CN106757307A - 1 13 method for monocrystal growth of a kind of 14 inch arsenide gallium monocrystal stoves and its drawing - Google Patents
1 13 method for monocrystal growth of a kind of 14 inch arsenide gallium monocrystal stoves and its drawing Download PDFInfo
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- CN106757307A CN106757307A CN201710102779.1A CN201710102779A CN106757307A CN 106757307 A CN106757307 A CN 106757307A CN 201710102779 A CN201710102779 A CN 201710102779A CN 106757307 A CN106757307 A CN 106757307A
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
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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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/42—Gallium arsenide
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses 1 13 method for monocrystal growth of a kind of 14 inch arsenide gallium monocrystal stove and its drawing, including 14 inch burner hearths, 2 inch PBN components, heat-preservation cotton, combustion chamber, quartz ampoule, annular-heating piece, capping;The 14 inch burner hearth is cylindrical, and 3 10 sections of thermal fields are divided into along its short transverse in the 14 inch burner hearth, and multiple temperature control points are provided with the region of 3 10 sections of thermal fields, and the quartz ampoule is arranged on the bottom in 14 inch burner hearths, and the combustion chamber is arranged in quartz ampoule;A kind of growing method of 14 inch arsenide gallium monocrystal, the growing method is synthesized using multicell arsenide gallium monocrystal growth furnace.Present device high precision, the temperature control point for being wherein distributed in 3 10 sections of thermal fields has 3 10, stability contorting thermal field, set up suitable thermal field gradient, and then the suitable temperature control rule that multiple 2 inch monocrystal rods grow simultaneously is effectively grasped, and disposably batch type growth 1 13 monocrystalline can be obtained, the production efficiency of GaAs crystal bar can be greatly improved, and shaping rate is higher, up to 80% 100%.
Description
Technical field
The present invention relates to single crystal preparation technical field, more particularly to a kind of 14 inch arsenide gallium monocrystal stove and its drawing 1-13 root lists
Crystals growth method.
Background technology
GaAs (gallium arsenide), belongs to group Ⅲ-Ⅴ compound semiconductor, with high-frequency, high electron mobility
The advantageous characteristic such as rate, high-output power, low noise and the linearity be good.High-end Military Electronics application, optical fiber is related generally to lead to
The fields such as letter system, broadband satellite wireless communication system, tester, automotive electronics, laser, illumination.Partly led as important
Body material, the electron mobility of GaAs is 5 times of silicon and gallium nitride, for middle low power microwave device there is lower power to damage
Consumption, therefore occupied an leading position in the fields such as mobile communication, LAWN local area wireless network, GPS and car radar.
Method for monocrystal growth uses VGF (VGF).Gallium arsenide polycrystal is placed in PBN crucibles, then
Sealed after being vacuumized in quartz ampoule is placed on, is then placed into single crystal growing furnace, by adjusting the temperature change of each warm area in stove, promoted
Growth interface movement generation monocrystalline.The method is typically disposably to grow a crystal bar, it is impossible to accomplish disposable batch type growth,
That is a stove draws many with crystal bar.This is because VGF pulling monocrystal is higher to temperature control requirement, it is necessary to have
A whole set of complete, ripe temperature control scheme could grow mass crystal bar higher.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.Therefore, of the invention
One purpose is to propose a kind of 14 inch arsenide gallium monocrystal stove and its draw 1-13 root method for monocrystal growth, greatly improves GaAs brilliant
The production efficiency of rod, temperature control scheme is ripe, disposably batch type growth can obtain 1-13 root monocrystalline.
A kind of 14 inch arsenide gallium monocrystal stove according to embodiments of the present invention, including 14 inch burner hearths, 2 inch PBN components, insulation
Cotton, combustion chamber, quartz ampoule, annular-heating piece, capping;
The 14 inch burner hearth is cylindrical, and 3-10 sections of thermal field, the 3- are divided into along its short transverse in the 14 inch burner hearth
Multiple temperature control points are provided with the 10 sections of 3-10 of thermal field sections of regions, the quartz ampoule is arranged on the bottom in 14 inch burner hearths, the stove
Core is arranged in quartz ampoule, and heat-preservation cotton is provided between the quartz ampoule and combustion chamber, and the annular-heating piece is fixed on 14 inch burner hearths
Inwall on, and annular-heating piece is serrated near the one side of quartz ampoule, and the 2 inch PBN components are integrally cylindrical, its
Bottom is in funnel-form, described to cover the top open part for being arranged on 14 inch burner hearths inside quartz supports.
Further, the quantity of temperature control point is 21-35, and 10 temperature are evenly distributed with the 3-10 sections of epimere region of thermal field
Control point, is evenly distributed with 15 temperature control points in the 3-10 sections of stage casing region of thermal field, uniformly divide in the 3-10 sections of hypomere region of thermal field
It is furnished with 10 temperature control points.
Further, the quantity of the 2 inch PBN components is 13, is uniformly arranged in the arbitrary arrangement mode of 3-2-3-2-3
Row.
A kind of 14 inch arsenide gallium monocrystal stove draws the growing method of 1-13 root monocrystalline, comprises the following steps:
(1) 3-10 sections of 1150-1200 DEG C of the epimere region of thermal field, stage casing region 1280- were heated to 1.5 hours
1350 DEG C, 3-10 sections 1220-1260 DEG C of the hypomere regions of thermal field, are then incubated 1.5 hours;
(2) gallium arsenide polycrystal, seed crystal are fitted into 2 inch PBN components, then are placed in quartz ampoule and vacuumize, when vacuum is
6.5×10-3After Pa, soldering and sealing is carried out to quartz ampoule by oxyhydrogen flame, then quartz ampoule is put into 14 inch burner hearths;
(3) growth temperature in 3-10 sections of thermal field is controlled by temperature control point, heats to the 3-10 sections of hypomere area of thermal field
1240 DEG C of the hypomere region of 1300 DEG C, 3-10 sections of the stage casing region thermal field of 1200 DEG C, 3-10 sections of domain thermal field, is incubated 1.5 hours, makes
Raw materials melt, then the upper of 3-10 sections of thermal field of holding, stage casing regional temperature are constant, the 3-10 sections of hypomere regional stability reduction of thermal field
It is 1180 DEG C, temperature fall time is 24 hours, grows crystal shoulder stabilization, then at the uniform velocity reduce temperature, makes 3-10 sections of thermal field
1220 DEG C of the hypomere region of 1280 DEG C, 3-10 sections of the stage casing region thermal field of 1160 DEG C, 3-10 sections of hypomere region thermal field, temperature fall time
It is 12 hours, grows crystal equal-diameter part stabilization;
(4) after gallium arsenide terminates, in-furnace temperature is reduced to 1150 DEG C, is incubated 12h, then with 25 DEG C/it is small
When near room temperature, crystal growth finishes, and obtains the inch arsenide gallium monocrystal of 1-13 roots 2.
In the present invention, equipment precision is high, wherein the temperature control point for being distributed in 3-10 sections of thermal field has 10, stability contorting thermal field,
Suitable thermal field gradient is set up, and then effectively grasps the suitable temperature control rule that multiple 2 inch monocrystal rods grow simultaneously, can be significantly
The production efficiency of GaAs crystal bar is improved, and shaping rate is higher, up to 80%-100%, 3-10 sections of thermal field temperature control o'clock is more than 50
Individual, stability contorting thermal field, top laying heat-preservation cotton is simultaneously covered, and with sealed thermal insulating, energy saving, using annular-heating piece, makes heat
The uniform energy-conservation in field, disposably batch type growth can obtain the inch monocrystalline of 1-13 roots 14.
Further, the length of arsenide gallium monocrystal is 120-350mm.
The setting of the annular-heating piece of 3-10 sections of thermal field of the present invention plays an important role to thermal field uniformity;Greatly improve list
Brilliant yield;Effect to monocrystalline Quality advance.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the cross-sectional view of 14 inch arsenide gallium monocrystal stove of the invention;
Fig. 2 is the top cross-sectional view of 14 inch arsenide gallium monocrystal stove of the invention;
Fig. 3 is the part-structure schematic diagram of annular-heating piece.
In figure:1 14 inch burner hearths, 22 inch PBN components, 3 heat-preservation cottons, combustion chamber 4,5 quartz ampoules, 6 annular-heating pieces, 7 capping,
8 3-10 sections of thermal field.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.
The example of the embodiment is shown in the drawings, wherein same or similar label represents identical or class from start to finish
As element or the element with same or like function.Embodiment below with reference to Description of Drawings is exemplary, purport
For explaining the present invention, and it is not considered as limiting the invention.
In the description of the invention, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
" thickness ", " on ", D score, "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom " " interior ", " outward ", " up time
The orientation or position relationship of the instruction such as pin ", " counterclockwise ", " axial direction ", " radial direction ", " circumference " be based on orientation shown in the drawings or
Position relationship, is for only for ease of the description present invention and simplifies description, must rather than the device or element for indicating or imply meaning
With specific orientation, with specific azimuth configuration and operation, therefore must be not considered as limiting the invention.
Additionally, term " first ", " second " are only used for describing purpose, and it is not intended that indicating or implying relative importance
Or the implicit quantity for indicating indicated technical characteristic.Thus, define " first ", the feature of " second " can express or
Implicitly include one or more this feature.In the description of the invention, " multiple " is meant that two or more,
Unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " fixation " etc.
Term should be interpreted broadly, for example, it may be fixedly connected, or be detachably connected, or integrally;Can be that machinery connects
Connect, or electrically connect;Can be joined directly together, it is also possible to be indirectly connected to by intermediary, can be in two elements
The connection in portion or two interaction relationships of element.For the ordinary skill in the art, can be according to specific feelings
Condition understands above-mentioned term concrete meaning in the present invention.
Embodiment 1
Reference picture 1-3, a kind of 14 inch arsenide gallium monocrystal stove, including 14 inch burner hearths 1,2 inch PBN components, heat-preservation cotton 3, combustion chamber
4th, quartz ampoule 5, annular-heating piece 6, capping 7;
14 inch burner hearths are cylindrical, and 3 sections of thermal fields 8, the 3-10 sections of region of thermal field 8 are divided into along its short transverse in 14 inch burner hearths
Multiple temperature control points are inside provided with, quartz ampoule 5 is arranged on the bottom in 14 inch burner hearths 1, and combustion chamber 4 is arranged in quartz ampoule 5, quartz ampoule 5
Heat-preservation cotton 3 is provided between combustion chamber 4, annular-heating piece 6 is fixed on the inwall of 14 inch burner hearths 1, and annular-heating piece 6 is close to
The one side of quartz ampoule 5 is serrated, and increases the area of annular-heating piece 6 so that the uniform simultaneously energy-conservation of thermal field, 2 inch PBN components 2 are overall
Cylindrical, its bottom is in funnel-form, and inside quartz supports 5, capping 7 is arranged on the top open part of 14 inch burner hearths 1.
Further, the quantity of temperature control point is 21, and 3 temperature control points are evenly distributed with 3 sections of hypomere regions of thermal field 8,
15 temperature control points are evenly distributed with the 3-10 sections of stage casing region of thermal field 8, are evenly distributed with the 3-10 sections of hypomere region of thermal field 8
3 temperature control points.
Further, the quantity of 2 inch PBN components 2 is 13, evenly distributed in the arbitrary arrangement mode of 3-2-3-2-3.
A kind of 14 inch arsenide gallium monocrystal stove draws the growing method of 1-13 root monocrystalline, comprises the following steps:
(1) 3-10 sections of 1150 DEG C of the epimere region of thermal field 8,1280 DEG C of stage casing region, 3-10 were heated to 1.5 hours
1220 DEG C of the hypomere region of section thermal field 8, is then incubated 1.5 hours;
(2) gallium arsenide polycrystal, seed crystal are fitted into 2 inch PBN components 2, then are placed in quartz ampoule 5 and vacuumize, work as vacuum
It is 6.5 × 10-3After Pa, soldering and sealing is carried out to quartz ampoule 5 by oxyhydrogen flame, then quartz ampoule is put into 14 inch burner hearths;
(3) growth temperature in 3-10 sections of thermal field 8 is controlled by temperature control point, heats to the 3-10 sections of hypomere of thermal field 8
1240 DEG C of the hypomere region of 1300 DEG C, 3-10 sections of the stage casing region thermal field 8 of 1200 DEG C, 3-10 sections of region thermal field 8, insulation 1.5 is small
When, make raw materials melt, then the upper of 3-10 sections of thermal field 8 of holding, stage casing regional temperature are constant, the 3-10 sections of hypomere region of thermal field 8
Steady decrease is 1180 DEG C, and temperature fall time is 24 hours, grows crystal shoulder stabilization, then at the uniform velocity reduces temperature, makes 3-10
The hypomere region 1220 of 1280 DEG C, 3-10 sections of the stage casing region thermal field 8 of 1160 DEG C, 3-10 sections of the hypomere region thermal field 8 of section thermal field 8
DEG C, temperature fall time is 12 hours, grows crystal equal-diameter part stabilization;
(4) after gallium arsenide terminates, in-furnace temperature is reduced to 1150 DEG C, is incubated 12h, then with 25 DEG C/it is small
When near room temperature, crystal growth finishes, and obtains the inch arsenide gallium monocrystal of 1-13 roots 2.
The length of arsenide gallium monocrystal is 120mm
14 inch arsenide gallium monocrystal furnace apparatus high precisions of the invention, wherein the temperature control point for being distributed in 3-10 sections of thermal field 8 has 10,
Stability contorting thermal field, sets up suitable thermal field gradient, and then effectively grasp the suitable temperature control that multiple 2 inch monocrystal rods grow simultaneously
Rule, can greatly improve the production efficiency of GaAs crystal bar, and shaping rate is higher, up to 80%-100%, 3-10 sections of thermal field 8
More than 20, stability contorting thermal field, top laying heat-preservation cotton is simultaneously covered, and with sealed thermal insulating, energy saving uses annular for temperature control o'clock
Heating plate, makes the uniform energy-conservation of thermal field.
Embodiment 2
A kind of 14 inch arsenide gallium monocrystal stove draws the growing method of 1-13 root monocrystalline, and method and step is with embodiment 1, different process
Parameter is:
The quantity of temperature control point is 35, and 10 temperature control points, 3-10 temperature are evenly distributed with the 3-10 sections of epimere region of thermal field
15 temperature control points are evenly distributed with the stage casing region of field, 10 temperature controls are evenly distributed with the 3-10 sections of hypomere region of thermal field
Point.
(1) 3-10 sections of 1200 DEG C of the epimere region of thermal field 8,1350 DEG C of stage casing region, 3-10 were heated to 1.5 hours
1260 DEG C of the hypomere region of section thermal field 8, is then incubated 1.5 hours;
Embodiment 3
A kind of 14 inch arsenide gallium monocrystal stove draws the growing method of 1-13 root monocrystalline, and method and step is with embodiment 1, different process
Parameter is:
The quantity of temperature control point is 30, and 7 temperature control points, 3-10 thermal fields are evenly distributed with the 3-10 sections of epimere region of thermal field
Stage casing region in be evenly distributed with 15 temperature control points, 8 temperature control points are evenly distributed with the 3-10 sections of hypomere region of thermal field.
(1) 3-10 sections of 1155 DEG C of the epimere region of thermal field 8,1300 DEG C of stage casing region, 3-10 were heated to 1.5 hours
1245 DEG C of the hypomere region of section thermal field 8, is then incubated 1.5 hours;
The length of arsenide gallium monocrystal is 350mm
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be with
It is the first and second feature directly contacts, or the first and second features are by intermediary mediate contact.And, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature are directly over second feature or oblique upper, or be merely representative of
Fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " lower section " and " below " can be
One feature is immediately below second feature or obliquely downward, or is merely representative of fisrt feature level height less than second feature.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or spy that the embodiment or example are described
Point is contained at least one embodiment of the invention or example.In this manual, to the schematic representation of above-mentioned term not
Necessarily refer to identical embodiment or example.And, the specific features of description, structure, material or feature can be any
One or more embodiments or example in combine in an appropriate manner.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (5)
1. a kind of 14 inch arsenide gallium monocrystal stove, it is characterised in that:Including 14 inch burner hearths, 2 inch PBN components, heat-preservation cotton, combustion chamber, stone
Ying Guan, annular-heating piece, capping;
The 14 inch burner hearth is cylindrical, and 3-10 sections of thermal field is divided into along its short transverse in the 14 inch burner hearth, described 3-10 sections
Multiple temperature control points are provided with the region of thermal field, the quartz ampoule is arranged on the bottom in 14 inch burner hearths, and the combustion chamber is arranged on stone
In English pipe, heat-preservation cotton is provided between the quartz ampoule and combustion chamber, the annular-heating piece is fixed on the inwall of 14 inch burner hearths, and
And annular-heating piece is serrated near the one side of quartz ampoule, the 2 inch PBN components are integrally cylindrical, and its bottom is in funnel
Shape, it is described to cover the top open part for being arranged on 14 inch burner hearths inside quartz supports.
2. 14 inch arsenide gallium monocrystal stove according to claim 1, it is characterised in that:The quantity of temperature control point is 21-35,3-
3-10 temperature control point is evenly distributed with 10 sections of epimere regions of thermal field, 15 are evenly distributed with the stage casing region of 3-10 thermal fields
Temperature control point, is evenly distributed with 3-10 temperature control point in the 3-10 sections of hypomere region of thermal field.
3. 14 inch arsenide gallium monocrystal stove according to claim 1, it is characterised in that:The quantity of the 2 inch PBN components is 13
It is individual, it is evenly distributed in the arbitrary arrangement mode of 3-2-3-2-3.
4. the method that the 14 inch arsenide gallium monocrystal stoves according to claim any one of 1-3 draw 1-13 root monocrystalline, its feature exists
In:Comprise the following steps:
(1 with heat within 1.5 hours 3-10 sections of 1150-1200 DEG C of the epimere region of thermal field, 1280-1350 DEG C of stage casing region,
1220-1260 DEG C of hypomere region, is then incubated 1.5 hours;
(2) gallium arsenide polycrystal, seed crystal are fitted into 2 inch PBN components, then are placed in quartz ampoule and vacuumize, when vacuum be 6.5 ×
10-3After Pa, soldering and sealing is carried out to quartz ampoule by oxyhydrogen flame, then quartz ampoule is put into 14 inch burner hearths;
(3) growth temperature in 3-10 sections of thermal field is controlled by temperature control point, heats to the 3-10 sections of hypomere region of thermal field
1200 DEG C, 5-6 sections 1240 DEG C of the hypomere regions of 1300 DEG C, 3-4 sections of the stage casing region of thermal field thermal field, are incubated 1.5 hours, make raw material
Melting, then the upper of 3-10 sections of thermal field of holding, stage casing regional temperature are constant, and the hypomere regional stability of 3-10 sections of thermal field is reduced to
1180 DEG C, temperature fall time is 24 hours, grows crystal shoulder stabilization, temperature is then at the uniform velocity reduced, under making 3-10 sections of thermal field
1220 DEG C of the hypomere region of 1280 DEG C, 3-10 sections of the stage casing region thermal field of section 1160 DEG C, 3-10 sections of region thermal field, temperature fall time is
12 hours, grow crystal equal-diameter part stabilization;
(4) after gallium arsenide terminates, in-furnace temperature is reduced to 1150 DEG C, is incubated 12h, then will with 25 DEG C/h
To room temperature, crystal growth is finished, and obtains 1-13 root arsenide gallium monocrystals.
5. the length of arsenide gallium monocrystal prepared by method and step according to claim 4 is 120-350mm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110923802A (en) * | 2019-12-24 | 2020-03-27 | 西安交通大学 | A multi-crucible crystal growth furnace with independently controllable stations and control method |
CN114485171A (en) * | 2021-12-31 | 2022-05-13 | 武汉锐科光纤激光技术股份有限公司 | Temperature control furnace and temperature control method thereof |
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CN105696072A (en) * | 2016-04-12 | 2016-06-22 | 常州亿晶光电科技有限公司 | Sapphire crystal growth furnace |
CN207452293U (en) * | 2017-02-24 | 2018-06-05 | 江西德义半导体科技有限公司 | A kind of 14 inches of arsenide gallium monocrystal stoves |
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JPH08259371A (en) * | 1995-03-27 | 1996-10-08 | Sumitomo Sitix Corp | Single crystal growth method with excellent SR uniformity |
US6139627A (en) * | 1998-09-21 | 2000-10-31 | The University Of Akron | Transparent multi-zone crystal growth furnace and method for controlling the same |
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CN110923802A (en) * | 2019-12-24 | 2020-03-27 | 西安交通大学 | A multi-crucible crystal growth furnace with independently controllable stations and control method |
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