CN112064108B - Vacuum high-pressure single crystal furnace system for growing mercury telluride crystal and control method thereof - Google Patents
Vacuum high-pressure single crystal furnace system for growing mercury telluride crystal and control method thereof Download PDFInfo
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- CN112064108B CN112064108B CN202010953790.0A CN202010953790A CN112064108B CN 112064108 B CN112064108 B CN 112064108B CN 202010953790 A CN202010953790 A CN 202010953790A CN 112064108 B CN112064108 B CN 112064108B
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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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
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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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/28—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- 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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Abstract
The invention discloses a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals and a control method thereof, which solve the problem of how to complete the growth of mercury telluride crystals. The device comprises a single crystal furnace bracket (33), a vacuum pump (36), an argon filling device, a circulating water cooling device (37), an electric control cabinet (34) and a driving shaft lifting driving device (38), wherein a lower furnace body (1) and an upper furnace body (3) are respectively arranged on the single crystal furnace bracket (33), a driving shaft extending hole (24) is arranged at the center of the bottom plate of the lower furnace body (1), a driving shaft (23) is arranged in the driving shaft extending hole, a quartz crucible (16) is arranged at the top end of the driving shaft (23) extending into the inner cavity of the furnace body, a closed quartz tube (17) filled with mercury telluride powdery materials is arranged in the quartz crucible, and the lower end of the driving shaft arranged outside the furnace body is mechanically connected with the driving shaft lifting driving device (38); the growth of large-diameter mercury telluride crystals is realized.
Description
Technical Field
The invention relates to a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals, in particular to a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals and a control method thereof.
Background
The mercury telluride is a semiconductor material, has excellent thermoelectric performance and negative thermal expansion coefficient, and can be used for manufacturing an infrared detector; mercury telluride crystals are prepared by the bridgman method of zone melting, which is: the method comprises the steps of (1) loading a mercury telluride powder material into a closed cylindrical quartz tube, placing the quartz tube into a crucible, placing the crucible into a single crystal furnace, setting a heating field with a certain temperature gradient from high to low in the single crystal furnace, controlling the temperature of a high temperature area in the furnace to be slightly higher than the melting point of the mercury telluride powder material, starting melting the mercury telluride powder material in the quartz tube in the high temperature area, and keeping the melting point of the mercury telluride powder material for a period of time, wherein mercury vapor with higher pressure is generated in the closed quartz tube along with the complete melting of mercury telluride powder in the quartz tube, and filling high-pressure argon into the closed single crystal furnace to balance the internal and external pressures of the quartz tube in order to prevent the quartz tube from bursting; then, the mechanical control system controls the crucible support to slowly move the crucible from a high temperature field to a low temperature field in the furnace gradually, even if the crucible gradually passes through a heating field with a certain temperature gradient, in the moving process, after the temperature of the bottom of the crucible is reduced to a temperature field below the melting point of mercury telluride, the molten mercury telluride raw material starts to grow crystal, the crystal starts to grow, and the crystal continuously grows along with the descending of the crucible, so that the growth of the mercury telluride in the quartz tube is completed.
The generation of mercury telluride crystals in a single crystal furnace has close relation with the arrangement of a gradient temperature field in the furnace and the stability of the gradient temperature field, the temperature of a high temperature area in the single crystal furnace is up to 1000 ℃, the temperature of a low temperature area is 500 ℃, the stable formation of the temperature field with large temperature difference in the same single crystal furnace is realized by what means, and the problem to be solved when the structure of the temperature field in the single crystal furnace is designed is solved, the mercury telluride raw material is melted in the high temperature area, the crystal grows in the low temperature area, and the problem that how to ensure the temperature difference between the high temperature area and the low temperature area to be stable at 110 ℃ is another problem to be solved in the design of furnace body equipment; in addition, when the mercury telluride powder material is melted in a sealed quartz tube, a large vapor pressure is generated in the tube, and in order to balance the pressure in the tube and avoid bursting of the quartz tube, argon with a certain pressure is required to be filled in the single crystal furnace to balance the pressure inside and outside the quartz tube, but if accidents occur, such as cracking of the quartz tube, how to protect the environment of a furnace chamber in the furnace body and clean broken quartz tube slag is a problem to be considered in the structural design of the furnace body.
The existing single crystal furnace consists of a cylindrical upper furnace body and a cylindrical lower furnace body, wherein the upper furnace body is buckled on the lower furnace body, and after the upper furnace body and the lower furnace body are buckled together, a furnace inner cavity is formed by the inner cavity of the upper furnace body and the inner cavity of the lower furnace body; the mercury telluride crystal growth needs to be carried out in a closed oxygen-free high-pressure furnace cavity, and the furnace cavity needs to be vacuumized and then filled with high-pressure argon; in the whole process, the inner cavity of the furnace is required to be reliably sealed, the locking and sealing between the upper furnace body and the lower furnace body are required to be realized, and the situation of bearing the positive pressure and the negative pressure in the furnace is also required to be considered, so that the reliable locking and sealing of the connecting part of the upper furnace body and the lower furnace body is directly related to the mercury telluride crystal growth process; in addition, in the process of growing the mercury telluride, a driving shaft of a bracket for supporting the crucible moves from top to bottom, the driving shaft penetrates out of the furnace from the furnace bottom in the furnace and is mechanically connected with a driving mechanism, dynamic sealing between the driving shaft and the furnace body is also an important link of the equipment, once the crucible leaks in the lifting or rotating process, the temperature field and the pressure in the furnace can be destroyed if the dynamic sealing between the furnace body and the driving shaft leaks, the quality of the mercury telluride growing crystal is influenced, and particularly, the life safety of operators nearby can be endangered after the mercury telluride vapor is toxic and leaks; sealing of the furnace body is therefore particularly important.
In the crystal growth of a single crystal furnace, the temperature in the furnace reaches thousands of DEG, how to realize the heat preservation of a temperature field in the furnace is a theme, how to realize the cooling of the furnace wall outside the furnace body, especially the cooling of a driving shaft which is used for bearing the movement of a crucible and extends out of the furnace body, and how to realize the cooling of a locking sealing ring between an upper furnace body and a lower furnace body are also a problem to be solved on site.
Disclosure of Invention
The invention provides a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals and a control method thereof, which solve the technical problem of how to complete the growth of mercury telluride crystals.
The invention solves the technical problems by the following technical proposal:
a high-pressure single crystal furnace body structure for realizing gradient distribution of temperature fields in a furnace comprises a lower furnace body and an upper furnace body, wherein the upper furnace body is buckled on an upper port staggered tooth flange plate of the lower furnace body through a lower port staggered tooth flange plate of the upper furnace body, so that an inner cavity of the upper furnace body is communicated with an inner cavity of the lower furnace body, a driving shaft extending hole is formed in the center of a bottom plate of the lower furnace body, a lower heat preservation cylinder along the vertical direction is arranged in the inner cavity of the lower furnace body, a lower heat preservation cylinder heating resistance wire is arranged on the inner side wall of the lower heat preservation cylinder, the driving shaft extending hole is arranged in the lower heat preservation cylinder, an upper heat preservation cylinder supporting bracket is arranged on the upper port staggered tooth flange plate, an upper heat preservation cylinder arranged along the vertical direction is arranged on the upper heat preservation cylinder supporting bracket, an upper heat-preserving cylinder heating resistance wire is arranged on the inner side wall of the upper heat-preserving cylinder, a cover plate is arranged at the top end of the upper heat-preserving cylinder, the lower heat-preserving cylinder is in butt joint with the bottom end of the upper heat-preserving cylinder, a closed furnace temperature field space is formed by the bottom plate of the lower furnace body, the lower heat-preserving cylinder, the upper heat-preserving cylinder and the cover plate, a metal temperature-homogenizing cylinder is arranged in the closed furnace temperature field space, an explosion-proof quartz cylinder is arranged in the metal temperature-homogenizing cylinder, a driving shaft penetrates through a driving shaft extending hole from bottom to top and then is arranged in the explosion-proof quartz cylinder, a quartz crucible bracket is arranged at the top end of the driving shaft, a quartz crucible is arranged on the quartz crucible bracket, and a closed quartz tube filled with mercury telluride powdery materials is placed in the quartz crucible; argon is filled in the inner cavity of the furnace body and the inner cavity of the lower furnace body which are communicated together in a closed way; the temperature in the upper heat preservation cylinder is 720-1000 ℃, and the temperature in the lower heat preservation cylinder is 500-700 ℃.
The upper heat-preserving cylinder heating resistance wire arranged on the inner side wall of the upper heat-preserving cylinder is a heating resistance wire controlled by three sections respectively, the lower heat-preserving cylinder heating resistance wire arranged on the inner side wall of the lower heat-preserving cylinder is a heating resistance wire controlled by two sections respectively, five sections of gradient distribution temperature fields with the temperature ranging from high to low are formed in the anti-burst quartz cylinder from top to bottom, a temperature sensor is arranged at the center of each section of temperature field, the temperature in the temperature field with the lowest temperature is 500 ℃, and the temperature in the temperature field with the highest temperature is 1000 ℃.
The lower furnace body is respectively provided with a vacuumizing port, an argon filling port and a temperature sensor connecting seat in the furnace chamber, and the upper port staggered tooth flange is provided with a heating resistance wire electrode outgoing line.
The upper furnace body and the lower furnace body of the high-pressure single crystal furnace are locked and sealed, comprising a lower furnace body and an upper furnace body, wherein the upper furnace body is buckled on an upper port staggered tooth flange plate of the lower furnace body through a lower port staggered tooth flange plate of the upper furnace body; a dynamic sealing flange plate is arranged in the driving shaft extending hole, a driving shaft is movably arranged in the dynamic sealing flange plate, a shaft sealing ring is arranged between the dynamic sealing flange plate and the driving shaft, and a hole sealing ring is arranged between the dynamic sealing flange plate and the driving shaft extending hole.
An upper furnace body water cooling jacket is arranged on the outer side furnace wall of the upper furnace body, a lower furnace body water cooling jacket is arranged on the outer side furnace wall of the lower furnace body, and an upper port staggered-tooth flange plate circulating waterway is arranged on the upper port staggered-tooth flange plate.
The driving shaft is a hollow shaft, a spiral water cooling passage is arranged in the driving shaft, and a water inlet and a water outlet of the spiral water cooling passage are arranged at the lower end of the driving shaft.
The vacuum high-pressure single crystal furnace system for growing mercury telluride crystals comprises a single crystal furnace bracket, a vacuum pump, an argon filling device, a circulating water cooling device, an electric control cabinet and a driving shaft lifting driving device, wherein a lower furnace body and an upper furnace body are respectively arranged on the single crystal furnace bracket; the lower furnace body is respectively provided with a vacuumizing port, an argon filling port and a temperature sensor connecting seat in the furnace chamber, the upper port staggered-tooth flange plate is provided with a heating resistance wire electrode outgoing line, the vacuumizing port is connected with a vacuum pump, the argon filling port is connected with an argon filling device, and the heating resistance wire electrode outgoing line and the temperature sensor connecting seat in the furnace chamber are respectively electrically connected with an electric control cabinet.
An upper furnace body lifting mechanism is arranged on the single crystal furnace support, the upper furnace body lifting mechanism (mechanically connected with an upper furnace body, a mercury analyzer is arranged on an electric control cabinet, an upper furnace body water cooling jacket is arranged on an outer side furnace wall of the upper furnace body, a lower furnace body water cooling jacket is arranged on an outer side furnace wall of the lower furnace body, an upper port staggered tooth flange plate circulating waterway is arranged on an upper port staggered tooth flange plate, and the upper furnace body water cooling jacket, the lower furnace body water cooling jacket and the upper port staggered tooth flange plate circulating waterway are respectively communicated with a circulating water cooling device.
A control method of a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals is characterized by comprising the following steps:
firstly, placing a closed quartz tube filled with mercury telluride powdery materials into a quartz crucible, fastening an upper furnace body and a lower furnace body together through an upper furnace body lifting mechanism, and locking a lower port staggered tooth flange plate and an upper port staggered tooth flange plate together through rotating a locking ring with staggered teeth;
secondly, vacuumizing a furnace cavity formed by the upper furnace cavity and the lower furnace cavity by a vacuum pump connected to a vacuumizing port, and after vacuumizing, filling argon into the furnace cavity by controlling an argon filling device;
thirdly, controlling a driving shaft lifting driving device to enable the quartz crucible to be arranged in a high-temperature field of a gradient distribution temperature field in the upper heat preservation cylinder;
fourth, the upper heat-preserving cylinder heating resistance wire and the lower heat-preserving cylinder heating resistance wire are controlled to be electrified through the electric control cabinet, the furnace chamber is heated, signals transmitted back to the electric control cabinet through the temperature sensor dynamically adjust the electrified power of the upper heat-preserving cylinder heating resistance wire and the lower heat-preserving cylinder heating resistance wire, so that the temperature at the center of a high temperature field of a gradient distribution temperature field in the upper heat-preserving cylinder is 720 ℃, and the temperature at the center of a low temperature field of the gradient distribution temperature field in the lower heat-preserving cylinder is 500 ℃;
fifthly, melting the powdered mercury telluride material in the airtight quartz tube, generating steam, and controlling an argon filling device by an electric control cabinet to continuously fill argon into the furnace cavity, so that the pressure of the argon filled into the furnace cavity is equal to the pressure of the mercury steam generated in the airtight quartz tube;
and sixthly, after all the powdered mercury telluride materials in the airtight quartz tube are melted, the electric control cabinet controls the driving shaft to descend through the driving shaft lifting driving device, so that the quartz crucible descends to a low-temperature field of a gradient distribution temperature field, the melted mercury telluride in the airtight quartz tube starts to grow, and after the quartz crucible descends by 100 mm, the melted mercury telluride in the airtight quartz tube is grown.
The electric control cabinet controls the circulating cooling water in the upper furnace body water cooling jacket, the circulating cooling water in the lower furnace body water cooling jacket and the circulating cooling water in the upper port staggered-tooth flange plate circulating waterway to circulate through the circulating water cooling device so as to finish cooling the outer side wall of the furnace body and the driving shaft.
The invention builds a reliable and stable temperature gradient field in the single crystal furnace in vacuum and high pressure environment, realizes the growth of large-diameter crystals, and improves the crystal quality and yield.
Drawings
FIG. 1 is a schematic general construction of the present invention;
FIG. 2 is a schematic view of the furnace structure of the present invention;
FIG. 3 is a diagram of the relationship between the furnace and the vacuum apparatus 36 and the drive shaft lift drive 38 of the present invention.
Detailed Description
The invention is described in detail below with reference to the attached drawing figures:
a high-pressure single crystal furnace body structure for realizing gradient distribution of a temperature field in a furnace comprises a lower furnace body 1 and an upper furnace body 3, wherein the upper furnace body 3 is buckled on an upper port staggered tooth flange 2 of the lower furnace body 1 through a lower port staggered tooth flange 4 of the upper furnace body 3, staggered teeth on the two flange plates are matched with staggered teeth on a locking ring 5 with staggered teeth, the lower furnace body 1 and the upper furnace body 3 are locked and connected together to enable an upper furnace body inner cavity 9 to be communicated with a lower furnace body inner cavity 18, a driving shaft extending hole 24 is arranged at the center of a furnace bottom plate of the lower furnace body 1, a lower heat preservation cylinder 20 along the vertical direction is arranged in the lower furnace body inner cavity 18, a lower heat preservation cylinder heating resistance wire 21 is arranged on the inner side wall of the lower heat preservation cylinder 20, the driving shaft extending hole 24 is arranged at the center of the lower port of the lower heat preservation cylinder 20, an upper heat preservation cylinder supporting bracket 10 is arranged at the inner side end of the upper port staggered tooth flange 2, an upper heat preservation cylinder 11 arranged along the vertical direction is arranged on an upper heat preservation cylinder support bracket 10, an upper heat preservation cylinder heating resistance wire 13 is arranged on the inner side wall of the upper heat preservation cylinder 11, a cover plate 12 is arranged at the top end of the upper heat preservation cylinder 11, the top end opening of a lower heat preservation cylinder 20 is butted with the bottom end opening of the upper heat preservation cylinder 11, a furnace bottom plate of a lower furnace body 1, the lower heat preservation cylinder 20, the upper heat preservation cylinder 11 and the cover plate 12 form a closed furnace temperature field space, a metal temperature equalization cylinder 14 is arranged in the closed furnace temperature field space, an explosion-proof quartz cylinder 15 is arranged in the metal temperature equalization cylinder 14, the top end of a driving shaft 23 passes through a driving shaft extending hole 24 from bottom to top and then is arranged in the explosion-proof quartz cylinder 15, a quartz crucible bracket 22 is arranged at the top end of the driving shaft 23, the lower end of the quartz crucible bracket 22 is fixedly connected with the top end of the driving shaft 23, a quartz crucible 16 is arranged on the quartz crucible support 22, and a closed quartz tube 17 filled with mercury telluride powdery material is arranged in the quartz crucible 16; argon is filled in the furnace body cavity 9 and the lower furnace body cavity 18 which are communicated together in a closed way; the temperature in the upper heat preservation cylinder 11 is 720-1000 ℃, and the temperature of the lower heat preservation cylinder 20 is 500-700 ℃; argon is filled in the metal temperature equalizing cylinder 14 and the anti-cracking quartz cylinder 15; if bursting of the closed quartz tube 17 with the mercury telluride powder material occurs, the broken glass will be collected in the bursting quartz tube 15.
The upper heat-preserving cylinder heating resistance wire 13 arranged on the inner side wall of the upper heat-preserving cylinder 11 is a three-section heating resistance wire which is controlled by sections respectively, the lower heat-preserving cylinder heating resistance wire 21 arranged on the inner side wall of the lower heat-preserving cylinder 20 is a two-section heating resistance wire which is controlled by sections respectively, five sections of gradient distribution temperature fields with the temperature from high to low are formed in the anti-cracking quartz cylinder 15 from top to bottom, a temperature sensor is arranged at the center of each section of temperature field, the temperature in the temperature field with the lowest temperature is 500 ℃, and the temperature in the temperature field with the highest temperature is 1000 ℃; the temperature of the five-section gradient distribution temperature field can be regulated and controlled by controlling the input power of the heating resistance wire of the five-section gradient distribution temperature field.
A vacuum pumping port 30, an argon filling port 31 and a temperature sensor connecting seat 32 in the furnace chamber are respectively arranged on the lower furnace body 1, and a heating resistance wire electrode outgoing line 29 is arranged on the upper port staggered-tooth flange 2; the external furnace equipment is connected with the internal furnace mechanism through the interfaces.
The upper furnace body and the lower furnace body of the high-pressure single crystal furnace are locked and the furnace body sealing structure comprises a lower furnace body 1 and an upper furnace body 3, wherein the upper furnace body 3 is buckled on an upper port staggered tooth flange 2 of the lower furnace body 1 through a lower port staggered tooth flange 4 of the upper furnace body, a driving shaft extending hole 24 is formed in the center of a furnace bottom plate of the lower furnace body 1, a locking ring 5 with staggered teeth is arranged between the lower port staggered tooth flange 4 and the upper port staggered tooth flange 2, a wedge block 40 is arranged on a locking tooth of the locking ring 5 with staggered teeth, the wedge surface of the wedge block 40 arranged on the locking tooth of the locking ring 5 with staggered teeth is matched with the staggered tooth top surface of the lower port staggered tooth flange 4 of the upper furnace body 3 through rotation of the locking ring 5 with staggered teeth, the lower furnace body 1 is locked with the upper furnace body 3, a lip sealing ring 6 and an O-shaped sealing ring 7 are respectively arranged between the lower port staggered tooth flange 4 and the upper port staggered tooth flange 2, and the lip sealing ring 6 can seal both an upper vertical connecting surface and a horizontal connecting surface under the condition of positive and negative pressure in the furnace; a dynamic sealing flange 25 is arranged in the driving shaft extending hole 24, a driving shaft 23 is movably arranged in the dynamic sealing flange 25, a shaft sealing ring 26 is arranged between the dynamic sealing flange 25 and the driving shaft 23, a hole sealing ring 27 is arranged between the dynamic sealing flange 25 and the driving shaft extending hole 24, and when the driving shaft 23 rotates or moves up and down, the hole sealing ring 27 can play a role in sealing the inside and the outside of the furnace chamber.
An upper furnace body water cooling jacket 8 is arranged on the outer side furnace wall of the upper furnace body 3, a lower furnace body water cooling jacket 19 is arranged on the outer side furnace wall of the lower furnace body 1, an upper port staggered tooth flange plate circulating water channel 41 is arranged on the upper port staggered tooth flange plate 2, and the arrangement of the cooling water channels ensures that the temperature of the outer side of the furnace body is not overhigh, and simultaneously plays a role in isolating the temperature transmission inside and outside the furnace body.
The driving shaft 23 is a hollow shaft, a spiral water cooling passage 28 is arranged in the driving shaft 23, and a water inlet and a water outlet of the spiral water cooling passage 28 are arranged at the lower end of the driving shaft 23; the electric signal circuit of the temperature sensor arranged in the quartz crucible 16 is transmitted to the outside of the furnace through the central through hole of the driving shaft 23, the spiral water cooling passages 28 are arranged at equal intervals on the driving shaft 23, and the water inlet waterway and the water return waterway are arranged at intervals.
The vacuum high-pressure single crystal furnace system for growing mercury telluride crystals comprises a single crystal furnace bracket 33, a vacuum pump 36, an argon filling device, a circulating water cooling device 37, an electric control cabinet 34 and a driving shaft lifting driving device 38, wherein a lower furnace body 1 and an upper furnace body 3 are respectively arranged on the single crystal furnace bracket 33, the upper furnace body 3 is buckled on an upper port staggered tooth flange 2 of the lower furnace body 1 through a lower port staggered tooth flange 4 of the upper furnace body 3, an upper furnace body cavity 9 and a lower furnace body cavity 18 are communicated to form a furnace body cavity, a driving shaft extending hole 24 is arranged at the center of a bottom plate of the lower furnace body 1, a driving shaft 23 is arranged in the driving shaft extending hole 24, a quartz crucible 16 is arranged at the top end of the driving shaft 23 extending into the furnace body cavity, a closed quartz tube 17 filled with mercury telluride powdery material is arranged in the quartz crucible 16, and the lower end of the driving shaft 23 arranged outside the furnace body is mechanically connected with the driving shaft lifting driving device 38; the lower furnace body 1 is respectively provided with a vacuum pumping port 30, an argon filling port 31 and a furnace chamber inner temperature sensor connecting seat 32, the upper port staggered-tooth flange plate 2 is provided with a heating resistance wire electrode outgoing line 29, the vacuum pumping port 30 is connected with a vacuum pump 36, the argon filling port 31 is connected with an argon filling device, and the heating resistance wire electrode outgoing line 29 and the furnace chamber inner temperature sensor connecting seat 32 are respectively electrically connected with an electric control cabinet 34; a control computer is arranged in the electric control cabinet 34, and a control program in the computer controls each system to work cooperatively so as to complete the crystal growth of the mercury telluride.
An upper furnace body lifting mechanism 35 is arranged on the single crystal furnace bracket 33, the upper furnace body lifting mechanism 35 is mechanically connected with the upper furnace body 3, and a mercury analyzer 39 is arranged on the electric control cabinet 34; an upper furnace body water cooling jacket 8 is arranged on the outer side furnace wall of the upper furnace body 3, a lower furnace body water cooling jacket 19 is arranged on the outer side furnace wall of the lower furnace body 1, a locking ring circulating water channel 41 is arranged in the locking ring 5 with staggered teeth, and the upper furnace body water cooling jacket 8, the lower furnace body water cooling jacket 19 and the locking ring circulating water channel 41 are respectively communicated with the circulating water cooling device 37.
A control method of a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals is characterized by comprising the following steps:
firstly, placing a closed quartz tube 17 filled with mercury telluride powder material into a quartz crucible 16, fastening an upper furnace body 3 and a lower furnace body 1 together through an upper furnace body lifting mechanism 35, and locking a lower port staggered tooth flange 4 and an upper port staggered tooth flange 2 together through rotating a locking ring 5 with staggered teeth;
secondly, vacuumizing a furnace cavity formed by the upper furnace cavity 9 and the lower furnace cavity 18 through a vacuum pump 36 connected to the vacuumizing port 30, and after vacuumizing, filling argon into the furnace cavity by controlling an argon filling device to create an oxygen-free environment and a pressurized argon environment in the furnace;
thirdly, controlling the driving shaft lifting driving device 38 to enable the quartz crucible 16 to be arranged in a high-temperature field of the gradient distribution temperature field in the upper heat preservation cylinder 11;
fourth, the electric control cabinet 34 is used for controlling the upper heat preservation cylinder heating resistance wire 13 and the lower heat preservation cylinder heating resistance wire 21 to be electrified, the furnace chamber is heated, signals transmitted back to the electric control cabinet 34 through the temperature sensor are used for dynamically adjusting the electric power of the upper heat preservation cylinder heating resistance wire 13 and the lower heat preservation cylinder heating resistance wire 21, so that the temperature at the center of a high temperature field of a gradient distribution temperature field in the upper heat preservation cylinder 11 is 720 ℃, and the temperature at the center of a low temperature field of a gradient distribution temperature field in the lower heat preservation cylinder 20 is 500 ℃;
fifthly, melting the mercury telluride powder material in the airtight quartz tube 17, generating steam, and controlling an argon filling device by the electric control cabinet 34 to continuously fill argon into the furnace cavity so that the pressure of the argon filled into the furnace cavity is equal to the pressure of the mercury steam generated in the airtight quartz tube 17;
and sixthly, after all the powdered mercury telluride materials in the sealed quartz tube 17 are melted, the electric control cabinet 34 controls the driving shaft 23 to descend through the driving shaft lifting driving device 38, so that the quartz crucible 16 descends into a low-temperature field of a gradient distribution temperature field, the melted mercury telluride in the sealed quartz tube 17 starts to grow, and after the quartz crucible 16 descends by 100 mm, the growth of the melted mercury telluride in the sealed quartz tube 17 is completed.
The electric control cabinet 34 controls the circulating cooling water in the upper furnace body water cooling jacket 8, the circulating cooling water in the lower furnace body water cooling jacket 19 and the circulating cooling water in the upper port staggered flange disc circulating water channel 41 to circulate through the circulating water cooling device 37 so as to finish cooling the outer side wall of the furnace body and the driving shaft 23; a stable temperature field gradient distribution environment is created in the furnace through the cooperation of the electric heating system and the water cooling system.
Claims (2)
1. A control method of a vacuum high-pressure single crystal furnace system for growing mercury telluride crystals comprises a single crystal furnace bracket (33), a vacuum pump (36), an argon filling device, a circulating water cooling device (37), an electric control cabinet (34) and a driving shaft lifting driving device (38), wherein a lower furnace body (1) and an upper furnace body (3) are respectively arranged on the single crystal furnace bracket (33), the upper furnace body (3) is buckled on an upper port staggered tooth flange (2) of the lower furnace body (1) through a lower port staggered tooth flange (4) of the upper furnace body, an upper furnace body inner cavity (9) is communicated with a lower furnace body inner cavity (18) to form a furnace body inner cavity, a driving shaft extending hole (24) is formed in the center of a furnace bottom plate of the lower furnace body (1), a driving shaft (23) is arranged in the driving shaft extending hole (24), a quartz crucible (16) is arranged at the top end of the driving shaft (23) extending into the furnace body inner cavity, a sealed quartz tube (17) filled with mercury telluride powdery material is arranged in the quartz crucible (16), and the lower end of the driving shaft (23) arranged outside the furnace body is mechanically connected with the driving shaft lifting driving device (38); a vacuum pumping port (30), an argon filling port (31) and a temperature sensor connecting seat (32) in the furnace chamber are respectively arranged on the lower furnace body (1), a heating resistance wire electrode outgoing line (29) is arranged on the upper port staggered flange plate (2), the vacuum pumping port (30) is connected with a vacuum pump (36), the argon filling port (31) is connected with an argon filling device, and the heating resistance wire electrode outgoing line (29) and the temperature sensor connecting seat (32) in the furnace chamber are respectively electrically connected with an electric control cabinet (34); an upper furnace body lifting mechanism (35) is arranged on the single crystal furnace bracket (33), the upper furnace body lifting mechanism (35) is mechanically connected with the upper furnace body (3), and a mercury analyzer (39) is arranged on the electric control cabinet (34); an upper furnace body water cooling jacket (8) is arranged on the outer side furnace wall of the upper furnace body (3), a lower furnace body water cooling jacket (19) is arranged on the outer side furnace wall of the lower furnace body (1), an upper port staggered tooth flange disc circulating water channel (41) is arranged on the upper port staggered tooth flange disc (2), and the upper furnace body water cooling jacket (8), the lower furnace body water cooling jacket (19) and the upper port staggered tooth flange disc circulating water channel (41) are respectively communicated with a circulating water cooling device (37); the method is characterized by comprising the following steps of:
firstly, placing a closed quartz tube (17) filled with mercury telluride powder material into a quartz crucible (16), fastening an upper furnace body (3) and a lower furnace body (1) together through an upper furnace body lifting mechanism (35), and locking a lower port staggered tooth flange plate (4) and an upper port staggered tooth flange plate (2) together through rotating a locking ring (5) with staggered teeth;
secondly, vacuumizing a furnace cavity formed by the upper furnace body cavity (9) and the lower furnace body cavity (18) through a vacuum pump (36) connected to the vacuumizing port (30), and after vacuumizing, filling argon into the furnace cavity through controlling an argon filling device;
thirdly, controlling a driving shaft lifting driving device (38) to enable the quartz crucible (16) to be arranged in a high-temperature field of a gradient distribution temperature field in the upper heat preservation cylinder (11);
fourth, the upper heat-preserving cylinder heating resistance wire (13) and the lower heat-preserving cylinder heating resistance wire (21) are controlled to be electrified through the electric control cabinet (34), the furnace chamber is heated, signals in the electric control cabinet (34) are returned through the temperature sensor, the electrifying power of the upper heat-preserving cylinder heating resistance wire (13) and the lower heat-preserving cylinder heating resistance wire (21) is dynamically adjusted, the temperature at the center of a high temperature field of a gradient distribution temperature field in the upper heat-preserving cylinder (11) is 720 ℃, and the temperature at the center of a low temperature field of a gradient distribution temperature field in the lower heat-preserving cylinder (20) is 500 ℃;
fifthly, melting the mercury telluride powder material in the airtight quartz tube (17) and generating steam, and controlling an argon filling device by an electric control cabinet (34) to continuously fill argon into the furnace cavity so that the pressure of the argon filled into the furnace cavity is equal to the pressure of the mercury steam generated in the airtight quartz tube (17);
and sixthly, after all the mercury telluride powder materials in the airtight quartz tube (17) are melted, the electric control cabinet (34) controls the driving shaft (23) to descend through the driving shaft lifting driving device (38) so as to enable the quartz crucible (16) to descend into a low-temperature field of a gradient distribution temperature field, crystal growth of the melted mercury telluride in the airtight quartz tube (17) is started, and after the quartz crucible (16) descends by 100 mm, crystal growth of the melted mercury telluride in the airtight quartz tube (17) is completed.
2. The control method of the vacuum high-pressure single crystal furnace system for growing mercury telluride crystals according to claim 1, wherein the electric control cabinet (34) controls the circulating cooling water in the upper furnace body water cooling jacket (8), the circulating cooling water in the lower furnace body water cooling jacket (19) and the circulating cooling water in the upper port staggered flange disc circulating waterway (41) to circulate through the circulating water cooling device (37) so as to finish cooling of the outer side wall of the furnace body and the driving shaft (23).
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