CN111733448A - 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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- CN111733448A CN111733448A CN202010783261.0A CN202010783261A CN111733448A CN 111733448 A CN111733448 A CN 111733448A CN 202010783261 A CN202010783261 A CN 202010783261A CN 111733448 A CN111733448 A CN 111733448A
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- 239000013078 crystal Substances 0.000 title claims abstract description 126
- 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 44
- 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 27
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- 229910052786 argon Inorganic materials 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims description 19
- 239000000155 melt Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000010899 nucleation Methods 0.000 claims description 3
- 238000004321 preservation 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
- 230000001360 synchronised effect Effects 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 5
- 238000003491 array Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 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
- 238000010586 diagram Methods 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
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
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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
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 a shouldering morphology adjusting device and method in an indium antimonide crystal growth process. The device 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 front-stage valve and a molecular pump. The invention greatly improves the continuous and stable shouldering process in the growth process of the indium antimonide single crystal, ensures the smooth and continuous shouldering angle of the crystal, has better regulation effect on the appearance of the crystal shouldering process and is beneficial to the growth of the high-quality indium antimonide single crystal by utilizing the accurate control of the dynamic atmosphere flow in the shouldering process and slowly and linearly increasing the dynamic atmosphere flow.
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 the shouldering appearance in the growth process of an indium antimonide crystal.
Background
The indium antimonide crystal has the maximum electron mobility and the minimum band gap in all known group III-V compound semiconductors, and the forbidden band width is 0.228eV at the temperature of 77K. The infrared light wave which easily penetrates through the atmosphere can be absorbed, and the excellent semiconductor performance determines that the semiconductor can be used for manufacturing a high-performance 3-5 um medium wave infrared detector. The detector scale is developed from unit and multi-element linear arrays to super large area array focal plane arrays, 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, astronomical observation and the like. Indium antimonide crystals are increasingly demanded as substrate materials of infrared devices, and the quality requirements of indium antimonide crystals are increasingly high in order to prepare large-scale arrays, high-sensitivity and high-temperature working infrared detectors. The indium antimonide single crystal with high quality and low dislocation is prepared, which is beneficial to the rapid development of infrared devices.
The Czochralski method is the main preparation technique for growing large-size indium antimonide crystals. As for the growth process of the indium antimonide single crystal, because the attribute of the material is difficult to control the shouldering angle, the root is that the self thermal conductivity is low and is only 17W/mK, the latent heat of crystallization is difficult to escape in the growth process, and local stress is very easy to form in the crystal to generate dislocation. For the growth of indium antimonide crystal with lower thermal conductivity, the shoulder-setting adjustment difficulty of the growth of indium antimonide crystal is increased. There are two cases where the first crystal rapidly shoulders and the crystal diameter rapidly increases nonlinearly with time, easily producing polycrystals and twins. The second crystal is difficult to shoulder, so that the shouldering-in-advance stage is too long, the crystal growth is not facilitated, and raw materials are wasted. Some adopt circulating water cooling to adjust and put the angle of shouldering, but the difficult arrival expectation situation of controlling of endless water yield. In an ideal state, after the material melting is finished, the seeding temperature is adjusted, the lower seed crystal is welded with the melt, and the neck is shouldered after dislocation in the original seed crystal is eliminated. The liquid phase method is used for growing the indium antimonide single crystal, the shouldering time is long in the growing process, the self thermal conductivity of the single crystal material is low, and the continuous smoothness of the shouldering angle of the single crystal is not easy to maintain.
The invention content is as follows:
in order to overcome the defects of the indium antimonide material, better grow towards an ideal state, reduce the crystal defects and improve the quality of the indium antimonide crystal, the invention utilizes a method of accurately and dynamically adjusting the air inlet flow to ensure that the shouldering process of the indium antimonide crystal is continuous and stable and the shouldering angle is smooth and continuous.
The technical scheme of the invention is that the device for adjusting the shouldering appearance 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 furnace external control device includes: 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 front-stage valve and a molecular pump; the hydrogen flowmeter and the argon flowmeter are arranged on a gas pipe of a gas inlet of the single crystal furnace device; the electric control valve is connected with the air outlet 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 backing valve of the molecular pump; the output end of the pressure transmitter is connected with the pressure control instrument, the argon gas flowmeter, 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 lead.
A method for adjusting shouldering morphology in an indium antimonide crystal growth process is characterized by comprising the following steps: the adjusting method comprises the following steps:
firstly, loading an indium antimonide polycrystalline raw material into a quartz crucible, and placing the crucible in a crucible supporting seat;
firstly, connecting an argon gas flowmeter with an argon gas cylinder, and connecting a hydrogen gas flowmeter with a hydrogen gas cylinder; starting the mechanical pump, setting the target pressure of the pressure control instrument to be 0mbar in the upper computer control device, setting the minimum opening of the electric control valve to be 95 percent and setting the maximum opening of the electric control valve to be 100 percent, and utilizing the air outlet, the mechanical pump and the electric control valveThe air path performs low vacuum pumping operation on the system until the vacuum of the system is reduced to 3 × 10-1Pa, setting the minimum opening of the electric control valve to be 0% and the maximum opening to be 0%, namely closing the gas path of the electric control valve, then opening the front valve of the molecular pump, starting the molecular pump to start high vacuum pumping operation, and waiting until the vacuum of the system is reduced to 1 × 10-3When Pa, closing the molecular pump and the molecular pump front-stage valve, and finally closing the mechanical pump;
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, feeding hydrogen and argon into a furnace body (1-3) through an air inlet, and setting the flow rates of the flowmeters to be 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
fourthly, a power supply is turned on, the induction heating body generates eddy current to heat the system, alternating current in the induction coil enables the induction heating body to generate eddy current to heat, and then the crucible and the raw materials in the heat preservation system are heated, after the raw materials are completely melted, the rotating speed of a crucible rotating motor is set to be 10rpm, and the direction 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 descended to a position 1cm above the liquid level of the melt;
setting the target pressure of a pressure control instrument to be 1080mbar in an upper computer control device, setting the flow of a hydrogen flowmeter to be 20ml/min, leading dynamic hydrogen to flow through the area above the crystal under the guidance of a guide cover to take away heat dissipated inside the newly generated crystal in time, setting the minimum opening of an electric control valve to be 5% and the maximum opening of the electric control valve to be 15%, finally starting a mechanical pump, waiting for 30 minutes, leading air inlet and air exhaust of a system to reach dynamic balance, stabilizing the system pressure to be 1080mbar, and controlling the vertical fluctuation to be +/-0.5 mbar;
sixthly, seed crystals are seeded by contacting the surfaces of the melts, after the lower end surfaces of the seed crystals and the melts are fused, the upper computer control device controls the seed crystal lifting motor to move up and down on the seed crystal lifting lead screw, the seed crystal lifting synchronization device enables the seed crystal rod to move up and down, and the seed crystals are lifted; 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 is moved up and down by the crucible lifting synchronization device; setting a seed crystal lifting motor in the upper computer control device, wherein the pulling speed of a seed crystal rod is 10 mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 0.1 mm/h; when the diameter of the crystal is 20mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 0.3 mm/h; when the diameter of the crystal is 30mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 0.6 mm/h; when the diameter of the crystal is 40mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 1 mm/h; when the diameter of the crystal is 50mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 1.5 mm/h; when the diameter of the crystal is 60mm, setting a crucible lifting motor, wherein the lifting rate of a crucible rod is 2mm/h, ending the shouldering process, and continuing the whole process for 8 hours;
and seventhly, 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, the flow is linearly increased to 100ml/min from the initial 20ml/min after 480 minutes, and when the shouldering process is finished, the flow of the hydrogen flowmeter is kept at 100 ml/min.
The method has the advantages that the method greatly improves the continuous and stable shouldering process in the indium antimonide single crystal growth process, ensures smooth and continuous shouldering angles of the crystal, has a good adjusting effect on the appearance of the crystal shouldering process and is beneficial to the growth of high-quality indium antimonide single crystals because the method utilizes the accurate control of the dynamic atmosphere flow in the shouldering process and slowly and linearly increases the dynamic atmosphere flow.
Drawings
FIG. 1 is a schematic diagram of the structure inside the furnace and the layout of the control system outside the furnace according to the present invention.
Detailed Description
As shown in fig. 1, the device for adjusting shouldering morphology during indium antimonide crystal growth comprises a single crystal furnace device 1 and an external furnace control device 2, wherein the external furnace control device 2 comprises: 2-1 parts of a hydrogen flowmeter, 2-2 parts of an argon flowmeter, 2-3 parts of an upper computer control device, 2-4 parts of a pressure transmitter, 2-5 parts of a pressure control instrument, 2-6 parts of an electric control valve, 2-7 parts of a mechanical pump, 2-8 parts of a molecular pump front-stage valve and 2-9 parts of a molecular pump; the hydrogen flowmeter 2-1 and the argon flowmeter 2-2 are arranged on a gas pipe of a gas inlet 1-2 of the single crystal furnace device 1; the electric control valve 2-6 is connected with the air outlet 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 front-stage 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 a hydrogen flowmeter 2-1, an argon flowmeter 2-2, a pressure control instrument 2-5, a seed crystal rotating motor 1-13, a seed crystal lifting motor 1-15, a crucible rotating motor 1-14 and a 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.
A method for adjusting shouldering appearance in an indium antimonide crystal growth process comprises the following steps:
firstly, loading an indium antimonide polycrystalline raw material into a quartz crucible 1-5, and placing the crucible 1-5 in a crucible supporting seat 1-9;
secondly, firstly connecting an argon gas flowmeter 2-2 with an argon gas bottle, connecting a hydrogen gas flowmeter 2-1 with a hydrogen gas 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 percent and the maximum opening to be 100 percent, performing low vacuum pumping operation on the system by utilizing a gas path of a gas outlet 1-12, the mechanical pump 2-7 and the electric control valve 2-6, and when the vacuum of the system is reduced to 3 × 10-1Pa, setting the minimum opening of the electric control valves 2-6 to be 0% and the maximum opening to be 0%, namely closing the gas path of the electric control valves 2-6, then opening the front valves 2-8 of the molecular pumps, starting the molecular pumps 2-9 to start high vacuum pumping operation, and when the vacuum of the system is reduced to 1 × 10-3When Pa is needed, closing the molecular pump 2-9 and the molecular pump front-stage valve 2-8, and finally closing the mechanical pump 2-7;
setting the flow rate of a hydrogen flowmeter 2-1 to be 1000ml/min and the flow rate of an argon flowmeter 2-2 to be 9000ml/min in an upper computer control device 2-3, feeding hydrogen and argon into a furnace body 1-3 through an air inlet 1-2, and setting the flow rates of the flowmeters 2-1 and 2-2 to be 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
fourthly, the power supply is turned on, alternating current in the induction coils 1 to 10 enables the induction heating bodies 1 to 6 to generate eddy currents to generate heat, then crucibles and raw materials in the heat preservation systems 1 to 7 are heated, after the raw materials are completely melted, the rotating speed of crucible rotating motors 1 to 14 is set to be 10rpm, and the direction 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 descended to the position 1cm above the melt liquid level;
setting the target pressure of a pressure control instrument 2-5 to be 1080mbar in an upper computer control device 2-3, setting the flow of a hydrogen flowmeter 2-1 to be 20ml/min, enabling dynamic hydrogen to flow through the area above the crystal under the guidance of an air guide sleeve 1-4 to take away heat dissipated inside the newly generated crystal in time, setting the minimum opening of an electric control valve 2-6 to be 5% and the maximum opening to be 15%, finally starting a mechanical pump 2-7, waiting for 30 minutes, enabling air intake and air exhaust of the system to be dynamically balanced, enabling the pressure of the system to be stable at 1080mbar, and controlling the fluctuation at +/-0.5 mbar up and down;
sixthly, seed crystals 1-8 are in contact with the surface of the melt for seeding, after the lower end face of the seed crystals is fused with the melt, the upper computer control device 2-3 controls the seed crystal lifting motor 1-15 to move up and down on the seed crystal lifting lead screw 1-19, the seed crystal lifting synchronizer 1-17 enables the seed crystal rod 1-1 to move up and down, and the seed crystals 1-8 are lifted and pulled; the crucible lifting motors 1-16 are controlled by the upper computer control device 2-3 to move up and down on the crucible rod lifting lead screws 1-20, and the crucible rods 1-11 are driven to move up and down by the crucible lifting synchronous devices 1-18; setting seed crystal lifting motors 1-15 in an upper computer control device 2-3, wherein the pulling speed of seed crystal rods 1-1 is 10 mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor 1-16, and setting the lifting speed of a crucible rod 1-11 to be 0.1 mm/h; when the diameter of the crystal is 20mm, setting a crucible lifting motor 1-15 and the lifting speed of a crucible rod 1-11 to be 0.3 mm/h; when the diameter of the crystal is 30mm, setting a crucible lifting motor 1-16 and the lifting speed of a crucible rod 1-11 to be 0.6 mm/h; when the diameter of the crystal is 40mm, setting a crucible lifting motor 1-16, and setting the lifting speed of a crucible rod 1-11 to be 1 mm/h; when the diameter of the crystal is 50mm, setting a crucible lifting motor 1-16 and the rising speed of a crucible rod 1-11 to be 1.5 mm/h; when the diameter of the crystal is 60mm, setting a crucible lifting motor 1-16, setting the lifting speed of a crucible rod 1-11 to be 2mm/h, ending the shouldering process, and continuing the whole process for 8 hours;
seventhly, 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 increasing dynamic process, namely, the flow is linearly increased to 100ml/min from the initial 20ml/min after 480 minutes, and when the shouldering process is finished, the flow of the hydrogen flowmeter 2-1 is kept at 100 ml/min.
After the crystal shouldering process is finished, the appearance of the crystal from the seed crystal position to the shouldering ending position is as follows: the crystal is conical in shape, the overall height is 80mm, and the diameter of the bottom of the crystal is about 60 mm. The traditional method that adopts to adopt seed crystal pole water-cooling has two drawbacks, and firstly the control accuracy of seed crystal pole circulation rivers does not have gas flowmeter accurate relatively, and secondly along with the continuation of shouldering the process, crystal length increases, and the water-cooling effect of seed crystal pole also can weaken gradually, and this phenomenon that can lead to the crystal appearance to appear unsmooth undulation. The invention utilizes the accurate control of the dynamic atmosphere flow in the shouldering process and slowly and linearly increases the dynamic atmosphere flow to ensure that the heat loss of the system reaches relative balance, so that the conical side surface of the crystal is in a continuous and smooth state, and the control effect is good.
Claims (2)
1. A shoulder appearance adjusting device in indium antimonide crystal growth process, includes single crystal furnace device (1) and external controlling means (2) of stove, its characterized in that: the furnace 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 front-stage valve (2-8) and a molecular pump (2-9); the hydrogen flowmeter (2-1) and the argon flowmeter (2-2) are arranged on a gas pipe of a gas inlet (1-2) of the single crystal furnace device (1); the electric control valve (2-6) is connected with the air outlet (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 installed on 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 front-stage 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.
2. Adjusting device for shouldering morphology in indium antimonide crystal growth process according to claim 1
The adjusting method is characterized in that: the adjusting method comprises the following steps:
firstly, loading an indium antimonide polycrystalline raw material into a quartz crucible (1-5), and placing the crucible (1-5) in a crucible supporting seat (1-9);
secondly, firstly connecting an argon gas flowmeter (2-2) with an argon gas bottle, connecting a hydrogen gas flowmeter (2-1) with a hydrogen gas 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 percent and the maximum opening to be 100 percent, performing low-vacuum air extraction operation on the system by utilizing an air passage of an air outlet (1-12), the mechanical pump (2-7) and the electric control valve (2-6), and when the vacuum of the system is reduced to 3 × 10-1Pa, setting the minimum opening degree of the electric control valves (2-6) to be 0% and the maximum opening degree to be 0%, namely closing the gas path of the electric control valves (2-6), then opening the front valves (2-8) of the molecular pumps, starting the molecular pumps (2-9) to start high vacuum pumping operation, and when the vacuum of the system is reduced to 1 × 10-3When Pa is needed, the molecular pump (2-9) and the molecular pump front-stage valve (2-8) are closed, and finally the mechanical pump (2-7) is closed;
setting the flow rate of a hydrogen flowmeter (2-1) to be 1000ml/min and the flow rate of an argon flowmeter (2-2) to be 9000ml/min in an upper computer control device (2-3), enabling the hydrogen and the argon to enter a furnace body (1-3) through an air inlet hole (1-2), and setting the flow rates of the flowmeters (2-1) and (2-2) to be 0ml/min when the inflation pressure in the furnace reaches 1000 mbar;
fourthly, a power supply is turned on, alternating current in the induction coils (1-10) enables the induction heating bodies (1-6) to generate eddy currents to generate heat, then crucibles and raw materials in the heat preservation systems (1-7) are heated, after the raw materials are completely melted, the rotating speed of crucible rotating motors (1-14) is set to be 10rpm, and the direction 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 descended to the position 1cm above the melt liquid level;
setting the target pressure of a pressure control instrument (2-5) to be 1080mbar in an upper computer control device (2-3), setting the flow of a hydrogen flowmeter (2-1) to be 20ml/min, enabling dynamic hydrogen to flow through the area above the crystal under the guidance of an air guide sleeve (1-4), then setting the minimum opening of an electric control valve (2-6) to be 5% and the maximum opening to be 15%, finally starting a mechanical pump (2-7), waiting for 30 minutes, enabling the air intake and the air exhaust of the system to achieve dynamic balance, enabling the pressure of the system to be stable at 1080mbar, and controlling the vertical fluctuation to be +/-0.5 mbar;
sixthly, seed crystals (1-8) are in contact with the surface of the melt for seeding, after the lower end face of the seed crystals and the melt are fused, the upper computer control device (2-3) controls the seed crystal lifting motor (1-15) to move up and down on the seed crystal lifting lead screw (1-19), the seed crystal rod (1-1) is made to move up and down through the seed crystal lifting synchronization device (1-17), and the seed crystals (1-8) are lifted and pulled; the crucible lifting motors (1-16) are controlled by the upper computer control device (2-3) to move up and down on the crucible rod lifting lead screws (1-20), and the crucible rods (1-11) are driven to move up and down by the crucible lifting synchronous devices (1-18); setting seed crystal lifting motors (1-15) in an upper computer control device (2-3), wherein the pulling speed of a seed crystal rod (1-1) is 10 mm/h; when the diameter of the crystal is 10mm, setting a crucible lifting motor (1-16), wherein the rising speed of a crucible rod (1-11) is 0.1 mm/h; when the diameter of the crystal is 20mm, setting a crucible lifting motor (1-15), and setting the lifting speed of a crucible rod (1-11) to be 0.3 mm/h; when the diameter of the crystal is 30mm, setting a crucible lifting motor (1-16), and setting the lifting speed of a crucible rod (1-11) to be 0.6 mm/h; when the diameter of the crystal is 40mm, setting a crucible lifting motor (1-16), and setting the lifting speed of a crucible rod (1-11) to be 1 mm/h; when the diameter of the crystal is 50mm, setting a crucible lifting motor (1-16) and the rising speed of a crucible rod (1-11) to be 1.5 mm/h; when the diameter of the crystal is 60mm, setting a crucible lifting motor (1-16), setting the rising speed of a crucible rod (1-11) to be 2mm/h, finishing the shouldering process, and continuing the whole process for 8 hours;
seventhly, 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 increasing dynamic process, namely, the flow is linearly increased to 100ml/min from the initial 20ml/min after 480 minutes, and when the shouldering process is finished, the flow of the hydrogen flowmeter (2-1) is kept at 100 ml/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112126982A (en) * | 2020-10-22 | 2020-12-25 | 中国电子科技集团公司第四十六研究所 | Method for rapidly growing InSb monocrystal |
| CN114318510A (en) * | 2021-12-30 | 2022-04-12 | 无锡晶名光电科技有限公司 | Indium antimonide crystal growth method and crystal growth furnace |
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| 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 |
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