CN110760931A - System for preparing indium phosphide crystal by indium phosphide mixture - Google Patents
System for preparing indium phosphide crystal by indium phosphide mixture Download PDFInfo
- Publication number
- CN110760931A CN110760931A CN201911155614.6A CN201911155614A CN110760931A CN 110760931 A CN110760931 A CN 110760931A CN 201911155614 A CN201911155614 A CN 201911155614A CN 110760931 A CN110760931 A CN 110760931A
- Authority
- CN
- China
- Prior art keywords
- chamber
- indium phosphide
- feeding
- crucible
- indium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000013078 crystal Substances 0.000 title claims abstract description 57
- 239000000203 mixture Substances 0.000 title claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 53
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 53
- 230000007246 mechanism Effects 0.000 claims abstract description 12
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 34
- 238000011068 loading method Methods 0.000 claims description 23
- 230000007306 turnover Effects 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 4
- 230000003028 elevating effect Effects 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 abstract description 9
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 abstract description 9
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- -1 and after synthesis Chemical compound 0.000 abstract 1
- 210000001503 joint Anatomy 0.000 abstract 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 20
- 229910052698 phosphorus Inorganic materials 0.000 description 20
- 239000011574 phosphorus Substances 0.000 description 20
- 239000007789 gas Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 18
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 14
- 229910052738 indium Inorganic materials 0.000 description 13
- 239000000155 melt Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012840 feeding operation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
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
- 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
-
- 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
-
- 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
Landscapes
- 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 system for preparing indium phosphide crystals by using an indium-phosphorus mixture, which belongs to the technical field of semiconductors and comprises a vacuum system, an air charging and discharging system, a temperature and pressure control system, an electrical control system, a cooling circulation system, a weighing system and a furnace body, wherein the furnace body is provided with a crucible rod rotating and lifting mechanism and a seed rod lifting mechanism, and the key points are that: the furnace body is divided into a synthetic growth chamber, a feeding chamber and a charging chamber, the charging chamber and the feeding chamber are divided by means of an inserting plate, an overturning feeding device is arranged in the charging chamber, a feeding pipe is arranged in the feeding chamber, one end of the feeding pipe is in butt joint with the overturning feeding device, and the other end of the feeding pipe extends into a crucible in the synthetic growth chamber to form an indium-phosphorus mixed ball feeding structure; the crucible is positioned on a crucible rod, and the seed rod lifting mechanism is arranged on the top cover of the synthesis growth chamber. The indium-phosphorus mixed balls can be quickly put into a crucible covered with liquid boron oxide, and after synthesis, indium phosphide crystals are formed by in-situ pulling, so that the synthesis speed is higher, and the industrial production is facilitated.
Description
Technical Field
The invention belongs to the technical field of semiconductors, relates to preparation of indium phosphide, and particularly relates to a method for synthesizing indium phosphide by using indium-phosphorus mixed balls.
Background
Indium phosphide (InP) is a III-V compound semiconductor material formed by compounding III-group element indium (In) and V-group element phosphorus (P), has very important strategic position In the field of semiconductor materials, and is an irreplaceable semiconductor material for photoelectric devices and microelectronic devices at present. InP has many advantages compared to germanium, silicon materials: the direct transition type energy band structure has high electro-optic conversion efficiency; the electron mobility is high, the semi-insulating material is easy to manufacture, and the preparation method is suitable for manufacturing high-frequency microwave devices and circuits; the working temperature is high; has strong radiation resistance; high conversion efficiency as a solar cell material, and the like. Therefore, InP and other materials are widely used in the high-tech fields of solid-state light emission, microwave communication, optical fiber communication, microwaves, millimeter wave devices, radiation-resistant solar cells, and the like. With the development of band engineering theory, ultra-thin material process technology and deep submicron manufacturing technology, InP also shows more and more its advantages in high-end microwave, millimeter wave electronic devices and optoelectronic devices, and becomes the preferred material for millimeter wave high-end devices, and is widely valued and has a very broad development and application prospect. The implementation of high-end InP-based microelectronic and optoelectronic devices depends on the preparation of high quality InP single crystals with good integrity, uniformity and thermal stability. The high-purity InP polycrystal materials with different melt ratios and no inclusion are the precondition for producing high-quality InP single crystal and carrying out InP related characteristic research. Many characteristics of InP single crystals are related to characteristics of the starting material, i.e., the polycrystalline material, such as the mixture ratio of the polycrystalline material and the purity of the material. The properties of polycrystalline materials have a large impact on crystal growth, electrical behavior of the crystal, integrity, uniformity of the crystal, and the like.
At present, several commonly used methods for synthesizing InP polycrystalline materials and the problems thereof are as follows:
(1) horizontal Bridgman method (HB) and horizontal gradient freezing method (HGF): the InP material is synthesized by adopting a horizontal Bridgman method (HB) and a horizontal gradient solidification method (HGF), the synthesis time is longer when the synthesis amount is larger, about 24 hours is required for synthesizing 1.5KgInP polycrystal by using an HB/HGF technology generally, and therefore, the contamination of Si is more obvious (the source is a quartz tube wall).
(2) Phosphorus injection method synthesis technology: the phosphorus injection method is characterized in that gasified phosphorus vapor is injected into the indium melt, the contact area of phosphorus gas and the indium melt is accelerated, convection in the indium melt is increased through crucible rotation, diffusion of solute in a solute diffusion layer is accelerated, and therefore the synthesis process is accelerated. Because the method injects phosphorus vapor by depending on the pressure difference between the inside and the outside of the quartz phosphorus container, once the pressure difference is controlled improperly, the bubbles are easy to be blown; on the other hand, part of phosphorus vapor is not absorbed by the indium melt, which affects the synthesis effect on the one hand, and on the other hand, the lost phosphorus vapor volatilizes into the furnace body, which brings great trouble to the cleaning of the furnace body. And it is very demanding for thermal field control in the synthesis system.
The synthesis methods of the horizontal Bridgman method (HB), the horizontal gradient solidification method (HGF), the ultrahigh pressure direct synthesis technology and the like firstly carry out InP synthesis in a synthesis furnace, then the synthesized InP polycrystalline material is taken out from the synthesis furnace, the polycrystalline material is cleaned and corroded, and then the polycrystalline material is put into a high-pressure single crystal furnace for InP single crystal growth. Synthesis and crystal growth are performed in a "two-step" process, which greatly increases the likelihood of contamination of the material and increases the cost of material preparation.
Disclosure of Invention
The invention provides a system for preparing indium phosphide by using an indium-phosphorus mixture, which can quickly put indium-phosphorus mixed balls into a crucible covered with liquid boron oxide, and pull an indium-phosphorus melt to form an indium phosphide crystal after the required synthesis amount is reached, so that the synthesis speed is higher, the control requirement is reduced, and the industrial production is facilitated.
The technical scheme of the invention is as follows: the utility model provides an utilize indium phosphorus mixture preparation indium phosphide crystal's system, includes vacuum system, fills gassing system, temperature and pressure control system, electric control system, cooling circulation system, weighing system and furnace body, is provided with rotatory elevating system of crucible pole and seed crystal pole elevating system on the furnace body, and the key lies in: the furnace body is divided into a synthetic growth chamber, a feeding chamber and a charging chamber, the charging chamber and the feeding chamber are divided by means of an inserting plate, an overturning feeder is arranged in the charging chamber, a feeding pipe is arranged in the feeding chamber, one end of the feeding pipe is upwards butted with the overturning feeder, and the other end of the feeding pipe extends downwards to a crucible in the synthetic growth chamber to form an indium-phosphorus mixed ball feeding structure; the crucible is positioned on a crucible rod, and the seed rod lifting mechanism is arranged on the top cover of the synthesis growth chamber.
In the system, the furnace body is divided into a synthesis growth chamber, a feeding chamber and a charging chamber, indium-phosphorus mixed balls can be loaded into an overturning feeder of the charging chamber, and then the indium-phosphorus mixed balls are fed into a crucible through feeding pipes of the feeding chamber and the synthesis growth chamber for melting and synthesis, and crystal growth can be carried out in situ after synthesis. The feeding chamber and the charging chamber are separated by the aid of the inserting plate, can be communicated during feeding, and can be isolated during charging of the material loading device, so that the synthesis or crystal growth in the synthesis growth chamber can be realized, and meanwhile, the feeding and the material supplementing are carried out.
Furthermore, the turnover feeder comprises a mechanical arm, a material loading device and a material loading device turnover driving device, wherein the upper end of the mechanical arm is positioned at the top of the loading chamber, the lower end of the mechanical arm is connected with the turnover driving device, and the turnover driving device is connected with the material loading device. The mechanical arm plays the roles of installation and positioning and is used for suspending the material loading device in the loading chamber so as to conveniently feed materials in a closed and low-temperature manner. The overturning driving device is used for driving the material loading device to overturn and feed.
Furthermore, in order to simplify the structure and facilitate control, the loader overturning driving device adopts a motor positioned at the bottom end of the mechanical arm, and a motor shaft is connected with the loader.
Furthermore, in order to avoid the influence of the environment in the furnace on the performance of the motor, the motor is coated with a heat insulation layer and a protective cover.
Further, the gas charging and discharging system comprises a low-temperature inert gas storage tank, a gas inlet and a gas outlet which are respectively arranged at the top of the charging chamber and the bottom of the synthetic growth chamber, and the gas inlet is higher than the inlet of the feeding pipe; the low-temperature inert gas enters the feeding chamber from the charging chamber, enters the synthetic growth chamber through the feeding pipe, is fed above the crucible and is discharged from the exhaust port. The system needs to control the temperature of the inert gas to be lower than the melting point of indium, namely the temperature is lower than 156 ℃. The low-temperature inert gas flows and is delivered along with the low-temperature inert gas, so that the low temperature in the process of feeding the indium-phosphorus mixed balls from the material loading device to the crucible can be kept, indium or phosphorus is not melted and gasified, the indium is prevented from melting and sticking to the wall, the phosphorus is prevented from volatilizing in the feeding process, and the synthetic ratio is prevented from being influenced.
Further, the pressure value in the furnace body is 3.5-5.0 MPa. The pressure is higher than the decompression pressure of the indium phosphide melt, so that the indium phosphide dissociation can be avoided, and the synthesis and growth can be ensured. Meanwhile, because the pressure of the feeding chamber is 0.05-0.1Mpa higher than that of the synthesis growth chamber, and low-temperature gas can enter from the upper part, the indium-phosphorus mixed balls and the low-temperature gas can be ensured to enter the upper part of a crucible of the synthesis growth space together, and the indium or phosphorus is prevented from being melted and gasified before the indium-phosphorus mixed balls enter a melt.
Furthermore, in order to facilitate the observation of the synthesis and the crystal growth, a first observation window is arranged on the furnace wall of the synthesis growth chamber. In order to facilitate observation of the charging and feeding conditions of the turnover feeder, a second observation window is arranged on the furnace wall of the charging chamber.
Further, in order to facilitate charging, a charging door is provided at the top of the charging chamber.
Furthermore, in order to isolate and seal the charging chamber and the feeding chamber, a sealing ring I is arranged between the inserting plate and the furnace wall. In order to facilitate material receiving and feeding, the feeding pipe comprises a funnel section positioned at the top and a vertical pipe section or an inclined pipe section leading from the feeding chamber into the synthetic growth chamber.
Furthermore, in order to assist in maintaining a low-temperature environment, the inserting plate is provided with an interlayer, and cooling water is filled in the interlayer. In order to cool the indium-phosphorus mixed balls and prevent the feeding pipe from being damaged due to overheating, cooling water is introduced into the pipe wall of the vertical pipe section or the inclined pipe section.
The invention has the beneficial effects that: 1. by adopting the system, the proportioned indium-phosphorus mixed balls can be directly put into a crucible for melting and synthesis, and crystal growth can be carried out in situ after synthesis; the method simplifies the operation flow, reduces the control requirement, has faster synthesis speed and higher preparation efficiency of the crystal, and is beneficial to industrial production. 2. The system for preparing the indium phosphide crystal can reduce the volatilization amount of phosphorus, reduce material pollution, improve the crystal purity, reduce the material cost and facilitate the synthesis and growth of the high-quality indium phosphide crystal with a mixture ratio.
Drawings
FIG. 1 is a schematic diagram of a system for preparing InP crystal from InP mixture according to example I;
FIG. 2 is a schematic diagram of the reaction process of the InP mixture when it is fed into an In-P melt;
FIG. 3 is a schematic view showing a feeding operation of a feeding chamber in the first embodiment;
FIG. 4 is a schematic structural view of a neutral feed tube according to a second embodiment;
FIG. 5 is a schematic structural diagram of an embodiment of an overturning feeder;
FIG. 6 is a schematic view of the connection structure of the motor and the loader in the embodiment;
in the drawing, 1 represents a synthesis growth chamber, 2 represents a seed crystal rod, 3 represents a seed crystal, 4 represents a melt temperature thermocouple, 5 represents a crystal, 6 represents a pressure gauge I, 7 represents a vacuum gauge I, 8 represents a heat-insulating jacket, 9 represents a main heater, 10 represents a crucible, 11 represents a boron oxide covering agent, 12 represents an indium-phosphorus melt, 13 represents a crucible support, 14 represents a lower heater, 15 represents an exhaust port, 16 represents a crucible rod, 17 represents a first observation window, 18 represents a feed pipe, 19 represents a feeding chamber, 20 represents a vacuum gauge II, 21 represents a pressure gauge II, 22 represents an insert plate, 22-1 represents a seal ring I, 23 represents an indium-phosphorus mixed ball, 24 represents a carrier, 25 represents a vacuum gauge III, 26 represents a pressure gauge III, 27 represents a charging chamber, 28 represents a robot arm, 29 represents a charging door, 30 represents a second observation window, and 31 represents an air inlet. 32 represents a turnover driving device, 32-1 represents a protective cover, 32-2 represents a heat insulation layer, 32-3 represents a motor, 32-4 represents a sealing ring II, 32-5 represents a pin, 33 represents a lead wire, and 34 represents a flange.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
In one embodiment, a system for preparing indium phosphide crystals by using an indium phosphide mixture comprises a vacuum system, an air charging and discharging system, a temperature and pressure control system, an electrical control system, a cooling circulation system and a weighing system. These systems are the basic systems commonly used in the art, especially single crystal furnaces for producing indium phosphide crystals based on in situ synthesis, and are the basic configuration and are not described herein. In order to realize the preparation of indium phosphide crystals by using indium-phosphorus mixed balls, the invention improves the furnace body.
Referring to fig. 1, the furnace body is divided into a synthetic growth chamber 1, a feeding chamber 19 and a charging chamber 27, the charging chamber 27 and the feeding chamber 19 are divided up and down by means of an inserting plate 22, a sealing ring I22-1 is arranged between the inserting plate 22 and the furnace wall, and the charging chamber 27 and the feeding chamber 19 can be isolated and sealed when the inserting plate is inserted. The charging chamber 27 is internally provided with a turnover feeder, the charging chamber 19 is internally provided with a feeding pipe 18, one end of the feeding pipe 18 is upwards butted with the turnover feeder, and the other end thereof downwards extends into the synthesis growth chamber 1.
The synthesis growth chamber 1 is internally provided with a lower heater 14, a main heater 9, a heat preservation sleeve 8, a crucible 10, a supporting crucible support 13 and a crucible rod 16. The crucible 10 is positioned on a graphite crucible support 13, and the crucible support 13 is fixedly connected with a crucible rod 16. The lower heater 14 and the main heater 9 are arranged at the periphery of the crucible 10 and the crucible support 13, and a heat insulation sleeve 8 is arranged between the main heater 9 and the inner wall of the synthesis growth chamber 1. The other end of the crucible rod 16 extends out of the furnace bottom of the synthetic growth chamber 1 and is connected with a crucible rod rotating and lifting mechanism. The crucible rod rotating and lifting mechanism is a common basic mechanism of single crystal furnaces and synthesis furnaces in the field and is used for driving a crucible to lift and rotate so as to uniformly mix indium and phosphorus and fully react, and details are not repeated here. A seed crystal rod 2 is arranged above the crucible 10, a seed crystal 3 and a weighing sensor are fixed on the seed crystal rod 2, and the seed crystal rod 2 penetrates out of the top cover of the synthesis growth chamber 1 to be connected with a seed crystal rod lifting mechanism. The seed rod lifting mechanism can drive the seed crystal 3 to lift so as to lift and pull the growing crystal. The load cell and the weighing system can calculate the growth weight of the crystal. The seed rod 2, the weighing sensor, the weighing system and the seed rod lifting mechanism are common basic mechanisms of a single crystal furnace for pulling and growing crystals, and are not described again. The synthesis growth chamber 1 is also provided with a melt temperature measuring thermocouple 4, a pressure gauge I6 and a vacuum gauge I7, the bottom of the synthesis growth chamber is provided with an exhaust port 15, and the top of the synthesis growth chamber is provided with a first observation window 17. A vacuum gauge II 20 and a pressure gauge II 21 are arranged on the furnace wall of the feeding chamber 19. The feed tube 18 comprises a funnel section at the top and an inclined tube section leading from the feed chamber 19 into the synthesis growth chamber 1, which inclined tube section extends above the crucible 10.
The top of the charging chamber is provided with a charging door 29, the furnace wall is provided with an air inlet 31, a vacuum gauge III 25 and a pressure gauge III 26 are arranged on the charging door 29, and a second observation window 30 is arranged on the charging door 29. The inverting feeder in the loading chamber 27 comprises a robotic arm 28, a loader 24 and a loader inverting drive 32. referring to fig. 5 and 6, the robotic arm 28 is positioned at the top of the loading chamber 27 at the upper end, the lower end is connected to the inverting drive 32, and the inverting drive 32 is connected to the loader 24. The loader overturning driving device 32 adopts a motor 32-3 positioned at the bottom end of the mechanical arm 28, and the shaft of the motor 32-3 is connected with the loader 24 through a pin 32-5. The motor 32-3 is externally coated with a heat insulation layer 32-2 and a protective cover 32-1, a flange 34 is coated outside a motor shaft, and a sealing ring II 32-4 is arranged. Wires 33 run through the robotic arm 28 to connect to the electrical control system.
The inflation and deflation system comprises a low-temperature inert gas storage tank, a gas inlet 31 and a gas outlet 15. Inert gas at a temperature below 156 ℃ enters the feeding chamber 19 from the charging chamber 27 and is discharged from the exhaust port 15 through the feeding pipe 18 to the synthetic growth chamber 1. The pressure value in the furnace body is 3.5-5.0 MPa.
In the second embodiment, referring to fig. 4, the difference between the first embodiment and the second embodiment is: in the embodiment, the feeding pipe 18 is a straight pipe, the synthesis growth chamber 1 and the feeding chamber 19 are overlapped in a staggered mode, so that the feeding pipe 18 is led into the crucible 10, and the first observation window 17 is positioned on the side wall of the synthesis growth chamber 1.
The steps of preparing the indium phosphide crystal by applying the system are as follows:
1) the high-purity indium powder and the high-purity phosphorus powder are uniformly mixed according to the mass ratio of 3.7: 1.0-1.5, and pressed into spherical indium-phosphorus mixed balls 23.
2) The indium phosphorus mixed balls 23 mixed with boron oxide powder are placed in a loader 24 in a charging chamber 27, and the bulk boron oxide is placed in the crucible 10.
3) The whole system is vacuumized to 10-10 ℃ through the air inlet 31-5Pa, then the inert gas with the temperature lower than 156 ℃ is filled into the feeding chamber 19 and the feeding chamber 27 through the air inlet 31, and the low-temperature inert gas enters the synthesis and growth chamber 1 through the feeding pipe 18, so that the indium-phosphorus mixed balls 23 are kept at low temperature all the time. The whole synthesis process keeps the gas flow between the gas inlet 31 and the gas outlet 15 and the gas pressure is stable, the pressure value is between 3.5 and 5.0MPa, and the pressure of the feeding chamber 19 is 0.05 to 0.1MPa higher than that of the synthesis growth chamber 1.
4) The crucible 10 is heated by the main heater 9 and the lower heater 14, the crucible 10 rotates to 5-35 r/min, after the massive boron oxide is melted, the crucible 10 is fully paved to form a boron oxide covering agent 11, and the melt temperature thermocouple 4 is inserted into the interface between the boron oxide covering agent 11 and the bottom of the crucible 10.
5) The indium phosphorus mixing balls 23 in the loader 24 are fed into the feeding pipe 18 by the mechanical arm 28, the indium phosphorus mixing balls 23 fall into the crucible 10, and the falling condition of the indium phosphorus mixing balls 23 at the opening of the feeding pipe 18 is observed through the first observation window 17. Referring to fig. 2, for the first or successive first few indium phosphorus mixing balls 23, the indium in the indium phosphorus mixing ball 23 melts and the phosphorus sublimes into phosphorus gas upon heating, which reacts with and is absorbed by the indium melt to form an indium-phosphorus melt 12. The indium in the subsequent indium-phosphorus mixed ball 23 melts and reacts with the indium-phosphorus melt 12 to form a new indium-phosphorus melt 12, the phosphorus in the indium-phosphorus mixed ball 23 is heated and sublimated into phosphorus gas, and the phosphorus gas reacts with and is absorbed by the indium-phosphorus melt 12. After the indium-phosphorus melt 12 is synthesized to cover the bottom of the crucible, the seed crystal 3 is lowered and the boron oxide covering agent 11 is pulled out.
6) The number of the indium phosphorus mixed balls 23 in the loader 24 is observed through the second observation window 30. After the indium-phosphorus mixed balls 23 in the loading device 24 are delivered, referring to fig. 3, the inserting plate 22 is inserted to separate the feeding chamber 19 from the loading chamber 27, and the synthesis and growth continues in the growth chamber 1. Simultaneously discharging high-pressure gas in the loading chamber 27 from the gas inlet 31 to atmospheric pressure, then opening the loading door 29, putting the indium-phosphorus mixed balls 23 into the loading device 24, closing the loading door 29, vacuumizing from the gas inlet 31, filling inert gas at the temperature lower than 156 ℃ until the pressure of the loading chamber 27 is the same as that of the synthesis and growth chamber 1 and the feeding chamber 19, opening the insert 22, sending the indium-phosphorus mixed balls 23 in the loading device 24 into the crucible 10 through the feeding pipe 18 by the mechanical arm 28 for continuous synthesis, and continuously pulling to form the crystal 5.
Claims (10)
1. The utility model provides a system for utilize indium phosphorus mixture preparation indium phosphide crystal, includes vacuum system, fills gassing system, temperature and pressure control system, electric control system, cooling circulation system, weighing system and furnace body, is provided with rotatory elevating system of crucible pole and seed crystal pole elevating system on the furnace body, its characterized in that: the furnace body is divided into a synthetic growth chamber (1), a feeding chamber (19) and a charging chamber (27), the charging chamber (27) and the feeding chamber (19) are separated by means of an inserting plate (22), a turnover feeding device is arranged in the charging chamber (27), a feeding pipe (18) is arranged in the feeding chamber (19), one end of the feeding pipe (18) is upwards butted with the turnover feeding device, and the other end of the feeding pipe downwards extends into a crucible (10) in the synthetic growth chamber (1) to form an indium-phosphorus mixed ball feeding structure; the crucible (10) is positioned on a crucible rod (16), and a seed rod lifting mechanism is arranged on the top cover of the synthesis growth chamber (1).
2. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: the turnover feeder comprises a mechanical arm (28), a material loading device (24) and a material loading device turnover driving device (32), wherein the upper end of the mechanical arm (28) is positioned at the top of the loading chamber (27), the lower end of the mechanical arm is connected with the turnover driving device (32), and the turnover driving device (32) is connected with the material loading device (24).
3. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 2, wherein: the loader overturning driving device (32) is a motor (32-3) positioned at the bottom end of the mechanical arm (28), and the shaft of the motor (32-3) is connected with the loader (24).
4. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 3, wherein: the motor (32-3) is externally coated with a heat insulation layer (32-2) and a protective cover (32-1).
5. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: the inflation and deflation system comprises a low-temperature inert gas storage tank, an air inlet (31) and an air outlet (15) which are respectively arranged at the top of the charging chamber (27) and the bottom of the synthetic growth chamber (1), wherein the air inlet (31) is higher than the inlet of the feeding pipe (18); inert gas at a temperature of below 156 ℃ enters the feeding chamber (19) from the charging chamber (27) and enters the synthesis growth chamber (1) through the feeding pipe (18), is fed to the upper part of the crucible (10) and is discharged from the exhaust port (15).
6. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 5, wherein: the pressure value in the furnace body is 3.5-5.0Mpa, and the pressure of the feeding chamber (19) is 0.05-0.1MPa higher than that of the synthetic growth chamber (1).
7. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: a first observation window (17) is arranged on the furnace wall of the synthetic growth chamber (1), and a second observation window (30) is arranged on the furnace wall of the charging chamber (27).
8. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: the top of the charging chamber is provided with a charging door (29).
9. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: a sealing ring I (22-1) is arranged between the inserting plate (22) and the furnace wall, and the feeding pipe (18) comprises a funnel section positioned at the top and a vertical pipe section or an inclined pipe section which is led into the synthetic growth chamber (1) from the feeding chamber (19).
10. The system for producing indium phosphide crystals using an indium phosphide mixture as set forth in claim 1, wherein: the pipe wall of the vertical pipe section or the inclined pipe section is internally communicated with cooling water, the inserting plate (22) is provided with an interlayer, and the interlayer is internally communicated with the cooling water.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911155614.6A CN110760931B (en) | 2019-11-22 | 2019-11-22 | System for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
| PCT/CN2020/114331 WO2021098347A1 (en) | 2019-11-22 | 2020-09-10 | System for preparing indium phosphide crystal from indium phosphorus mixture |
| JP2021534307A JP7254932B2 (en) | 2019-11-22 | 2020-09-10 | System for manufacturing indium phosphide crystals using indium-phosphorus mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911155614.6A CN110760931B (en) | 2019-11-22 | 2019-11-22 | System for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110760931A true CN110760931A (en) | 2020-02-07 |
| CN110760931B CN110760931B (en) | 2024-03-19 |
Family
ID=69338883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911155614.6A Active CN110760931B (en) | 2019-11-22 | 2019-11-22 | System for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP7254932B2 (en) |
| CN (1) | CN110760931B (en) |
| WO (1) | WO2021098347A1 (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021098347A1 (en) * | 2019-11-22 | 2021-05-27 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal from indium phosphorus mixture |
| WO2021098348A1 (en) * | 2019-11-22 | 2021-05-27 | 中国电子科技集团公司第十三研究所 | Method for preparing indium phosphide crystal using indium-phosphorus mixture |
| CN113174630A (en) * | 2021-04-08 | 2021-07-27 | 中国电子科技集团公司第十三研究所 | Large-size semiconductor single crystal growth system |
| CN113249778A (en) * | 2021-04-08 | 2021-08-13 | 中国电子科技集团公司第十三研究所 | Preparation method of large-size compound semiconductor single crystal |
| CN113308744A (en) * | 2021-06-03 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Preparation device of semi-insulating indium phosphide |
| CN113308739A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | System for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| CN113699584A (en) * | 2021-08-27 | 2021-11-26 | 昆明理工大学 | Czochralski silicon microwave rapid material supplementing continuous production system and production method thereof |
| WO2022166098A1 (en) * | 2021-02-03 | 2022-08-11 | 中国电子科技集团公司第十三研究所 | Growth device and method for low-stress crystal |
| CN115198347A (en) * | 2022-07-15 | 2022-10-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
| CN115522078A (en) * | 2022-10-25 | 2022-12-27 | 西安稀有金属材料研究院有限公司 | Device and method for preparing ultra-high-purity indium by vacuum distillation coupled single crystal pulling |
| CN116145252A (en) * | 2023-02-28 | 2023-05-23 | 昆明理工大学 | Method for synthesizing indium phosphide polycrystal in vacuum |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113512755B (en) * | 2021-07-06 | 2022-10-04 | 中国电子科技集团公司第十三研究所 | Immersion phosphide synthesizing and growing device under magnetic field |
| CN116183004A (en) * | 2023-02-21 | 2023-05-30 | 连城凯克斯科技有限公司 | Real-time measuring device for material weight in crucible of single crystal furnace |
| CN116767884B (en) * | 2023-08-25 | 2023-11-03 | 江苏天利智能科技有限公司 | Conveying equipment for crucible feeding |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02248399A (en) * | 1989-03-22 | 1990-10-04 | Furukawa Electric Co Ltd:The | Method for growing mixed crystal-type compound semiconductor |
| US5290395A (en) * | 1990-07-26 | 1994-03-01 | Sumitomo Electric Industries, Ltd. | Method of and apparatus for preparing single crystal |
| US5431125A (en) * | 1991-06-14 | 1995-07-11 | The United States Of America As Represented By The Secretary Of The Air Force | Twin-free crystal growth of III-V semiconductor material |
| JP2009023867A (en) * | 2007-07-19 | 2009-02-05 | Hitachi Cable Ltd | Manufacturing method of semiconductor crystal and its manufacturing apparatus |
| CN109402722A (en) * | 2018-12-14 | 2019-03-01 | 中国电子科技集团公司第十三研究所 | The trans- injection of one kind synthesizes continuous VGF crystal growing apparatus and method |
| CN209456611U (en) * | 2018-12-14 | 2019-10-01 | 中国电子科技集团公司第十三研究所 | The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device |
| US20190352794A1 (en) * | 2017-12-08 | 2019-11-21 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Device and method for continuous vgf crystal growth through rotation after horizontal injection synthesis |
| CN211112317U (en) * | 2019-11-22 | 2020-07-28 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by indium phosphide mixture |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0640592Y2 (en) * | 1989-06-20 | 1994-10-26 | 住友金属工業株式会社 | Silicon single crystal growth equipment |
| US5342475A (en) * | 1991-06-07 | 1994-08-30 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
| JPH07157390A (en) * | 1993-12-02 | 1995-06-20 | Fujitsu Ltd | Production of single crystal |
| JP4800292B2 (en) | 2007-12-26 | 2011-10-26 | シャープ株式会社 | Melting equipment |
| CN103014837A (en) * | 2012-12-26 | 2013-04-03 | 江苏华盛天龙光电设备股份有限公司 | Secondary charging method for single crystal furnace |
| CN204237887U (en) * | 2014-11-26 | 2015-04-01 | 中国电子科技集团公司第十三研究所 | Situ high pressure synthesizes multi-functional crystal growth system |
| CN108193275B (en) * | 2017-12-14 | 2019-09-10 | 广东先导先进材料股份有限公司 | For synthesizing InP polycrystalline feeding device and synthesis InP polycrystalline method |
| CN109629003B (en) * | 2018-12-29 | 2021-05-28 | 珠海鼎泰芯源晶体有限公司 | Preparation method of low-concentration P-type indium phosphide single crystal |
| CN110760931B (en) * | 2019-11-22 | 2024-03-19 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
-
2019
- 2019-11-22 CN CN201911155614.6A patent/CN110760931B/en active Active
-
2020
- 2020-09-10 WO PCT/CN2020/114331 patent/WO2021098347A1/en active Application Filing
- 2020-09-10 JP JP2021534307A patent/JP7254932B2/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02248399A (en) * | 1989-03-22 | 1990-10-04 | Furukawa Electric Co Ltd:The | Method for growing mixed crystal-type compound semiconductor |
| US5290395A (en) * | 1990-07-26 | 1994-03-01 | Sumitomo Electric Industries, Ltd. | Method of and apparatus for preparing single crystal |
| US5431125A (en) * | 1991-06-14 | 1995-07-11 | The United States Of America As Represented By The Secretary Of The Air Force | Twin-free crystal growth of III-V semiconductor material |
| JP2009023867A (en) * | 2007-07-19 | 2009-02-05 | Hitachi Cable Ltd | Manufacturing method of semiconductor crystal and its manufacturing apparatus |
| US20190352794A1 (en) * | 2017-12-08 | 2019-11-21 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Device and method for continuous vgf crystal growth through rotation after horizontal injection synthesis |
| CN109402722A (en) * | 2018-12-14 | 2019-03-01 | 中国电子科技集团公司第十三研究所 | The trans- injection of one kind synthesizes continuous VGF crystal growing apparatus and method |
| CN209456611U (en) * | 2018-12-14 | 2019-10-01 | 中国电子科技集团公司第十三研究所 | The trans- injection of one kind synthesizes continuous VGF crystal growing crucible and device |
| CN211112317U (en) * | 2019-11-22 | 2020-07-28 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal by indium phosphide mixture |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021098348A1 (en) * | 2019-11-22 | 2021-05-27 | 中国电子科技集团公司第十三研究所 | Method for preparing indium phosphide crystal using indium-phosphorus mixture |
| WO2021098347A1 (en) * | 2019-11-22 | 2021-05-27 | 中国电子科技集团公司第十三研究所 | System for preparing indium phosphide crystal from indium phosphorus mixture |
| US11781240B2 (en) | 2019-11-22 | 2023-10-10 | The 13Th Research Institute Of China Electronics Technology Group Corporation | Method for preparing indium phosphide crystal by utilizing indium-phosphorus mixture |
| WO2022166098A1 (en) * | 2021-02-03 | 2022-08-11 | 中国电子科技集团公司第十三研究所 | Growth device and method for low-stress crystal |
| CN113174630A (en) * | 2021-04-08 | 2021-07-27 | 中国电子科技集团公司第十三研究所 | Large-size semiconductor single crystal growth system |
| CN113249778A (en) * | 2021-04-08 | 2021-08-13 | 中国电子科技集团公司第十三研究所 | Preparation method of large-size compound semiconductor single crystal |
| CN113174630B (en) * | 2021-04-08 | 2022-08-19 | 中国电子科技集团公司第十三研究所 | Large-size semiconductor single crystal growth system |
| CN113249778B (en) * | 2021-04-08 | 2022-05-17 | 中国电子科技集团公司第十三研究所 | Preparation method of large-size compound semiconductor single crystal |
| CN113308739A (en) * | 2021-06-01 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | System for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| CN113308739B (en) * | 2021-06-01 | 2022-08-19 | 中国电子科技集团公司第十三研究所 | System for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis |
| CN113308744A (en) * | 2021-06-03 | 2021-08-27 | 中国电子科技集团公司第十三研究所 | Preparation device of semi-insulating indium phosphide |
| CN113308744B (en) * | 2021-06-03 | 2022-02-15 | 中国电子科技集团公司第十三研究所 | Preparation device of semi-insulating indium phosphide |
| CN113699584B (en) * | 2021-08-27 | 2022-05-06 | 昆明理工大学 | Czochralski silicon microwave rapid material supplementing continuous production system and production method thereof |
| CN113699584A (en) * | 2021-08-27 | 2021-11-26 | 昆明理工大学 | Czochralski silicon microwave rapid material supplementing continuous production system and production method thereof |
| CN115198347A (en) * | 2022-07-15 | 2022-10-18 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystal |
| CN115198347B (en) * | 2022-07-15 | 2024-06-11 | 中国电子科技集团公司第十三研究所 | Device and method for centrifugally synthesizing and growing compound crystals |
| CN115522078A (en) * | 2022-10-25 | 2022-12-27 | 西安稀有金属材料研究院有限公司 | Device and method for preparing ultra-high-purity indium by vacuum distillation coupled single crystal pulling |
| CN115522078B (en) * | 2022-10-25 | 2023-07-04 | 西安稀有金属材料研究院有限公司 | Device and method for vacuum distillation coupling single crystal pulling of ultra-high purity indium |
| CN116145252A (en) * | 2023-02-28 | 2023-05-23 | 昆明理工大学 | Method for synthesizing indium phosphide polycrystal in vacuum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110760931B (en) | 2024-03-19 |
| JP2022530592A (en) | 2022-06-30 |
| JP7254932B2 (en) | 2023-04-10 |
| WO2021098347A1 (en) | 2021-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110760931A (en) | System for preparing indium phosphide crystal by indium phosphide mixture | |
| CN110760932B (en) | Method for preparing indium phosphide crystal by indium phosphide mixture | |
| CN111424310B (en) | Method for synthesizing indium phosphide by liquid phosphorus injection method | |
| CN110257901B (en) | Preparation process of large-diameter efficient N-type monocrystalline silicon | |
| CN211112317U (en) | System for preparing indium phosphide crystal by indium phosphide mixture | |
| KR100876925B1 (en) | CdTe SINGLE CRYSTAL AND CdTe POLYCRYSTAL, AND METHOD FOR PREPARATION THEREOF | |
| US10519563B2 (en) | Device and method for continuous VGF crystal growth through rotation after horizontal injection synthesis | |
| WO2019109366A1 (en) | Method for in-situ injection and synthesis of phosphide by using bearing gas | |
| CN102965734A (en) | Rapid synthesis method of indium phosphide polycrystalline material and multi-tubular quartz phosphorus bubble thereof | |
| CN113638048B (en) | Method for growing indium phosphide single crystal by VGF method | |
| CN113699584B (en) | Czochralski silicon microwave rapid material supplementing continuous production system and production method thereof | |
| CN212895088U (en) | System for synthesizing indium phosphide by liquid phosphorus injection method | |
| US20240209545A1 (en) | Method for preparing compound semiconductor crystal by combining continuous lec and vgf after injection synthesis | |
| JP2012106870A (en) | Method of growing crystal | |
| CN214529324U (en) | Carbon doping device for growing semi-insulating gallium arsenide single crystal | |
| CN212404352U (en) | Gas stirring device and ingot furnace | |
| CN111647947A (en) | Synthesis device and method of gallium antimonide polycrystalline raw material | |
| CN113308739A (en) | System for preparing compound semiconductor crystal by combining continuous LEC and VGF after injection synthesis | |
| JP2517803B2 (en) | Method for synthesizing II-VI compound semiconductor polycrystal | |
| CN215828910U (en) | Connecting component of VGF crucible in inverted suction type compound semiconductor crystal synthesis system | |
| CN113136616B (en) | Carbon doping device and carbon doping method for growing semi-insulating gallium arsenide single crystal | |
| JP2000281500A (en) | Gallium arsenide single crystal, its production and apparatus for producing the same | |
| CN117604611A (en) | Gallium antimonide crystal growth method | |
| CN117071051A (en) | Balanced solidification method for preparing compound crystal by temperature gradient solidification | |
| CN117587496A (en) | Method for growing indium antimonide crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Sun Niefeng Inventor after: Ou Xin Inventor after: Song Ruiliang Inventor after: Liu Huisheng Inventor after: Sun Tongnian Inventor after: Bu Aimin Inventor after: Wang Shujie Inventor after: Shi Yanlei Inventor after: Shao Huimin Inventor after: Fu Lijie Inventor after: Li Xiaolan Inventor after: Wang Yang Inventor after: Xu Senfeng Inventor before: Sun Niefeng Inventor before: Sun Tongnian Inventor before: Wang Shujie Inventor before: Shi Yanlei Inventor before: Shao Huimin Inventor before: Fu Lijie Inventor before: Li Xiaolan Inventor before: Wang Yang Inventor before: Xu Senfeng Inventor before: Liu Huisheng |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |