crystal can be weakened, and the crystal is prevented from cracking.
Preferably, in step S2, as the crystal growth proceeds, the outer crucible is gradually raised, so that the melt in the outer crucible enters the inner crucible, and the liquid levels in the inner crucible and the outer crucible are always kept at the same height. The height of the liquid level is kept unchanged, so that the temperature gradient of the crystal growth is kept consistent, and the crystal growth defects caused by the temperature gradient change are reduced.
In addition, the invention also provides a crystal prepared by the crystal growth method. The crystal prepared by the growth device and the growth method has no defects of cracking, bubbles, inclusion, scattering and the like.
Preferably, the crystal is one of a doped garnet crystal, a doped yttrium vanadate crystal, a doped lutetium yttrium silicate crystal, a doped lithium niobate crystal, and a doped lithium tantalate crystal.
Compared with the prior art, the invention has the beneficial effects that:
the crystal prepared by the growth device and the growth method has no defects of cracking, bubbles, inclusion, scattering and the like.
Drawings
FIG. 1 is a schematic view of a structure of an apparatus for growing a crystal according to the present invention;
FIG. 2 is a graph showing the scattering behavior of a crystal without the growth apparatus and production method of the present invention (left) compared with the scattering behavior of a crystal grown with the growth apparatus and production method of the present invention (right);
FIG. 3 is a graph showing the comparison between the case of crystal dislocation without the growth apparatus and the production method of the present invention (left) and the case of crystal dislocation grown with the growth apparatus and the production method of the present invention (right).
Wherein, 1, an outer crucible; 2. an inner crucible; 3. a crucible cover; 4. an inner crucible fixing rod; 5. preserving the heat of the bottom of the crucible; 6. a crucible support; 7. a crucible supporting rod; 8. melting the materials; 9. a liquid level; 10. a seed rod; 11. and (4) crystals.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The structure schematic diagram of the crystal growth device is shown in the attached figure 1: comprises an outer crucible 1 and an inner crucible 2 which are mutually independent, wherein the diameter of the inner crucible 2 is smaller than that of the outer crucible 1; the bottom of the inner crucible 2 is provided with a small hole for the melt to flow in or out, and the diameter of the small hole is 2-5 mm; the top of the inner crucible 2 is provided with a crucible cover 3, the crucible cover 3 is provided with an inner crucible fixing rod 4, the bottom of the inner crucible fixing rod 4 is fixed on the crucible cover 3, and the top of the inner crucible fixing rod 4 is connected with the furnace body; the crucible supporting rod 7 for controlling the outer crucible 1 to lift is arranged at the bottom of the outer crucible 1, the heat preservation device 5 is arranged at the bottom of the outer crucible 1, the crucible support 6 is arranged at the bottom of the heat preservation device 5, and the crucible supporting rod 7 is arranged at the bottom of the crucible support 6.
The crystal growth method adopts the crystal growth device, and comprises the following specific steps:
s1, material melting stage: lowering the outer crucible 1 so that the bottom of the inner crucible 2 is higher than the top of the outer crucible 1, and placing the raw material in the outer crucible 1; heating to melt the raw materials until the melt 8 is stable;
s2, crystal growth stage: slowly raising the outer crucible 1 to ensure that the melt in the outer crucible 1 enters the inner crucible 2 through a small hole at the bottom of the inner crucible 2; after the melt is stable, keeping the height of the liquid level 9 unchanged, descending the seed crystal rod 10, and finishing the growth of the crystal 11 in the inner crucible 2; after the crystal 11 is grown, the outer crucible 1 is slowly descended at a descending rate of 0.5-2mm/h, so that the melt flows into the outer crucible 1 through the small hole at the bottom of the inner crucible 2, and the bottom of the inner crucible 2 is higher than the top of the outer crucible 1.
Example 1
In an embodiment of the crystal growth method of the present invention, the crystal growth method is performed by using the crystal growth apparatus, and specifically includes the following steps:
15kg of cerium-doped lutetium yttrium silicate polycrystalline raw material is put into an outer crucible, and an inner crucible is fixed on a fixing rod of the inner crucible; the height of the inner crucible and the outer crucible is adjusted to ensure that the bottom of the inner crucible is higher than the top of the outer crucible. And starting a power supply to enter a material melting stage, and starting heating to melt the material. After the melting was completed, the raw materials were observed to be completely melted and irregular particle impurities appeared in the center of the outer crucible. The outer crucible was slowly raised by the crucible support rod to bring the inner crucible into contact with the melt in the outer crucible and to let the melt enter the inner crucible through a hole of 2mm diameter in the bottom of the inner crucible. And after the melt is stabilized, descending the seed rod to start crystal growth. In the process of crystal growth, the outer crucible is slowly lifted by the crucible supporting rod, and the liquid level of the melt is kept at the same height. After the crystal growth is finished, the outer crucible is slowly descended through the crucible supporting rod, the descending rate of the outer crucible is 0.5mm/h, so that the melt in the inner crucible enters the outer crucible through the hole at the bottom, and the bottom of the inner crucible is higher than the top of the outer crucible and is lower than the bottom of the inner crucible.
The crystal prepared by the growth method is colorless, the diameter of the crystal is 80mm, the length of the crystal is 200mm, and the crystal has no defects of cracking, bubbles, inclusion, scattering and the like.
Example 2
In an embodiment of the crystal growth method of the present invention, the crystal growth method is performed by using the crystal growth apparatus, and specifically includes the following steps:
9kg of cerium-doped gadolinium gallium aluminum garnet raw material was loaded into an outer crucible, and the inner crucible was fixed on an inner crucible fixing rod. The height of the inner crucible and the outer crucible is adjusted to ensure that the bottom of the inner crucible is higher than the top of the outer crucible. And starting a power supply to enter a material melting stage, and starting heating to melt the material. After the melting was completed, the raw materials were observed to be completely melted and irregular particle impurities appeared in the center of the outer crucible. The outer crucible was slowly raised by the crucible support rod to bring the inner crucible into contact with the melt in the outer crucible and to let the melt enter the inner crucible through a hole with a diameter of 3mm at the bottom of the inner crucible. And after the melt is stabilized, descending the seed rod to start crystal growth. In the process of crystal growth, the outer crucible is slowly lifted by the crucible supporting rod, and the liquid level of the melt is kept at the same height. After the crystal growth is finished, the outer crucible is slowly descended through the crucible supporting rod, the descending rate of the outer crucible is 1mm/h, so that the melt in the inner crucible enters the outer crucible through the hole at the bottom, and the bottom of the inner crucible is higher than the top of the outer crucible and is lower than the bottom of the inner crucible.
The crystal prepared by the growth method is yellow, the diameter of the crystal is 60mm, the length of the crystal is 200mm, and the crystal has no defects of cracking, air bubbles, inclusion, scattering and the like.
Example 3
In an embodiment of the crystal growth method of the present invention, the crystal growth method is performed by using the crystal growth apparatus, and specifically includes the following steps:
27kg of raw material of neodymium-doped yttrium aluminum garnet was loaded into an induction crucible, and the inner crucible was fixed on an inner crucible fixing rod. The height of the inner crucible and the outer crucible is adjusted to ensure that the bottom of the inner crucible is higher than the top of the outer crucible. And starting a power supply to enter a material melting stage, and starting heating to melt the material. After the melting was completed, the raw materials were observed to be completely melted and irregular particle impurities appeared in the center of the outer crucible. The outer crucible was slowly raised by the crucible support rod to bring the inner crucible into contact with the melt in the outer crucible and to let the melt enter the inner crucible through a hole of 5mm diameter in the bottom of the inner crucible. And after the melt is stabilized, descending the seed rod to start crystal growth. In the process of crystal growth, the outer crucible is slowly lifted by the crucible supporting rod, and the liquid level of the melt is kept at the same height. After the crystal growth is finished, the outer crucible is slowly descended through the crucible supporting rod, the descending rate of the outer crucible is 2mm/h, so that the melt in the inner crucible enters the outer crucible through the hole at the bottom, and the bottom of the inner crucible is higher than the top of the outer crucible and is lower than the bottom of the inner crucible.
The crystal prepared by the growth method is purple, the diameter of the crystal is 100mm, the length of the crystal is 200mm, and the crystal has no defects of cracking, bubbles, inclusion, scattering and the like.
FIG. 2 is a graph showing the scattering behavior of a crystal without the growth apparatus and production method of the present invention (left) compared with the scattering behavior of a crystal grown with the growth apparatus and production method of the present invention (right); FIG. 3 is a graph comparing dislocation of a crystal not using the growth apparatus and production method of the present invention (left) with dislocation of a crystal grown using the growth apparatus and production method (right); it can be seen that the crystal prepared by the crystal growth device and the crystal growth method has no defects of cracking, bubbles, inclusion, scattering and the like, and the dislocation density is obviously reduced.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A crystal growing apparatus, comprising an outer crucible and an inner crucible which are independent from each other, wherein the diameter of the inner crucible is smaller than that of the outer crucible; the bottom of the inner crucible is provided with a small hole for enabling melt to flow in or out, the top of the inner crucible is provided with a crucible cover, an inner crucible fixing rod is arranged on the crucible cover, the bottom of the inner crucible fixing rod is fixed on the crucible cover, and the top of the inner crucible fixing rod is connected with a furnace body; and a crucible supporting rod for controlling the outer crucible to lift is arranged at the bottom of the outer crucible.
2. The crystal growing apparatus of claim 1, wherein the diameter of said aperture is 2-5 mm.
3. The crystal growing apparatus according to claim 1, wherein a heat retaining device is provided at the bottom of the outer crucible, a susceptor is provided at the bottom of the heat retaining device, and the crucible support rod is provided at the bottom of the susceptor.
4. A method for growing a crystal, characterized in that the crystal is grown by using the growing apparatus of claim 1 to 3.
5. The method of growing a crystal according to claim 4, comprising the steps of:
s1, material melting stage: sleeving the outer crucible outside the inner crucible; lowering the outer crucible so that the bottom of the inner crucible is higher than the top of the outer crucible; then placing the raw materials in an outer crucible, and heating to melt the raw materials until the melt is stable;
s2, crystal growth stage: slowly raising the outer crucible to ensure that the melt in the outer crucible enters the inner crucible through a small hole at the bottom of the inner crucible; after the melt is stabilized, crystal growth is completed in the inner crucible.
6. The method of claim 5, wherein after the crystal growth is completed, the outer crucible is slowly lowered to allow the melt to flow into the outer crucible through the bottom aperture of the inner crucible and to allow the bottom of the inner crucible to be higher than the top of the outer crucible, and then the melt is cooled in step S2.
7. The method for growing a crystal according to claim 6, wherein in step S2, the lowering rate of the outer crucible after the crystal growth is completed is 0.5 to 2 mm/h.
8. A method for growing a crystal as defined in claim 5, wherein in step S2, the outer crucible is gradually raised as the crystal growth progresses, so that the melt in the outer crucible enters the inner crucible, and the liquid levels in the inner crucible and the outer crucible are always maintained at the same level.
9. A crystal produced by the crystal growth method according to any one of claims 4 to 8.
10. The crystal of claim 9, wherein the crystal is one of a doped garnet crystal, a doped yttrium vanadate crystal, a doped lutetium yttrium silicate crystal, a doped lithium niobate crystal, and a doped lithium tantalate crystal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010417703.XA CN111485283A (en) | 2020-05-15 | 2020-05-15 | Crystal growth device and method |
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| CN202010417703.XA CN111485283A (en) | 2020-05-15 | 2020-05-15 | Crystal growth device and method |
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| CN111485283A true CN111485283A (en) | 2020-08-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061980A (en) * | 2021-04-13 | 2021-07-02 | 秦皇岛本征晶体科技有限公司 | Device and method for growing lithium fluoride single crystal |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065105A (en) * | 1991-03-21 | 1992-10-07 | 北京有色金属研究总院 | The double crucible that the preparation semiconductor monocrystal is used |
| JPH07277875A (en) * | 1994-04-01 | 1995-10-24 | Sumitomo Sitix Corp | Method for growing crystal |
| CN1654715A (en) * | 2004-08-10 | 2005-08-17 | 山东大学 | Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process |
| CN202099408U (en) * | 2011-05-12 | 2012-01-04 | 天津市环欧半导体材料技术有限公司 | Biquartz crucible device used for producing czochralski silicon single crystal |
| CN202246997U (en) * | 2011-09-19 | 2012-05-30 | 浙江思博恩新材料科技有限公司 | Double-layer crucible |
-
2020
- 2020-05-15 CN CN202010417703.XA patent/CN111485283A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065105A (en) * | 1991-03-21 | 1992-10-07 | 北京有色金属研究总院 | The double crucible that the preparation semiconductor monocrystal is used |
| JPH07277875A (en) * | 1994-04-01 | 1995-10-24 | Sumitomo Sitix Corp | Method for growing crystal |
| CN1654715A (en) * | 2004-08-10 | 2005-08-17 | 山东大学 | Suspension crucible for growth of lithium niobate crystal with near stoichiometric ratio and its growth process |
| CN202099408U (en) * | 2011-05-12 | 2012-01-04 | 天津市环欧半导体材料技术有限公司 | Biquartz crucible device used for producing czochralski silicon single crystal |
| CN202246997U (en) * | 2011-09-19 | 2012-05-30 | 浙江思博恩新材料科技有限公司 | Double-layer crucible |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113061980A (en) * | 2021-04-13 | 2021-07-02 | 秦皇岛本征晶体科技有限公司 | Device and method for growing lithium fluoride single crystal |
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Effective date of registration: 20210706 Address after: 239000 100 Nanjing Road, Langya Economic Development Zone, Chuzhou City, Anhui Province Applicant after: Anhui Zhongfei Technology Co.,Ltd. Address before: Industrial Zone, Heyun Town, Qingxin District, Qingyuan City, Guangdong Province Applicant before: FIRST RARE MATERIALS Co.,Ltd. |
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Application publication date: 20200804 |