CN116516493A - Parallel efficient crystal growth system and method - Google Patents
Parallel efficient crystal growth system and method Download PDFInfo
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- CN116516493A CN116516493A CN202310471751.0A CN202310471751A CN116516493A CN 116516493 A CN116516493 A CN 116516493A CN 202310471751 A CN202310471751 A CN 202310471751A CN 116516493 A CN116516493 A CN 116516493A
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- 239000013078 crystal Substances 0.000 title claims abstract description 192
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000009413 insulation Methods 0.000 claims abstract description 111
- 238000010438 heat treatment Methods 0.000 claims abstract description 88
- 230000002093 peripheral effect Effects 0.000 claims abstract description 17
- 238000006073 displacement reaction Methods 0.000 claims abstract description 13
- 230000001105 regulatory effect Effects 0.000 claims abstract description 11
- 238000002109 crystal growth method Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 43
- 238000007789 sealing Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 19
- 239000004964 aerogel Substances 0.000 claims description 17
- 229920000742 Cotton Polymers 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000001360 synchronised effect Effects 0.000 abstract description 7
- 239000010453 quartz Substances 0.000 description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 230000033228 biological regulation Effects 0.000 description 8
- 238000012546 transfer Methods 0.000 description 8
- 230000017525 heat dissipation Effects 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 238000009529 body temperature measurement Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of crystal growth, in particular to a parallel efficient crystal growth system and a parallel efficient crystal growth method, comprising the following steps: a plurality of crystal growth units arranged in succession in a vertical direction; the gradient heating modules are respectively arranged around the peripheral wall of each crystal growth unit; a heat insulation module is arranged between two adjacent gradient heating modules. According to the invention, the plurality of crystal growth units and the gradient heating modules are arranged in a stacked manner in the vertical direction, and meanwhile, the heat insulation module is additionally arranged at the connecting interface, so that heat exchange in a high-temperature and low-temperature area can be blocked, and the mutual influence between the upper growth unit and the lower growth unit is eliminated. The displacement of each crystal growth unit can be synchronously regulated and controlled, so that synchronous and uniform growth is realized, and the method has the characteristics of high crystal preparation efficiency, strong temperature controllability, good growth uniformity and the like.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a parallel efficient crystal growth system and method.
Background
Most common compound semiconductor crystals have the attribute problems of low heat conductivity, high viscosity and the like, so that the crystal growth rate is relatively slow, generally 2-16 mm/d, the stacking fault energy is relatively low during crystal growth, defects such as twin crystals and polycrystal are easy to generate, the factors severely restrict the preparation of large-size single crystals, and the growth efficiency of the large-size single crystals needs to be improved to meet the application requirements of the large-size single crystals.
When various large-size single crystals are prepared at present, the single crystal rate has a certain bottleneck because the multi-component compound crystals are difficult to realize the whole single crystal growth. To increase productivity, it is generally performed by increasing the crystal size or increasing the number of crystal growth apparatuses. However, due to the limitation of the physical properties of the crystal, when the diameter of the crystal is increased to a certain extent, the radial direction of the crystal is greatly uneven, so that the diameter size has a critical value and cannot be continuously increased; because of segregation, when the crystal grows to a certain length, larger component deviation exists along the axial direction, and the length of the crystal is not too long. The method has the advantages that crystal growth equipment is increased, the crystal preparation quantity is increased, and the method is an effective method for improving the productivity, but the method has higher investment in site and equipment cost and is not suitable for large-scale popularization and application. There are also methods for growing multiple crystal bodies by using multiple growth bodies, i.e. a set of control system corresponding to multiple growth bodies, so as to achieve the purpose of simultaneously growing multiple crystal bodies. The method can also adopt a large cavity for growth in a mode of placing a plurality of crystal growth crucibles inside, has the problem of uneven temperature field around the crystal, is not suitable for growth of the crystal with high requirement on uniformity, and has narrower application range.
The crystal growth furnace generally includes a high temperature zone and a low temperature zone to effect melting and crystallization of the crystal material to complete the growth. Therefore, the uniformity of crystal growth is closely related to temperature control, and the requirement on temperature stability is high, and the requirement of +/-0.1 ℃ is usually required, if a plurality of growth crucibles are vertically arranged, the problem that the temperature of the upper crucible and the temperature of the lower crucible are greatly influenced by heat conduction and heat radiation needs to be considered. If the crucibles are vertically arranged at intervals, on the one hand, the occupied space is large, and on the other hand, synchronous assembly and regulation and control of the crucibles are difficult to realize, so that the improvement degree of the growth efficiency is limited. Thus, no crucible vertically aligned growth system is known in the prior art. It would be of great importance in the art to provide a vertically oriented and efficient growth system.
Disclosure of Invention
The invention aims to provide a parallel high-efficiency crystal growth system and a parallel high-efficiency crystal growth method, wherein a plurality of crystal growth units and gradient heating modules are arranged in a stacked mode in the vertical direction, and meanwhile, a heat insulation module is additionally arranged at a connecting interface to reduce heat exchange in a high-temperature and low-temperature area, so that displacement of each crystal growth unit can be synchronously regulated and controlled to realize synchronous and uniform growth, and the parallel high-efficiency crystal growth system has the characteristics of high crystal preparation efficiency, strong temperature controllability, good growth uniformity and the like.
To achieve the above object, the present invention provides a crystal growth system comprising:
a plurality of crystal growth units arranged in succession in a vertical direction;
a gradient heating module is arranged on the peripheral wall of each crystal growth unit in a surrounding way;
a heat insulation module is arranged between two adjacent gradient heating modules.
Further, a cooling module is arranged between two adjacent gradient heating modules, and the cooling module and the heat insulation module are both arranged around the crystal growth unit;
preferably, the heat insulating module is disposed around a peripheral wall of the crystal growth unit; the cooling module is arranged on the outer side of the heat insulation module in a surrounding mode;
preferably, the cooling module comprises a liquid cooling pipe which is arranged on the outer side of the heat insulation module in a surrounding mode.
Further, heat insulation cotton is also arranged between the heat insulation module and the crystal growth unit in a ring mode.
Further, each of the crystal growth units includes:
a growth crucible comprising a crystal growth cavity at the bottom and a thermally insulated cavity at the top; the crucible peripheral wall of the crystal growth cavity is of a transparent structure, and the crucible peripheral wall of the heat insulation cavity is of a frosted structure; the heat insulation cavity is used for forming a frosted surface by carrying out sand blasting on the upper part of the growth crucible, and the frosted surface is opaque and is used for reducing the radiation heat from the lower part to the upper part of the quartz crucible;
sealing a round plug for sealing the growth crucible;
preferably, a heat insulation layer is further arranged in the heat insulation cavity;
the heat insulation layer comprises graphite felt and/or aerogel, and the graphite felt and/or aerogel are substances with smaller heat conductivity, are stable in chemical property and light-proof, and can effectively block heat transfer between two adjacent growth crucibles.
The heat insulation cotton is arranged between the heat insulation module and the heat insulation cavity, the cross section is preferably inverted L-shaped, and sealing heat insulation between the heat insulation module and the heat insulation cavity is realized. The heat insulation cotton is resistant to high temperature, has certain elasticity, is convenient for up-and-down movement of the crystal growth unit, and does not influence heat insulation tightness.
Further, adjacent crystal growth units are detachably connected, and the central axes of each crystal growth unit are coincident.
Further, each of the gradient heating modules includes at least one high temperature heating module and at least one low temperature heating module; the gradient heating module is preferably a hollow cylindrical heating furnace body, the temperature field inside the cylindrical heating furnace body is uniform, the temperature field in the circumferential direction of the crucible is uniformly distributed, and the uniformity of crystals can be remarkably improved.
Preferably, in each of the gradient heating modules, the high temperature heating module is disposed above the low temperature heating module.
Further, each gradient heating module is provided with a temperature monitoring assembly, preferably a thermocouple;
and/or a liftable support base is arranged below the bottommost crystal growth unit;
and/or a first heat-insulating layer is arranged below the gradient heating module at the bottommost part, and an aluminum silicate block is arranged between the first heat-insulating layer and the crystal growth unit in a ring manner;
and/or a second heat-insulating layer is arranged above the gradient heating module at the top, and a limiting component is arranged between the second heat-insulating layer and the crystal growth unit in a surrounding manner;
the spacing component is preferably an alumina ceramic ring.
In order to achieve the above object, the present invention also provides a crystal growth method, employing the crystal growth system described in any one of the above, the growth method comprising: and regulating and controlling the growth process of the internal crystal material by regulating the displacement of the crystal growth unit in the vertical direction.
Further, the step of adjusting the growth process of the internal crystal material by adjusting the displacement of the crystal growth unit in the vertical direction includes:
s1, respectively filling polycrystalline materials into each growth crucible, sealing by adopting a sealing round plug, and then filling a first growth crucible into a cavity formed by the gradient heating module;
s2, a heat insulation layer is arranged in a heat insulation cavity at the top of the first growth crucible;
s3, sleeving a second growth crucible in the heat insulation cavity of the first growth crucible, and repeating the step S2, and sequentially loading the second growth crucible into the crystal growth units for assembly;
s4, starting the gradient heating module and the cooling module, and synchronously driving each growth crucible to descend through the support base after the polycrystalline material is completely melted, so that growth is completed.
The beneficial effects of the invention are as follows:
1. according to the crystal growth system provided by the invention, the plurality of crystal growth units and the gradient heating modules are arranged in a stacked manner in the vertical direction, and meanwhile, the heat insulation module is additionally arranged at the connecting interface of the gradient heating modules to block heat exchange in a high-temperature and low-temperature region, so that the displacement of each crystal growth unit can be synchronously regulated and controlled to realize synchronous and uniform growth, and the crystal growth system has the characteristics of high crystal preparation efficiency, strong temperature controllability, good growth uniformity and the like.
2. The cooling module is arranged at the connecting interface of the gradient heating module, so that the temperature interaction between two adjacent units can be blocked through two modes of heat insulation and heat dissipation, the high-precision regulation and control of the temperature can be realized, and the relative width of the two units can be reasonably designed to realize the optimal regulation and control of the temperature stability, so that the structure flexibility is high.
3. According to the invention, the tail part of the crucible is frosted, and heat insulation materials such as graphite felt, aerogel and the like are filled in the crucible, so that heat can be effectively prevented from being transferred upwards along quartz, the upper part of the crystal is kept at high temperature to be fully overheated, and meanwhile, heat transfer upwards is blocked, and the influence is generated on a low-temperature area of an upper unit.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a crystal growth system provided by the present invention;
FIG. 2 is a schematic view of the cooling module of FIG. 1;
fig. 3 is a schematic cross-sectional view of the insulation module of fig. 1.
Reference numerals:
100-stainless steel outer furnace shell; 101-a crucible support base; 102-aluminum silicate blocks at the lower furnace mouth; 103-heat preservation cotton at the lower furnace mouth; 104-alumina ring; 105-feeding aluminum silicate blocks;
110-a crystal growth unit; 111-growing a quartz crucible; 112-crystal number one; 113-quartz sealing a round plug; 114-graphite felt at the tail of the first crucible; 115-first crucible tail aerogel; 116-a first insulating chamber;
a crystal growth unit No. 120; growing a quartz crucible No. 121; 122-crystal No. two; 123-quartz sealing round plugs; 124-graphite felt at the tail of the No. II crucible; 125-No. two crucible tail aerogel; 126-a second insulating chamber;
130-No. three crystal growth units; 131-growing a quartz crucible; 132-No. three crystals; 133-quartz sealing round plugs; 134-No. three crucible tail graphite felt; 135-No. three crucible tail aerogel; 136-third heat insulation cavity;
141-heating module number one; 142-heating module number two; 143-heating module III; 144-heating module number four; 145-a heating module number five; 146-heating module number six;
151-a first insulation module; 152-first gap filling cotton; 153-a second insulation module; 154-second gap filling cotton; 155-a third heat insulation module; 156-third gap filling cotton; 157-fourth heat preservation module;
161-water cooling inlet number one; 162-water cooling outlet number one; 163-a water cooling inlet; 164-a second water cooling outlet; 165-a water cooling inlet; 166-a water-cooled outlet;
171-first temperature measurement thermocouple; 172 No. two temperature measurement thermocouples; 173-third temperature thermocouple; 174-No. four temperature measurement thermocouple; 175-fifth temperature thermocouple; 176-No. six temperature measurement thermocouples.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-3, the crystal growth system provided by the present invention includes:
a plurality of crystal growth units arranged in succession in a vertical direction; the gradient heating modules are respectively arranged around the peripheral wall of each crystal growth unit; and a heat insulation module is arranged between two adjacent gradient heating modules. The number of the crystal growth units and the gradient heating modules is more than or equal to 2, for example, 3-10, and can be set according to practical application requirements, but not limited to the number. The invention can simultaneously grow a plurality of crystals by adopting a single furnace body, and improves the preparation efficiency of large-size single crystals.
Each gradient heating module is arranged in a continuous surrounding mode, a continuous cavity is formed in the gradient heating module, and when the gradient heating module is used, a crystal growth unit filled with crystal materials is sequentially placed in the cavity, heat preservation and sealing are conducted on the bottom and the top, and synchronous growth of a plurality of crystals can be started. Therefore, the invention has reasonable and simple structure arrangement, small occupied space, good practicality and convenient practical application, and can ensure the uniformity of the temperature field around each crystal.
So arranged, each crystal growth unit corresponds to one gradient heating module, and when the crystal grows, the temperature gradient of the crystal material in the crystal growth unit is controlled through the temperature setting of the crystal growth unit; and because the crystal growth units are continuously arranged, the space can be saved, and the vertical displacement of the crystal growth units can be synchronously regulated and controlled to realize synchronous growth of a plurality of crystals. Meanwhile, heat transfer is reduced through the heat insulation modules between two adjacent gradient heating modules, so that the temperature stability of each crystal growth unit is ensured, and stable regulation and control of +/-0.1 ℃ are achieved.
As shown in fig. 1, in some embodiments, the crystal growth units include a first crystal growth unit 110, a second crystal growth unit 120, and a third crystal growth unit 130.
Each crystal growth unit includes: a growth crucible and a sealing round plug for sealing the growth crucible; the growth crucible includes a crystal growth chamber at the bottom and an insulating chamber at the top. The frosted crucible at the top is formed by frosting the upper part of the growth crucible. The crucible peripheral wall of the crystal growth cavity is of a transparent structure, the crucible peripheral wall of the heat insulation cavity is of a frosted structure, and the heat insulation cavity is in a non-transparent state, so that heat radiation can be reduced. The crucible for crystal growth is usually a transparent crucible to meet the heat transfer, but the invention skillfully frosts the top of the crucible on the basis of vertically and continuously arranging the growth crucibles, thereby effectively reducing the heat radiation between adjacent crucibles and improving the stability of crystal growth.
The heat insulation cavity and the heat insulation module are arranged at the junction of the two crystal growth units, the heat insulation module can block heat transfer between the gradient heating modules, and the heat transfer in the cavity of the gradient heating module can be reduced by the heat insulation cavity, so that the stability of temperature control and the uniformity of crystal growth are realized through the double heat insulation structure.
In particular, a heat insulation layer is also arranged in the heat insulation cavity; the heat insulation layer comprises graphite felt and/or aerogel, so that the heat insulation effect in the cavity is further improved. The connecting end of the growth crucible above is sleeved in the heat insulation cavity below.
As a preferred embodiment, adjacent crystal growth units are detachably connected, and the central axes of each crystal growth unit coincide. So set up, through the relation of connection between the crystal growth unit, can realize synchronous lift regulation and control, and then realize that a furnace body grows a plurality of crystals simultaneously, for example, when setting up three crystal growth unit, braced system only need remove 300mm displacement, just can grow out the crystal that accumulated total length is 900mm, and crystal preparation efficiency is showing and is improving. The length of a single crystal growth according to the present invention may be set to a range of 100-600mm, and the individual elements of the crystal growth unit may be sized accordingly.
Specifically, the first crystal growth unit 110 includes a first growth quartz crucible 111, a first crystal 112 grown inside, a first quartz sealing round plug 113 for sealing the first growth quartz crucible 111, a first heat insulation cavity 116 obtained by polishing the top of the first growth quartz crucible 111, and a heat insulation layer sequentially disposed inside the first heat insulation cavity 116: a number one crucible tail graphite felt 114 and a number one crucible tail aerogel 115. By the arrangement, heat can be effectively prevented from being transferred upwards along quartz, so that the upper part of the crystal is kept at high temperature, and the crystal is fully overheated.
The second crystal growth unit 120 includes a second growth quartz crucible 121, a second crystal 122 grown inside, a second quartz sealing round plug 123 for sealing the second growth quartz crucible 121, a second heat insulation cavity 126 obtained by frosting the top of the second growth quartz crucible 121, and a heat insulation layer sequentially disposed inside the second heat insulation cavity 126: a No. two crucible tail graphite felt 124 and a No. two crucible tail aerogel 125. The second growth quartz crucible 121 is sleeved in the first heat insulation cavity 116, the bottom of the second growth quartz crucible is in contact with the surface of the aerogel 115 at the tail of the first crucible, and a limiting block protruding outwards is arranged on the peripheral wall close to the bottom of the second growth quartz crucible and is in contact with the peripheral wall at the top of the first heat insulation cavity 116 so as to support the second growth quartz crucible 121.
The third crystal growth unit 130 comprises a third growth quartz crucible 131, a third crystal 132 growing inside, a third quartz sealing round plug 133 used for sealing the third growth quartz crucible 131, a third heat insulation cavity 136 obtained by frosting the top of the third growth quartz crucible 131, and a heat insulation layer sequentially arranged inside the third heat insulation cavity 136: a No. three crucible tail graphite felt 134 and a No. three crucible tail aerogel 135. The third growth quartz crucible 131 is sleeved in the second heat insulation cavity 126, the bottom of the third growth quartz crucible is in contact with the surface of the second crucible tail aerogel 125, and a limiting block protruding outwards is arranged on the peripheral wall close to the bottom of the third growth quartz crucible and is in contact with the top peripheral wall of the second heat insulation cavity 126 so as to support the third growth quartz crucible 131. Repeating this, more crystal growth units can be set according to the actual requirements.
Each gradient heating module comprises at least one high temperature heating module and at least one low temperature heating module; respectively used for realizing the melting and crystallization processes of the crystal material. In actual operation, the high temperature heating module and the low temperature heating module can perform a plurality of temperature gradient control again to realize finer temperature adjustment. The invention can adopt a descent method to realize crystal growth, namely, a high-temperature heating module is arranged above a low-temperature heating module, and after the crystal material is completely melted, the crystal material is gradually lowered to a low-temperature area downwards to realize crystallization.
In particular, each of the gradient heating modules is provided with a temperature monitoring assembly, preferably a thermocouple. Moreover, the thermocouple can be inserted into a required position through punching holes on the furnace body so as to monitor the temperature of the temperature field.
As shown in fig. 2 and 3, an insulation module is provided between two adjacent gradient heating modules in order to prevent heat transfer. And heat insulation cotton is also arranged between the heat insulation module and the crystal growth unit in a ring manner, so that heat insulation tightness is improved, and the heat insulation cotton is soft in texture and does not influence movement of the crystal growth unit.
In order to further prevent the heat transfer from the lower high temperature to the upper low temperature, a cooling module is further arranged between two adjacent gradient heating modules, and the cooling module and the heat insulation module are both arranged around the crystal growth unit. In particular, the thermal insulation module is disposed around a peripheral wall of the crystal growth unit; the cooling module is arranged on the outer side of the heat insulation module in a surrounding mode. Through the heat insulation mode and the heat radiation mode, the high-precision regulation and control of the temperature are realized, and the problem that the temperature is difficult to control when the crystal growth units are continuously arranged in the vertical direction is solved.
In some embodiments, the cooling module includes a liquid cooled tube, such as a water cooled tube, that is looped around the outside of the insulation module. The cross section of the water cooling pipe is circular, the height of the water cooling pipe is the same as that of the heat insulation module, and the width of the water cooling pipe can be flexibly set according to actual heat dissipation requirements. The total width of the water cooling pipe and the heat insulation module is larger than or equal to the width of the gradient heating module. So set up, both accessible thermal-insulated and two kinds of modes of heat dissipation realize the high accuracy regulation and control of temperature, can carry out reasonable design to both relative widths again to realize the best regulation and control of temperature stability, consequently the structural flexibility is high.
Specifically, the first crystal growth unit 110 is disposed in a cavity formed by the first heating module 141 and the second heating module 142; the second crystal growth unit 120 is disposed in a cavity formed by the third heating module 143 and the fourth heating module 144; the third crystal growth unit 130 is disposed in a cavity formed by the fifth heating module 145 and the sixth heating module 146.
A first heat insulation module 151 is arranged between the second heating module 142 and the third heating module 143, a first gap filling cotton 152 is arranged between the first heat insulation module 151 and the first heat insulation cavity 116, the cross section of the first gap filling cotton 152 is preferably inverted L-shaped, and sealing heat insulation between the first heat insulation module 151 and the first heat insulation cavity 116 is achieved.
The outer periphery of the first heat insulation module 151 is also provided with a liquid cooling system in a surrounding manner, for example, the first water cooling inlet 161 and the first water cooling outlet 162 in fig. 3 are used for performing water cooling heat dissipation.
A second heat insulation module 153 is arranged between the fourth heating module 144 and the fifth heating module 145, and a second gap filling cotton 154 is arranged between the second heat insulation module 153 and the second heat insulation cavity 126. The periphery of the second heat insulation module 153 is also provided with a liquid cooling system in a surrounding manner, and the liquid cooling system comprises a second water cooling inlet 163 and a second water cooling outlet 164 for performing water cooling heat dissipation.
A third heat insulation module 155 is also arranged above the sixth heating module 146, and a third gap filling cotton 156 is arranged between the third heat insulation module 155 and the third heat insulation cavity 136. The periphery of the third heat insulation module 155 is also provided with a liquid cooling system in a surrounding mode, and the liquid cooling system comprises a third water cooling inlet 165 and a third water cooling outlet 166 for water cooling and heat dissipation.
Particularly, a first heat preservation layer is arranged below the bottommost gradient heating module, and an aluminum silicate block is arranged between the first heat preservation layer and the crystal growth unit in a surrounding mode. In this embodiment, the lower furnace mouth aluminum silicate block 102 below the first heating module 141 is provided with a lower furnace mouth insulation cotton 103 between the lower furnace mouth aluminum silicate block 102 and the first growth quartz crucible 111.
A second heat-insulating layer is arranged above the topmost gradient heating module, a limiting component is arranged between the second heat-insulating layer and the crystal growth unit in a ring mode, and the limiting component is preferably an alumina ceramic ring. In this embodiment, the upper furnace mouth aluminum silicate block 105 above the third heat insulation module 155, an aluminum oxide ring 104 is arranged between the upper furnace mouth aluminum silicate block 105 and the third heat insulation cavity 136,
in particular, a fourth insulation module 157 is also provided between the third insulation module 155 and the upper furnace mouth aluminum silicate block 105.
A liftable supporting base is arranged below the bottommost crystal growth unit. In this embodiment, a liftable support base, such as crucible support base 101 in fig. 1, is provided below growth quartz crucible 111.
So set up, the crucible lower part adopts braced system to fix, and the top adopts the alumina ring to carry out spacingly, and restriction crucible radial displacement from top to bottom simultaneously can make the crucible lift in-process remain better concentricity with the furnace body all the time.
The above elements (e.g., crystal growth unit, gradient heating module, thermal insulation module, etc.) are all disposed within the stainless steel outer furnace shell 100.
In summary, the crystal growth system provided by the invention has the following characteristics:
1. the invention solves the defect of adopting a large cavity to carry out the growth of a plurality of crystals, adopts a cylindrical heating furnace body (namely, a gradient heating module forms a cylindrical cavity), has uniform temperature field in the furnace body and uniform temperature field distribution in the circumferential direction of the crucible, and can obviously improve the uniformity of the crystals.
2. The crystal growth unit is of a step-by-step stacking structure, and each module can be detached independently, so that maintenance and construction are facilitated.
3. According to the system provided by the invention, the number of the crystal growth units can be adjusted according to the requirement, the furnace body can be continuously built upwards according to the similar structure, the number of crystals can be continuously increased, and the number of crystals which can be grown can be customized according to the requirement.
4. The diameter size of the multi-crucible growth equipment is consistent with that of a single crystal growth furnace, and the multi-crucible growth equipment only extends in the height direction, so that the occupied area is small.
5. The tail part of the crucible is frosted, and heat insulation materials such as graphite felt, aerogel and the like are filled in the crucible, so that heat can be effectively prevented from being transferred upwards along quartz, the upper part of the crystal is kept at high temperature, and full overheating is performed.
6. The direct-insert type connection mode is adopted between the upper crucible and the lower crucible, the structure is simple, the implementation is easy, the production of a plurality of support structures is avoided, and the cost is saved.
7. The lower part of the crucible is fixed by adopting a supporting system, the top part of the crucible is limited by adopting an alumina ring, and the radial displacement of the crucible is limited up and down at the same time, so that the crucible can always keep good concentricity with the furnace body in the lifting process;
8. the water cooling jacket is added at the bottom of the low temperature region, so that heat of the lower high temperature region and the upper low temperature region can be taken away, the temperature difference between the high temperature region and the low temperature region is increased, and the growth temperature gradient is further increased.
9. Temperature thermocouples are arranged above and below the initial crystal growth interface, so that the temperature of a high-temperature area and a low-temperature area can be adjusted in real time according to thermocouple feedback without measuring the temperature in advance, the requirements of crystal growth temperature and gradient are met, and time is saved.
The invention also provides a crystal growth method, which adopts the crystal growth system, and comprises the following steps: and regulating and controlling the growth process of the internal crystal material by regulating the displacement of the crystal growth unit in the vertical direction. The invention can grow to obtain a plurality of crystals only by adopting the same descending height as the prior art, thereby obviously improving the growth efficiency.
Specifically, the growth method comprises:
s1, respectively filling polycrystalline materials into each growth crucible, sealing by adopting a sealing round plug, and then filling a first growth crucible into a cavity formed by the gradient heating module;
for example, the first grown quartz crucible 111 is filled with the polycrystalline material, sealed, and then filled into a cavity formed by the first heating module 141 and the second heating module 142;
s2, performing sand blasting treatment on the upper part of the growth crucible to form a frosted heat insulation cavity, and arranging a heat insulation layer in the heat insulation cavity;
for example, the top of the first grown quartz crucible 111 is frosted to form a first heat insulation cavity 116, and then a first crucible tail graphite felt 114 and a first crucible tail aerogel 115 are sequentially placed inside the first heat insulation cavity;
s3, sleeving a second growth crucible in the first heat insulation cavity 116, and repeating the step S2, and sequentially loading the second growth crucible into each crystal growth unit for assembly;
for example, a second growth quartz crucible 121 is sleeved in the first heat insulation cavity 116, the bottom of the second growth quartz crucible is clung to the first crucible tail aerogel 115, then a second heat insulation cavity 126 is arranged at the top of the second growth quartz crucible, and a second crucible tail graphite felt 124 and a second crucible tail aerogel 125 are sequentially arranged in the second heat insulation cavity 126. Other crystal growth units were placed in the same manner.
And S4, after the crystal growth units are assembled and sealed, synchronously starting the gradient heating modules and the cooling modules, and synchronously driving each growth crucible to descend through the support base after the polycrystalline materials are completely melted, so as to complete growth.
Specifically, the temperature of the heating zone at the initial position of the crystal is higher than that of the lower heating zone, so that a temperature gradient is generated;
after the temperature is raised to the high temperature, the temperature of the high temperature area and the temperature of the low temperature area are adjusted according to thermocouple feedback data, so that the high temperature is higher than the crystal growth point, and the material is ensured to be sufficiently melted; then according to the temperature gradient requirement, the low temperature and the water cooling liquid temperature are adjusted to enable the gradient to meet the crystal growth requirement;
and then setting the growth displacement and speed, and starting to descend the crucible supporting system to drive the crucible to synchronously descend so as to realize the simultaneous growth of a plurality of crystals.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A crystal growth system, comprising:
a plurality of crystal growth units arranged in succession in a vertical direction;
a gradient heating module is arranged on the peripheral wall of each crystal growth unit in a surrounding way;
and a heat insulation module is arranged between two adjacent gradient heating modules.
2. The crystal growth system of claim 1, wherein a cooling module is further disposed between two adjacent gradient heating modules, the cooling module and the insulating module each being disposed around the crystal growth unit;
preferably, the heat insulating module is disposed around a peripheral wall of the crystal growth unit; the cooling module is arranged on the outer side of the heat insulation module in a surrounding mode;
preferably, the cooling module comprises a liquid cooling pipe which is arranged on the outer side of the heat insulation module in a surrounding mode.
3. The crystal growth system of claim 2, wherein a thermal insulation cotton is further disposed between the thermal insulation module and the crystal growth unit in a ring shape, and the thermal insulation cotton has an inverted "L" shape in cross section.
4. A crystal growth system according to any one of claims 1-3, wherein each of the crystal growth units comprises:
a growth crucible comprising a crystal growth cavity at the bottom and a thermally insulated cavity at the top; the crucible peripheral wall of the crystal growth cavity is of a transparent structure, and the crucible peripheral wall of the heat insulation cavity is of a frosted structure;
and sealing a round plug for sealing the growth crucible.
5. The crystal growth system of claim 4, wherein adjacent ones of the crystal growth units are detachably connected with each other and central axes of the crystal growth units coincide.
6. The crystal growth system of claim 5, wherein the insulating chamber is further provided with an insulating layer;
preferably, the insulating layer comprises graphite felt and/or aerogel.
7. The crystal growth system of any of claims 1-6, wherein each of the gradient heating modules comprises at least one high temperature heating module and at least one low temperature heating module;
preferably, in each of the gradient heating modules, the high temperature heating module is disposed above the low temperature heating module.
8. Crystal growth system according to any of claims 1-7, wherein each of the gradient heating modules is provided with a temperature monitoring assembly, preferably a thermocouple;
and/or a liftable support base is arranged below the bottommost crystal growth unit;
and/or a first heat-insulating layer is arranged below the gradient heating module at the bottommost part, and an aluminum silicate block is arranged between the first heat-insulating layer and the crystal growth unit in a ring manner;
and/or a second heat-insulating layer is arranged above the gradient heating module at the top, and a limiting component is arranged between the second heat-insulating layer and the crystal growth unit in a surrounding manner;
the spacing component is preferably an alumina ceramic ring.
9. A crystal growth method, characterized in that the crystal growth system according to any one of claims 1 to 8 is employed, the crystal growth method comprising:
and regulating and controlling the growth process of the internal crystal material by regulating the displacement of the crystal growth unit in the vertical direction.
10. The crystal growth method according to claim 9, wherein the step of regulating the growth process of the internal crystal material by adjusting the displacement of the crystal growth unit in the vertical direction comprises:
s1, respectively filling polycrystalline materials into each growth crucible, sealing by adopting a sealing round plug, and then filling a first growth crucible into a cavity formed by the gradient heating module;
s2, a heat insulation layer is arranged in a heat insulation cavity at the top of the first growth crucible;
s3, sleeving a second growth crucible in the heat insulation cavity of the first growth crucible, and repeating the step S2, and sequentially loading the second growth crucible into the crystal growth units for assembly;
s4, starting the gradient heating module and the cooling module, and synchronously driving each growth crucible to descend through the support base after the polycrystalline material is completely melted, so that growth is completed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117232259A (en) * | 2023-11-15 | 2023-12-15 | 国镓芯科(成都)半导体科技有限公司 | Sectional type samming heating furnace |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117232259A (en) * | 2023-11-15 | 2023-12-15 | 国镓芯科(成都)半导体科技有限公司 | Sectional type samming heating furnace |
| CN117232259B (en) * | 2023-11-15 | 2024-01-26 | 国镓芯科(成都)半导体科技有限公司 | Sectional type samming heating furnace |
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