CN111733448B - Device and method for adjusting shouldering morphology in indium antimonide crystal growth process - Google Patents
Device and method for adjusting shouldering morphology in indium antimonide crystal growth process Download PDFInfo
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- CN111733448B CN111733448B CN202010783261.0A CN202010783261A CN111733448B CN 111733448 B CN111733448 B CN 111733448B CN 202010783261 A CN202010783261 A CN 202010783261A CN 111733448 B CN111733448 B CN 111733448B
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- 239000013078 crystal Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 62
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 46
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000001257 hydrogen Substances 0.000 claims abstract description 33
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 33
- 229910052786 argon Inorganic materials 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 8
- 230000006698 induction Effects 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003491 array Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
-
- 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
-
- 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)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a crystal morphology adjusting method in a shouldering process in a liquid phase crystal pulling growth process, in particular to an adjusting device and an adjusting method for the shouldering morphology in an indium antimonide crystal growth process. Comprises a single crystal furnace device and an external furnace control device, wherein the external furnace control device comprises: the device comprises a hydrogen flowmeter, an argon flowmeter, an upper computer control device, a pressure transmitter, a pressure control instrument, an electric control valve, a mechanical pump, a molecular pump backing valve and a molecular pump. The invention utilizes the accurate control of the dynamic atmosphere flow in the shouldering process, and greatly improves the continuous and stable shouldering process in the indium antimonide single crystal growth process by slowly and linearly increasing the dynamic atmosphere flow, and the shouldering angle of the crystal is smooth and continuous, thereby having better regulation effect on the morphology of the crystal shouldering process and being beneficial to the growth of high-quality indium antimonide single crystals.
Description
Technical Field
The invention relates to a crystal morphology adjusting method in the shouldering process in the liquid phase crystal pulling growth process,
in particular to a device and a method for adjusting shouldering morphology in the growth process of indium antimonide crystals.
Background
Indium antimonide crystals have the maximum electron mobility and the minimum band gap in all known group iii-v compound semiconductors, and the band gap width is 0.228eV at 77K temperature. The infrared light wave which is easy to penetrate through the atmosphere can be absorbed, and the excellent semiconductor performance determines that the infrared light wave can be used for manufacturing high-performance 3-5 um medium wave infrared detectors. The detector scale has been developed from a unit array and a multi-element array to an ultra-large area array focal plane array, the working temperature is increased to 95K, 110K and 130K, and the increase of the working temperature is an important research aspect of the infrared detector in the future. The indium antimonide product is widely applied to military and civil infrared systems such as infrared tracking, guidance, thermal imaging, monitoring, early warning and astronomical observation. The demand of indium antimonide crystals as substrate materials of infrared devices is increasing, and the quality requirements on the indium antimonide crystals are increasing in order to prepare infrared detectors which are large-scale arrays, high in sensitivity and high in temperature. The prepared indium antimonide monocrystal with high quality and low dislocation is beneficial to the rapid development of infrared devices.
The Czochralski method is the main preparation technique for growing large-sized indium antimonide crystals. For the growth process of the indium antimonide single crystal, the property of the material is difficult to control the angle of shoulder angle, the root is that the thermal conductivity of the material is lower and is only 17W/mK, the latent heat of crystallization is difficult to escape in the growth process, and local stress is easy to form in the crystal, so that dislocation is generated. For the growth of the indium antimonide crystal with lower heat conductivity, the difficulty of shoulder adjustment of the growth of the indium antimonide crystal is increased. There are two cases where the first crystal rapidly spreads out and the crystal diameter increases rapidly with time nonlinearity, and polycrystal and twin crystal are easily generated. The second crystal is difficult to shoulder, so that the pre-shoulder stage is too long, the crystal growth is not facilitated, and raw materials are wasted. The shoulder angle is adjusted by adopting circulating water cooling, but the circulating water quantity is difficult to control and difficult to achieve the expected situation. In an ideal state, after the material melting is completed, the seeding temperature is regulated, the seed crystal is welded with the melt, and the neck is shouldered after dislocation in the original seed crystal is eliminated. The shoulder time is long in the growth process of the indium antimonide monocrystal by the liquid phase method, the monocrystal material with low self heat conductivity is not easy to maintain, and the continuous and smooth shoulder angle of the crystal is not easy to maintain.
Disclosure of Invention
In order to overcome the defects of the indium antimonide material, grow better towards ideal conditions, reduce crystal defects and improve the quality of indium antimonide crystals, the invention utilizes a method for accurately and dynamically adjusting the air inlet flow to ensure that the shouldering process of the indium antimonide crystals is continuous and stable, and the shouldering angle is smooth and continuous.
The technical scheme of the invention is that the shoulder-placing morphology adjusting device in the indium antimonide crystal growth process comprises a single crystal furnace device and an external furnace control device, and is characterized in that: the external control device comprises: the device comprises a hydrogen flowmeter, an argon flowmeter, an upper computer control device, a pressure transmitter, a pressure control instrument, an electric control valve, a mechanical pump, a molecular pump backing valve and a molecular pump; the hydrogen flowmeter and the argon flowmeter are arranged on an air pipe of an air inlet hole of the single crystal furnace device; the electric control valve is connected with the air outlet hole through an air pipe, the mechanical pump is connected with the electric control valve through an air pipe, the molecular pump is arranged on the outer side of the bottom of the furnace body, and the molecular pump is connected with the mechanical pump through an air pipe for a molecular pump backing valve; the output end of the pressure transmitter is connected with the pressure control instrument, the argon flow meter, the pressure control instrument, the seed crystal rotating motor, the seed crystal lifting motor, the crucible rotating motor and the crucible lifting motor; the pressure control instrument is connected with the pressure transmitter through a lead; the electric control valve is connected with the pressure control instrument through a wire.
A method for adjusting shoulder-relief morphology in the growth process of indium antimonide crystals is characterized by comprising the following steps: the adjusting method comprises the following steps:
1. firstly, loading an indium antimonide polycrystalline raw material into a quartz crucible, and placing the crucible into a crucible supporting seat;
2. firstly, an argon flow meter is connected with an argon bottle, and a hydrogen flow meter is connected with a hydrogen bottle; starting a mechanical pump, setting the target pressure of a pressure control instrument to be 0mbar in an upper computer control device, setting the minimum opening of an electric control valve to be 95%, setting the maximum opening of the electric control valve to be 100%, and performing low vacuum air extraction operation on the system by using an air channel of an air outlet hole, the mechanical pump and the electric control valve; to reduce the vacuum of the system to 3X 10 -1 Pa, setting the minimum opening degree of the electric control valve to be 0%, and setting the maximum opening degree of the electric control valve to be 0%, namely closing the gas path of the electric control valve, then opening the forevalve of the molecular pump, simultaneously starting the molecular pump to start high-vacuum pumping operation, and reducing the system vacuum to 1X 10 -3 Closing the molecular pump and a molecular pump backing valve during Pa, and finally closing the mechanical pump;
3. setting the flow rate of a hydrogen flowmeter to be 1000ml/min and the flow rate of an argon flowmeter to be 9000ml/min in an upper computer control device, enabling hydrogen and argon to enter a furnace body (1-3) through an air inlet hole, and setting the flow rates of the flowmeter and the argon flowmeter to be 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
4. the method comprises the steps of starting a power supply, heating a system by generating eddy current by an induction heating body, heating by using alternating current in an induction coil to enable the induction heating body to generate eddy current, heating a crucible and raw materials in a heat preservation system, and setting the rotating speed of a crucible rotating motor to be 10rpm after the raw materials are completely melted, wherein the rotating speed is anticlockwise; the rotation speed of the seed crystal rotating motor is 15rpm, the direction is clockwise, and the seed crystal (1-8) is slowly lowered to a position 1cm above the liquid level of the melt;
5. setting the target pressure of a pressure control instrument to 1080mbar in an upper computer control device, setting the flow rate of a hydrogen flowmeter to 20ml/min, timely taking away heat emitted by a new crystal in a dynamic hydrogen flowing through an area above the crystal under the guidance of a guide cover, setting the minimum opening of an electric control valve to 5%, the maximum opening to 15%, and finally starting a mechanical pump to wait for 30 minutes, wherein the air inlet and the air exhaust of the system reach dynamic balance, the pressure of the system is stabilized at 1080mbar, and the up-down fluctuation is controlled at +/-0.5 mbar;
6. after the lower end surface of the seed crystal is fused with the melt, the seed crystal lifting motor is controlled by the upper computer control device to move up and down on the seed crystal lifting screw rod, the seed crystal rod is enabled to move up and down through the seed crystal lifting synchronization device, and the seed crystal is pulled up; the crucible lifting motor is controlled by the upper computer control device to move up and down on the crucible rod lifting screw rod, and the crucible rod moves up and down through the crucible lifting synchronization device; setting a seed crystal lifting motor in an upper computer control device, wherein the pulling speed of a seed crystal rod is 10mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 0.1mm/h; when the crystal diameter is 20mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 0.3mm/h; when the crystal diameter is 30mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 0.6mm/h; when the crystal diameter is 40mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 1mm/h; when the diameter of the crystal is 50mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 1.5mm/h; when the crystal diameter is 60mm, setting a crucible lifting motor, wherein the lifting speed of a crucible rod is 2mm/h, ending the shouldering process, and continuing the whole process for 8 hours;
7. in the whole shouldering process, when the diameter of the crystal grows to 10mm, setting the flow of the hydrogen flowmeter in the upper computer control device to execute a linear-increasing dynamic process, namely, linearly increasing the flow from the initial 20ml/min to 100ml/min over 480 minutes, and keeping the flow of the hydrogen flowmeter at 100ml/min when the shouldering process is finished.
The invention has the beneficial effects that as the invention utilizes the accurate control of the dynamic atmosphere flow in the shouldering process, and increases the dynamic atmosphere flow slowly and linearly, the shouldering process in the indium antimonide single crystal growth process is continuously and stably improved, the shouldering angle of the crystal is smooth and continuous, the shape of the crystal shouldering process is better regulated, and the invention is beneficial to the growth of high-quality indium antimonide single crystal.
Drawings
FIG. 1 is a schematic view of the structure of the furnace in the present invention and a layout of the control system outside the furnace.
Detailed Description
As shown in fig. 1, an apparatus for adjusting shoulder morphology in an indium antimonide crystal growth process comprises a single crystal furnace apparatus 1 and an external furnace control apparatus 2, wherein the external furnace control apparatus 2 comprises: the device comprises a hydrogen flowmeter 2-1, an argon flowmeter 2-2, an upper computer control device 2-3, a pressure transmitter 2-4, a pressure control instrument 2-5, an electric control valve 2-6, a mechanical pump 2-7, a molecular pump backing valve 2-8 and a molecular pump 2-9; the hydrogen flowmeter 2-1 and the argon flowmeter 2-2 are arranged on an air pipe of an air inlet hole 1-2 of the single crystal furnace device 1; the electric control valve 2-6 is connected with the air outlet hole 1-12 through an air pipe, the mechanical pump 2-7 is connected with the electric control valve 2-6 through an air pipe, the molecular pump 2-9 is arranged at the outer side of the bottom of the furnace body 1-3, and the molecular pump 2-9 is connected with the mechanical pump 2-7 through a molecular pump backing valve 2-8 through an air pipe; the output end of the pressure transmitter 2-4 is connected with the signal input end of the pressure control instrument 2-5; the upper computer control device 2-3 is respectively connected with the hydrogen flowmeter 2-1, the argon flowmeter 2-2, the pressure control instrument 2-5, the seed crystal rotating motor 1-13, the seed crystal lifting motor 1-15, the crucible rotating motor 1-14 and the crucible lifting motor 1-16 through communication cables; the pressure control instrument 2-5 is connected with the pressure transmitter 2-4 through a lead; the electric control valve 2-6 is connected with the pressure control instrument 2-5 through a lead.
The method for adjusting the shoulder-relief morphology in the growth process of the indium antimonide crystal comprises the following steps:
1. firstly, loading an indium antimonide polycrystalline raw material into a quartz crucible 1-5, and placing the crucible 1-5 into a crucible supporting seat 1-9;
2. firstly, an argon flow meter 2-2 is connected with an argon bottle, and a hydrogen flow meter 2-1 is connected with a hydrogen bottle; starting a mechanical pump 2-7, setting the target pressure of a pressure control instrument 2-5 to be 0mbar in an upper computer control device 2-3, setting the minimum opening of an electric control valve 2-6 to be 95%, setting the maximum opening to be 100%, and performing low vacuum air extraction operation on the system by using one air path of an air outlet hole 1-12, the mechanical pump 2-7 and the electric control valve 2-6; to reduce the vacuum of the system to 3X 10 -1 Pa, setting the minimum opening degree of the electric control valve 2-6 to be 0%, and setting the maximum opening degree to be 0%, namely closing the air path of the electric control valve 2-6, then opening the molecular pump backing valve 2-8, simultaneously starting the molecular pump 2-9 to start high vacuum pumping operation, and reducing the system vacuum to 1X 10 -3 Closing the molecular pump 2-9 and the molecular pump backing valve 2-8 during Pa, and finally closing the mechanical pump 2-7;
3. setting the flow rate of a hydrogen flowmeter 2-1 in an upper computer control device 2-3 to be 1000ml/min, setting the flow rate of an argon flowmeter 2-2 to be 9000ml/min, enabling hydrogen and argon to enter a furnace body 1-3 through an air inlet hole 1-2, and setting the flow rates of the flowmeter 2-1 and the flowmeter 2-2 to be 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
4. turning on a power supply, enabling the induction heating body 1-6 to generate eddy current by alternating current in the induction coil 1-10 to generate heat, further heating a crucible and raw materials in the heat preservation system 1-7, and setting the rotating speed of the crucible rotating motor 1-14 to be 10rpm after the raw materials are completely melted, wherein the rotating speed is anticlockwise; the rotation speed of the seed crystal rotating motor 1-13 is 15rpm, the direction is clockwise, and the seed crystal 1-8 is slowly lowered to the position 1cm above the liquid level of the melt;
5. setting a target pressure of a pressure control instrument 2-5 to 1080mbar in an upper computer control device 2-3, setting a flow rate of a hydrogen flowmeter 2-1 to 20ml/min, timely taking away heat emitted by a new crystal in a dynamic hydrogen flowing through an area above the crystal under the guidance of a guide cover 1-4, setting a minimum opening of an electric control valve 2-6 to 5%, a maximum opening of the electric control valve to 15%, and finally starting a mechanical pump 2-7 for 30 minutes, wherein the air inlet and the air exhaust of the system reach dynamic balance, the pressure of the system is stabilized at 1080mbar, and the fluctuation is controlled to be +/-0.5 mbar;
6. seeding the surface of a melt contacted with a seed crystal 1-8, controlling a seed crystal lifting motor 1-15 to move up and down on a seed crystal lifting screw rod 1-19 through an upper computer control device 2-3 after the lower end surface of the seed crystal is fused with the melt, and enabling a seed crystal rod 1-1 to move up and down through a seed crystal lifting synchronization device 1-17 to start lifting operation on the seed crystal 1-8; the crucible lifting motor 1-16 is controlled by the upper computer control device 2-3 to move up and down on the crucible rod lifting screw rod 1-20, and the crucible rod 1-11 is made to move up and down by the crucible lifting synchronization device 1-18; setting a seed crystal lifting motor 1-15 in an upper computer control device 2-3, wherein the pulling speed of a seed crystal rod 1-1 is 10mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor 1-16, wherein the lifting speed of a crucible rod 1-11 is 0.1mm/h; when the crystal diameter is 20mm, setting a crucible lifting motor 1-15, and setting the lifting speed of a crucible rod 1-11 to be 0.3mm/h; when the crystal diameter is 30mm, setting a crucible lifting motor 1-16, and setting the lifting speed of a crucible rod 1-11 to be 0.6mm/h; when the crystal diameter is 40mm, setting a crucible lifting motor 1-16, and setting the lifting speed of a crucible rod 1-11 to be 1mm/h; when the crystal diameter is 50mm, setting a crucible lifting motor 1-16, and setting the lifting speed of a crucible rod 1-11 to be 1.5mm/h; when the crystal diameter is 60mm, setting a crucible lifting motor 1-16, wherein the lifting speed of a crucible rod 1-11 is 2mm/h, ending the shouldering process, and continuing the whole process for 8 hours;
7. in the whole shouldering process, when the crystal diameter grows to 10mm, setting the flow of the hydrogen flowmeter 2-1 in the upper computer control device 2-3 to execute a linear increase dynamic process, namely, the flow is linearly increased to 100ml/min from the initial 20ml/min for 480 minutes, and when the shouldering process is finished, the flow of the hydrogen flowmeter 2-1 is kept at 100ml/min.
After the crystal shouldering process is completed, the morphology of the crystal from the seed crystal position to the shouldering end position is as follows: the shape of the crystal is cone, the total height is 80mm, and the diameter of the bottom of the crystal is about 60 mm. The traditional method for adopting the water cooling of the seed rod has two defects, namely that the control precision of the circulating water flow of the seed rod is relatively accurate without a gas flowmeter, and the water cooling effect of the seed rod is gradually weakened along with the increase of the crystal length along with the continuous shouldering process, so that the phenomenon of concave-convex fluctuation of the appearance of the crystal is caused. The invention utilizes the accurate control of the dynamic atmosphere flow in the shouldering process, and the heat dissipation of the system is relatively balanced by slowly and linearly increasing the dynamic atmosphere flow, so that the conical side surface of the crystal is in a continuous smooth state, and the control effect is good.
Claims (1)
1. A method for adjusting shoulder-relief morphology in the growth process of indium antimonide crystals is characterized by comprising the following steps: the adjusting method comprises the following steps:
1. firstly, loading an indium antimonide polycrystalline raw material into a crucible (1-5), and placing the quartz crucible (1-5) in a crucible supporting seat (1-9);
2. firstly, an argon flow meter (2-2) is connected with an argon bottle, and a hydrogen flow meter (2-1) is connected with a hydrogen bottle; starting a mechanical pump (2-7), setting the target pressure of a pressure control instrument (2-5) to be 0mbar in an upper computer control device (2-3), setting the minimum opening of an electric control valve (2-6) to be 95%, and setting the maximum opening to be 100%, and performing low vacuum air extraction operation on the system by using an air channel of an air outlet hole (1-12), the mechanical pump (2-7) and the electric control valve (2-6); to reduce the vacuum of the system to 3X 10 -1 Pa, setting the minimum opening degree of the electric control valve (2-6) to be 0%, and setting the maximum opening degree to be 0%, namely closing the air path of the electric control valve (2-6), then opening the molecular pump backing valve (2-8), simultaneously starting the molecular pump (2-9) to start high-vacuum pumping operation, and reducing the system vacuum to 1X 10 -3 When Pa, closing the molecular pump (2-9) and the molecular pump backing valve (2-8), and finally closing the mechanical pump (2-7);
3. setting the flow rate of a hydrogen flowmeter (2-1) to 1000ml/min in an upper computer control device (2-3), setting the flow rate of an argon flowmeter (2-2) to 9000ml/min, enabling hydrogen and argon to enter a furnace body (1-3) through an air inlet hole (1-2), and setting the flow rates of the flowmeter (2-1) and the flowmeter (2-2) to 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
4. turning on a power supply, enabling an alternating current in an induction coil (1-10) to enable an induction heating body (1-6) to generate vortex so as to generate heat, further heating a crucible and raw materials in a heat preservation system (1-7), and setting the rotating speed of a crucible rotating motor (1-14) to be 10rpm after the raw materials are completely melted, wherein the rotating speed is anticlockwise; the rotating speed of the seed crystal rotating motor (1-13) is 15rpm, the direction is clockwise, and the seed crystal (1-8) is slowly lowered to a position 1cm above the liquid level of the melt;
5. setting a target pressure of a pressure control instrument (2-5) to 1080mbar in an upper computer control device (2-3), setting the flow rate of a hydrogen flowmeter (2-1) to 20ml/min, enabling dynamic hydrogen to flow through a region above a crystal under the guidance of a guide cover (1-4), setting the minimum opening of an electric control valve (2-6) to 5%, setting the maximum opening of the electric control valve to 15%, finally starting a mechanical pump (2-7), waiting for 30 minutes, enabling the air inlet and the air exhaust of the system to reach dynamic balance, stabilizing the pressure of the system to 1080mbar, and controlling the fluctuation of the system to +/-0.5 mbar;
6. after the lower end surface of the seed crystal is fused with the melt, an upper computer control device (2-3) controls a seed crystal lifting motor (1-15) to move up and down on a seed crystal lifting screw rod (1-19), and a seed crystal lifting synchronization device (1-17) enables the seed crystal rod (1-1) to move up and down, so that the seed crystal (1-8) starts to be lifted; the crucible lifting motor (1-16) is controlled by the upper computer control device (2-3) to move up and down on the crucible rod lifting screw rod (1-20), and the crucible rod (1-11) is enabled to move up and down by the crucible lifting synchronization device (1-18); setting a seed crystal lifting motor (1-15) in an upper computer control device (2-3), wherein the pulling speed of a seed crystal rod (1-1) is 10mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 0.1mm/h; when the crystal diameter is 20mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 0.3mm/h; when the crystal diameter is 30mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 0.6mm/h; when the crystal diameter is 40mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 1mm/h; when the crystal diameter is 50mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 1.5mm/h; when the crystal diameter is 60mm, setting a crucible lifting motor (1-16), wherein the lifting speed of a crucible rod (1-11) is 2mm/h, ending the shouldering process, and continuing the whole process for 8 hours;
7. in the whole shouldering process, when the diameter of the crystal grows to 10mm, setting the flow of the hydrogen flowmeter (2-1) in the upper computer control device (2-3) to execute a linear increase dynamic process, namely, linearly increasing the flow from the initial 20ml/min to 100ml/min after 480 minutes, and keeping the flow of the hydrogen flowmeter (2-1) at 100ml/min when the shouldering process is finished;
the device used by the shouldering morphology adjusting method in the indium antimonide crystal growth process comprises a single crystal furnace device (1) and an external furnace control device (2), and is characterized in that: the external control device (2) comprises: the device comprises a hydrogen flowmeter (2-1), an argon flowmeter (2-2), an upper computer control device (2-3), a pressure transmitter (2-4), a pressure control instrument (2-5), an electric control valve (2-6), a mechanical pump (2-7), a molecular pump backing valve (2-8) and a molecular pump (2-9); the hydrogen flowmeter (2-1) and the argon flowmeter (2-2) are arranged on an air pipe of an air inlet hole (1-2) of the single crystal furnace device (1); the electric control valve (2-6) is connected with the air outlet hole (1-12) through an air pipe, the mechanical pump (2-7) is connected with the electric control valve (2-6) through an air pipe, the molecular pump (2-9) is arranged at the outer side of the bottom of the furnace body (1-3), and the molecular pump (2-9) is connected with the mechanical pump (2-7) through an air pipe through a molecular pump backing valve (2-8); the output end of the pressure transmitter (2-4) is connected with the signal input end of the pressure control instrument (2-5); the upper computer control device (2-3) is respectively connected with the hydrogen flowmeter (2-1), the argon flowmeter (2-2), the pressure control instrument (2-5), the seed crystal rotating motor (1-13), the seed crystal lifting motor (1-15), the crucible rotating motor (1-14) and the crucible lifting motor (1-16) through communication cables; the pressure control instrument (2-5) is connected with the pressure transmitter (2-4) through a lead; the electric control valve (2-6) is connected with the pressure control instrument (2-5) through a lead.
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| US3206286A (en) * | 1959-07-23 | 1965-09-14 | Westinghouse Electric Corp | Apparatus for growing crystals |
| CN102732944A (en) * | 2011-04-02 | 2012-10-17 | 江苏同人电子有限公司 | Crystal growth technology and crystal growth furnace |
| CN109280978A (en) * | 2018-11-29 | 2019-01-29 | 云南北方昆物光电科技发展有限公司 | A kind of preparation method of low dislocation indium antimonide<111>direction monocrystalline |
| CN110552060A (en) * | 2019-09-11 | 2019-12-10 | 中国电子科技集团公司第十一研究所 | InSb crystal growth solid-liquid interface control method and device |
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|---|---|---|---|---|
| US3206286A (en) * | 1959-07-23 | 1965-09-14 | Westinghouse Electric Corp | Apparatus for growing crystals |
| CN102732944A (en) * | 2011-04-02 | 2012-10-17 | 江苏同人电子有限公司 | Crystal growth technology and crystal growth furnace |
| CN109280978A (en) * | 2018-11-29 | 2019-01-29 | 云南北方昆物光电科技发展有限公司 | A kind of preparation method of low dislocation indium antimonide<111>direction monocrystalline |
| CN110552060A (en) * | 2019-09-11 | 2019-12-10 | 中国电子科技集团公司第十一研究所 | InSb crystal growth solid-liquid interface control method and device |
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