Gallium antimonide crystal growth device and growth method

Abstract

The invention provides a gallium antimonide crystal growing device and growing method. The gallium antimonide crystal growing device comprises a liquid sealing agent supplementing mechanism, and the liquid sealing agent supplementing mechanism is used for supplementing a corresponding amount of NaCl + KCl liquid sealing agent melt along with the growth of a crystal when the gallium antimonide crystal is grown by adopting a liquid sealing czochralski method. The gallium antimonide crystal growth method comprises the following steps: filling a gallium antimonide polycrystal, a doping agent and a liquid sealing agent into a crystal growth crucible, wherein the liquid sealing agent is NaCl + KCl mixed solid particles; filling the liquid sealing agent NaCl + KCl solid particles into a material adding crucible; vacuumizing, driving air and detecting leakage; filling nitrogen into the furnace body; raising the temperature; after the temperature is stable, the crystal grows; along with the growth of the crystal, a flow switch is adjusted, so that the liquid sealing agent in the feeding crucible is continuously supplemented and flows into the crystal growth crucible; after crystal growth is finished, the crystal growth crucible starts a cooling procedure, and the material adding crucible stops supplementing the liquid sealing agent to the crystal growth crucible until cooling is finished; and exhausting and injecting air, opening the furnace body, and cutting off the crystal bar.

Description

Technical Field

[0001] The present disclosure relates to the field of crystal growth, and more specifically to a gallium antimonide crystal growth device and a growth method. Background Art

[0002] GaSb (gallium antimonide) is a III-V compound semiconductor material. Its bandgap is well matched with other III-V alloys and ternary and quaternary antimony-containing compounds. Therefore, GaSb is an excellent substrate material for electronic and optoelectronic devices. It can be used in superlattice infrared detectors, solar cells, light-emitting diodes and other fields.

[0003] At present, GaSb is mostly grown by LEC method, that is, liquid-sealed Czochralski method. This process requires the use of a liquid sealant during crystal growth to reduce the volatilization of Sb elements in the melt, so that higher quality GaSb single crystals can be obtained. At present, the commonly used liquid sealants are mostly a mixture of NaCl and KCl. The mixture has the advantages of low melting point, low viscosity, low cost, and no reaction with GaSb. However, the saturated vapor pressure of the mixture liquid sealant near the melting point of GaSb is large, and the volatilization is more serious. As GaSb grows, the liquid sealant becomes thinner and thinner, resulting in more and more serious volatilization of Sb elements. In addition, in the initial stage of crystal growth, it is hoped that the thickness of the liquid sealant should not be too thick. Too thick liquid sealants will affect the observation of the crystal seeding stage, and it is very easy to obtain defective crystal materials. In addition, too thick liquid sealants will also lead to a small temperature gradient, and polycrystalline is easy to produce in the seeding stage. However, as the crystal grows, the crystal diameter and height become larger and larger, the heat scattered by the crystal increases, and the temperature gradient of the solid-liquid interface of the crystal growth is further increased, making it easier for dislocations to proliferate.

[0004] Therefore, it is necessary to design a crystal growth device and method. Summary of the invention

[0005] In view of the problems existing in the background technology, an object of the present invention is to provide a gallium antimonide crystal growth device and a growth method, which can achieve a liquid sealant thickness that not only reduces the volatilization of the Sb element but also reduces the temperature gradient during crystal growth and cooling, and reduces crystal dislocations during the entire liquid-sealed Czochralski method for growing gallium antimonide crystals.

[0006] Therefore, a gallium antimonide crystal growing device is provided, which includes a liquid sealing agent replenishing mechanism, which is used to replenish a corresponding amount of NaCl+KCl liquid sealing agent melt as the crystal grows when growing gallium antimonide crystals using a liquid-sealed Czochralski method.

[0007] A gallium antimonide crystal growth method comprises the steps of:

[0008] S1, loading gallium antimonide polycrystal, dopant and liquid sealing agent into a crystal growth crucible in a furnace body of a gallium antimonide crystal growth device, wherein the liquid sealing agent is a NaCl+KCl mixed solid particles;

[0009] S2, loading the liquid sealing agent NaCl+KCl solid particles into the feeding crucible;

[0010] S3, vacuuming, degassing, and leak detection;

[0011] S4, filling the furnace with nitrogen until the pressure inside the furnace reaches 0.1 MPa, and then stopping filling the furnace;

[0012] S5, raising the temperature to make the temperature of the crystal growth crucible reach the melting temperature of the GaSb polycrystal and the temperature of the feed crucible reach the melting temperature;

[0013] S6, after the temperature is stabilized, the seed crystal rod drives the seed crystal to extend under the liquid sealant on the surface of the crystal growth crucible, and the liquid seal Czochralski method is started to grow the crystal;

[0014] S7, as the crystal grows, adjust the flow switch so that the liquid sealing agent in the feeding crucible is continuously replenished and flows into the crystal growth crucible. The flow rate L of the liquid sealing agent and the pulling speed V of the crystal, the diameter d of the crystal during the pulling process, and the inner diameter D of the crystal growth crucible have the following relationship:

[0015]

[0016] S8, after the crystal growth is completed, the crystal growth crucible starts a cooling procedure, and until the cooling is completed, the feeding crucible stops replenishing the liquid sealing agent to the crystal growth crucible;

[0017] S9, evacuate the furnace body and inject air, then open the furnace body and cut the crystal rod off the lifting rod.

[0018] The beneficial effects of the present disclosure are as follows: in the gallium antimonide crystal growth device and growth method according to the present disclosure, during the entire process of growing gallium antimonide crystals by the liquid-sealed Czochralski method, the thickness of the liquid sealant can be achieved to not only reduce the volatilization of the Sb element but also reduce the temperature gradient during crystal growth and cooling, and reduce crystal dislocations. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic structural diagram of a gallium antimonide crystal growth device according to the present disclosure.

[0020] Figure 2 This is the EPD distribution diagram of the dislocation EPD scan of the GaSb crystal slice of Example 1

[0021] Figure 3 This is the EPD distribution diagram of the GaSb crystal slice of Comparative Example 1 after dislocation EPD scanning.

[0022] The description of the accompanying drawings is as follows.

[0023] 100 GaSb crystal growth device 163 base

[0024] 11Liquid sealant replenishing mechanism 164 screw

[0025] 111 feeding crucible 17 second heater

[0026] 112 first heater T1 graphite heater

[0027] 113 pipeline T2 graphite double layer insulation cover

[0028] 114 flow switch T21 inner layer

[0029] 12 controller T22 outer layer

[0030] 13 Crystal Growth Crucible T3 Carbon Felt

[0031] 14 seed crystal 18 vacuum interface

[0032] 15 lifting rod 19 gas inlet

[0033] 16 furnace body 20 first bracket

[0034] 161 top cover 21 second bracket

[0035] 162 Middle DETAILED DESCRIPTION

[0036] The accompanying drawings show embodiments of the present disclosure, and it will be understood that the disclosed embodiments are merely examples of the present disclosure, and the present disclosure can be implemented in various forms. Therefore, the specific details disclosed herein should not be interpreted as limiting, but merely as the basis for the claims and as a representative basis for teaching ordinary technicians in the field to implement the present disclosure in various ways.

[0037] [Gallium Antimonide Crystal Growth Device]

[0038] Reference Figure 1 According to the gallium antimonide crystal growing device 100 disclosed in the present invention, the liquid sealing agent replenishing mechanism 11 is used to replenish a corresponding amount of NaCl+KCl liquid sealing agent melt as the crystal grows when the gallium antimonide crystal is grown by the liquid-sealed Czochralski method.

[0039] In the gallium antimonide crystal growth device 100 according to the present disclosure, by setting the liquid sealing agent replenishing mechanism 11, a corresponding amount of NaCl+KCl liquid sealing agent melt can be replenished as the crystal grows when the gallium antimonide crystal is grown by the liquid sealing Czochralski method. In this way, during the entire process of growing the gallium antimonide crystal by the liquid sealing Czochralski method, the thickness of the liquid sealing agent can be achieved to not only reduce the volatilization of the Sb element but also reduce the temperature gradient during crystal growth and cooling, and reduce crystal dislocations.

[0040] like Figure 1 As shown, in one example, the gallium antimonide crystal growth device 100 further includes a controller 12 and a crystal growth crucible 13. The crystal growth crucible 13 is used to load gallium antimonide polycrystals and NaCl+KCl initial liquid sealant. The liquid sealant replenishing mechanism 11 includes a feed crucible 111, a first heater 112, a pipeline 113, and a flow switch 114. The feeding crucible 111 is used to load NaCl+KCl supplementary liquid sealing agent; the first heater 112 is used to heat the feeding crucible 111 to form a supplementary liquid sealing agent melt and to cool the feeding crucible 111; one end of the pipe 113 is connected to the feeding crucible 111 and the other end is located above the crystal growth crucible 13 so that the pipe 113 is used to replenish the molten supplementary liquid sealing agent melt in the feeding crucible 111 into the crystal growth crucible 13 during the process of growing gallium antimonide crystals by the liquid-sealed Czochralski method; the flow switch 114 is arranged on the pipe 113 and is communicatively connected to the controller 12 to control the flow of the supplementary liquid sealing agent transported through the pipe 113. Through the first heater 112, the flow switch 114 and the controller 12, a corresponding amount of NaCl+KCl liquid sealing agent melt is replenished to the crystal growth crucible 13.

[0041] In addition, for example, the crystal growth crucible 13 is initially charged with a dopant. Further, the dopant is gallium telluride. In one example, the mass fraction of the dopant relative to the gallium antimonide polycrystal charged in the crystal growth crucible 13 is 10-100 ppm.

[0042] The flow switch 114 may be, but is not limited to, a pipeline flow meter.

[0043] In addition, the gallium antimonide crystal growth device 100 also includes a speed meter (not shown) and an infrared measuring instrument (not shown). The speed meter is used to measure the pulling speed of the crystal, and the speed meter is communicatively connected to the controller 12; the infrared measuring instrument is used to monitor the diameter of the crystal and the inner diameter of the crystal growth crucible 13 during the pulling process, and the infrared measuring instrument is communicatively connected to the controller 12.

[0044] like Figure 1As shown, the gallium antimonide crystal growth device 100 also includes a seed crystal 14 and a lifting rod 15. The seed crystal 14 is fixed to the end of the lifting rod 15. For example, the seed crystal 14 is a gallium antimonide single crystal with a purity of 6N. The lifting rod 15 can move back and forth in the up and down directions, and the lifting rod 15 is used to drive the seed crystal 14 to move downward into the crystal growth crucible 13 to grow the gallium antimonide crystal by the liquid-sealed vertical pulling method. The lifting rod 15 is connected to a corresponding rotating mechanism (not shown) and a corresponding lifting mechanism (not shown) so as to be able to move linearly upward and rotate at the same time. Accordingly, the flow rate L of the liquid sealing agent supplemented by the liquid sealing agent supplementing mechanism 11 and the pulling speed V of the crystal, the diameter d of the crystal during the pulling process, and the inner diameter D of the crystal growth crucible 13 have the following relationship:

[0045]

[0046] like Figure 1 As shown, the GaSb crystal growth device 100 further includes a furnace body 16 . A feed crucible 111 is located in the furnace body 16 , a first heater 112 is located in the furnace body 16 , and a lifting rod 15 is disposed in the furnace body 16 .

[0047] Reference Figure 1 , the gallium antimonide crystal growth device 100 also includes a second heater 17, a vacuum interface 18, and a gas inlet 19. The crystal growth crucible 13, the feed crucible 111, the first heater 112, and the flow switch 114 are located in the furnace body 16. The second heater 17 is located in the furnace body 16, and the second heater is used to heat up and cool down the crystal growth crucible 13. The vacuum interface 18 and the gas inlet 19 are arranged on the furnace body 16, and the vacuum interface 18 is used to vacuum the furnace body 16, and the gas inlet 19 is used to fill the furnace body 16 with the required gas (such as the gas for driving out the gas, the gas during crystal growth).

[0048] Specifically, for example, Figure 1 As shown, the first heater 112 and the second heater 17 both include: a graphite heater T1, a graphite double-layer heat-insulating cover T2 and a carbon felt T3; the graphite heater T1 is arranged around a corresponding one of the crystal growth crucible 13 and the feed crucible 111, and the graphite double-layer heat-insulating cover T2 is arranged around the graphite heater T1. Figure 1 As shown, the graphite double-layer heat-insulating cover T2 includes an inner layer T21 and an outer layer T22; the carbon felt T3 is filled between the inner layer T21 and the outer layer T22 of the graphite double-layer heat-insulating cover T2.

[0049] like Figure 1As shown, in one example, the gallium antimonide crystal growth device 100 also includes a first bracket 20 and a second bracket 21; the first bracket 20 fixes the first heater 112; the second bracket 21 fixes the second heater 17. The first bracket 20 can be fixed. Furthermore, the second bracket 21 is connected to an external rotating mechanism (not shown) and an external lifting mechanism (not shown) so as to be able to rotate and rise simultaneously during crystal growth, so that the liquid level in the crystal growth crucible 13 is within the range heated by the second device 17, and the rotation of the crystal growth crucible 13 is opposite to the rotation of the lifting rod 15. For example, during the growth of gallium antimonide crystals, the crystal growth crucible 13 and the lifting rod 15 maintain opposite rotation speeds, the rotation speed of the crystal growth crucible 13 is 1rpm, and the rotation speed of the lifting rod 15 is 3rpm. Refer to Figure 1 In one example, the furnace body 16 includes a top cover 161 , a middle cylinder 162 and a base 163 which are arranged in sequence from top to bottom. The top cover 161 and the middle cylinder 162 are detachably assembled via screws 164 , and the middle cylinder 162 and the base 163 are detachably assembled via screws 164 .

[0050] [Gallium Antimonide Crystal Growth Method]

[0051] Reference Figure 1 According to the present invention, the gallium antimonide crystal growth method comprises the steps of:

[0052] S1, GaSb polycrystal, dopant and liquid sealing agent are loaded into the crystal growth crucible 13 in the furnace body 16 of the GaSb crystal growth device 100, wherein the liquid sealing agent is NaCl+KCl mixed solid particles;

[0053] S2, loading the liquid sealing agent NaCl+KCl solid particles into the feeding crucible 111;

[0054] S3, vacuuming, degassing, and leak detection;

[0055] S4, filling the furnace body 16 with nitrogen until the pressure in the furnace body 16 reaches 0.1 MPa, and then stopping filling the furnace body 16;

[0056] S5, raising the temperature to make the temperature of the crystal growth crucible 13 reach the melting temperature of the gallium antimonide polycrystal, and the temperature of the feed crucible 111 reach the melting temperature;

[0057] S6, after the temperature is stabilized, the seed crystal rod 15 drives the seed crystal 14 to extend under the liquid sealant on the surface of the crystal growth crucible 13, and the liquid seal Czochralski method is started to grow the crystal;

[0058] S7, as the crystal growth proceeds, the flow switch 114 is adjusted to allow the liquid sealing agent in the feed crucible 111 to continuously flow into the crystal growth crucible 13.

[0059] The flow rate L of the liquid sealing agent, the pulling speed V of the crystal, the diameter d of the crystal during the pulling process, and the inner diameter D of the crystal growth crucible 13 have the following relationship:

[0060]

[0061] S8, after the crystal growth is completed, the crystal growth crucible 13 starts a cooling procedure, and until the cooling is completed, the feeding crucible 111 stops replenishing the liquid sealing agent to the crystal growth crucible 13;

[0062] S9, evacuating the furnace body 16 and injecting air, then opening the furnace body 16 and cutting the crystal rod off the lifting rod 15.

[0063] In the gallium antimonide crystal growth method according to the present disclosure, the liquid sealing agent is arranged in the crystal growth crucible 13 in step S1, the feeding crucible 111 for replenishing the liquid sealing agent is arranged in step S2, and the temperature of the feeding crucible 111 is increased in step S5 to form a stable NaCl+KCl liquid sealing agent melt. In step S7, the liquid sealing agent is continuously replenished from the feeding crucible 111 to the crystal growth crucible 13. In this way, during the entire process of growing gallium antimonide crystals by the liquid-sealed Czochralski method, the thickness of the liquid sealing agent (i.e., the thickness of the liquid sealing agent in the crystal growth crucible 13) can be achieved to not only reduce the volatilization of the Sb element but also reduce the temperature gradient during crystal growth and cooling, and reduce crystal dislocations.

[0064] In addition, the gallium antimonide crystal growth method according to the present disclosure may adopt the aforementioned gallium antimonide crystal growth device 100 . The specific structure, effect, and operation of the gallium antimonide crystal growth device 100 are described above and will not be repeated here.

[0065] In one example, in step S1, the initial thickness of the liquid sealant in the crystal growth crucible 13 is 10 mm. For example, in step S1, in the crystal growth crucible 13, the liquid sealant is finally spread on the gallium antimonide polycrystal and the dopant, so as to minimize the time for the liquid sealant to absorb moisture. In step S1, for example, the dopant is gallium telluride, and the mass fraction of the dopant relative to the gallium antimonide polycrystal is 10-100 ppm.

[0066] For example, in step S1 and step S2, the molar ratio of NaCl to KCl is 1:1.

[0067] In one example, step S3 is to evacuate the furnace body 16 and fill the furnace body 16 with nitrogen alternately 2-3 times by using a vacuum pump, the vacuum pressure is 10Pa, and nitrogen is used for the gas removal.

[0068] In one example, in step S5, the temperature of the crystal growth crucible 13 reaches 712° C., and the temperature of the feed crucible 111 is the same as the temperature of the crystal growth crucible 13. The temperature of the feed crucible 111 is the same as the temperature of the crystal growth crucible 13. When the feed crucible 111 replenishes the liquid sealing agent to the crystal growth crucible 13, the temperature of the replenished liquid sealing agent will not affect the temperature fluctuation of the crystal growth crucible 13.

[0069] In one example, in step S6 , the temperature is stabilized for 10 hours.

[0070] In step S7, for example, the flow switch 114 is a pipeline flow meter and is in communication connection with the controller 12. For example, in step S7, the pulling speed V of the crystal is determined by measuring the speed of the lifting rod 15 by a tachometer (not shown), and the diameter d of the crystal during the pulling process and the inner diameter D of the crystal growth crucible 13 are monitored by an infrared measuring instrument (not shown). In one example, during the growth of gallium antimonide crystals, the crystal growth crucible 13 and the lifting rod 15 maintain opposite rotation speeds, the rotation speed of the crystal growth crucible 13 is 1 rpm, the rotation speed of the lifting rod 15 is 3 rpm, and the seed crystal 14 is a gallium antimonide single crystal with a purity of 6N.

[0071] [test]

[0072] Example 1

[0073] Example 1 adopts the above and Figure 1 In the gallium antimonide crystal growth device 100 with the entire structure, the lifting rod 15 is connected to the corresponding rotating mechanism (not shown) and the corresponding lifting mechanism (not shown), the first bracket 20 is fixed, and the second bracket 21 is connected to the external rotating mechanism (not shown) and the external lifting mechanism (not shown).

[0074] The gallium antimonide crystal growth method of Example 1 adopts the following steps:

[0075] S1, GaSb polycrystal, dopant and liquid sealing agent are loaded into the crystal growth crucible 13 in the furnace body 16 of the GaSb crystal growth device 100, the dopant is GaTe, the mass fraction of the dopant relative to the GaSb polycrystal is 50ppm, the liquid sealing agent is NaCl+KCl mixed solid particles, the molar ratio of NaCl to KCl is 1:1, the liquid sealing agent is finally spread on the GaSb polycrystal and the dopant, and the initial thickness of the liquid sealing agent in the crystal growth crucible 13 is 10mm;

[0076] S2, loading the liquid sealing agent NaCl+KCl solid particles into the feeding crucible 111, wherein the molar ratio of NaCl to KCl is 1:1;

[0077] S3, vacuuming, degassing, and leak detection, vacuuming the furnace body 16 through the vacuuming interface 18 by a vacuum pump and filling the furnace body 16 with nitrogen through the gas inlet 19, alternately 2-3 times, the vacuuming pressure is 10Pa, and nitrogen is used for degassing;

[0078] S4, nitrogen is charged into the furnace body 16 through the gas inlet 19 to make the pressure in the furnace body 16 reach 0.1 MPa (monitored by a pressure gauge (not shown)), and the charging of the furnace body 16 is stopped;

[0079] S5, the second heater 17 and the first heater 112 are heated to make the temperature of the crystal growth crucible 13 reach the melting temperature of gallium antimonide polycrystal 712°C, and the temperature of the feed crucible 111 reaches the melting temperature, the temperature of the feed crucible 111 is the same as the temperature of the crystal growth crucible 13 (i.e., both are 712°C), the first heater 112 and the second heater 17 both include: a graphite heater T1, a graphite double-layer insulation cover T2 and a carbon felt T3; the graphite heater T1 is arranged around a corresponding one of the crystal growth crucible 13 and the feed crucible 111, the graphite double-layer insulation cover T2 is arranged around the graphite heater T1, the graphite double-layer insulation cover T2 includes an inner layer T21 and an outer layer T22, and the carbon felt T3 is filled between the inner layer T21 and the outer layer T22 of the graphite double-layer insulation cover T2;

[0080] S6, after the temperature is stable for 10 hours, the seed crystal rod 15 drives the seed crystal 14 to extend under the liquid sealant on the surface of the crystal growth crucible 13, and the liquid seal Czochralski method is started to grow the crystal. The seed crystal 14 is a gallium antimonide single crystal with a purity of 6N;

[0081] S7, as the crystal growth proceeds, the flow switch 114 is adjusted so that the liquid sealing agent in the feeding crucible 111 is continuously replenished and flows into the crystal growth crucible 13 via the pipeline 113. The flow switch 114 is a pipeline flow meter and is in communication connection with the controller 12. The flow switch 114 controls the flow of the sealing agent;

[0082] The flow rate L of the liquid sealing agent, the pulling speed V of the crystal, the diameter d of the crystal during the pulling process, and the inner diameter D of the crystal growth crucible 13 have the following relationship:

[0083]

[0084] The pulling speed V of the crystal is determined by measuring the speed of the pulling rod 15 with a speed meter, and the diameter d of the crystal and the inner diameter D of the crystal growth crucible 13 during the pulling process are monitored by an infrared measuring instrument;

[0085] During the growth of GaSb crystals, the crystal growth crucible 13 and the lifting rod 15 maintain opposite rotation speeds, the rotation speed of the crystal growth crucible 13 is 1 rpm, and the rotation speed of the lifting rod 15 is 3 rpm;

[0086] S8, after the crystal growth is completed, the crystal growth crucible 13 starts a cooling procedure, and until the cooling is completed, the feeding crucible 111 stops replenishing the liquid sealing agent to the crystal growth crucible 13;

[0087] S9, evacuate the furnace body 16 through the vacuum port 18 and inject air through the air inlet 19, then open the furnace body 16 and cut the crystal rod off the lifting rod 15.

[0088] Comparative Example 1

[0089] Except that the GaSb crystal growth device 100 does not have the liquid sealing agent replenishing mechanism 11 and the first bracket 20, the GaSb crystal growth method does not have step S2, step S5 does not have the heating of the crucible 111, and step S7 and step S8 do not need the operation of the crucible 111, the rest is the same as Example 1. That is, Comparative Example 1 does not use the liquid sealing agent replenishing means in terms of the device or the method.

[0090] Figure 2 This is the EPD distribution diagram of the GaSb crystal slice of Example 1 after dislocation EPD scanning. Figure 3 This is an EPD distribution diagram after dislocation EPD scanning of the GaSb crystal slice of Comparative Example 1. The GaSb crystal slice is made from the obtained crystal rod.

[0091] from Figure 2 It can be seen that the average dislocation in the crystal is 1 / cm 2 ;from Figure 3 It can be seen that the average dislocation in the crystal is 321 / cm 2 .

[0092] The above detailed description is used to describe multiple exemplary embodiments, but this document is not intended to be limited to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined together to form multiple additional combinations that are not shown for the sake of simplicity.

Claims

1. A gallium antimonide crystal growth device, characterized in that: The gallium antimonide crystal growing device (100) comprises a liquid sealing agent replenishing mechanism (11), which is used to replenish a corresponding amount of NaCl+KCl liquid sealing agent melt as the crystal grows when a gallium antimonide crystal is grown by a liquid sealing Czochralski method.

2. The gallium antimonide crystal growth device according to claim 1, characterized in that: The gallium antimonide crystal growth device (100) also includes a controller (12) and a crystal growth crucible (13); The crystal growth crucible (13) is used to load gallium antimonide polycrystals and initial NaCl+KCl liquid sealing agent; The liquid sealing agent replenishing mechanism (11) comprises a material replenishing crucible (111), a first heater (112), a pipeline (113), and a flow switch (114). The feeding crucible (111) is used to load NaCl+KCl to supplement the liquid sealing agent; The first heater (112) is used to increase the temperature of the feeding crucible (111) to form a supplementary liquid sealing agent melt and to reduce the temperature of the feeding crucible (111); One end of the pipe (113) is connected to the feeding crucible (111) and the other end is located above the crystal growth crucible (13) so that the pipe (113) is used to replenish the molten supplementary liquid sealing agent melt in the feeding crucible (111) into the crystal growth crucible (13) during the process of growing gallium antimonide crystals by the liquid sealing Czochralski method; The flow switch (114) is disposed on the pipeline (113) and is communicatively connected to the controller (12) to control the flow of the supplementary liquid sealing agent transported through the pipeline (113).

3. The gallium antimonide crystal growth device according to claim 2, characterized in that: The crystal growth crucible (13) is also initially charged with dopants.

4. The gallium antimonide crystal growth device according to claim 2, characterized in that: The flow switch (114) is a pipeline flow meter.

5. The gallium antimonide crystal growth device according to claim 4, characterized in that: The gallium antimonide crystal growth device (100) further comprises a speed meter and an infrared measuring instrument. The speed meter is used to measure the pulling speed of the crystal, and the speed meter is communicatively connected to the controller (12); The infrared measuring instrument is used to monitor the diameter of the crystal and the inner diameter of the crystal growth crucible (13) during the pulling process, and the infrared measuring instrument is communicatively connected to the controller (12).

6. A method for growing gallium antimonide crystals, characterized in that: Includes steps: S1, loading gallium antimonide polycrystals, dopants and liquid sealing agents into a crystal growth crucible (13) in a furnace body (16) of a gallium antimonide crystal growth device (100), wherein the liquid sealing agent is a NaCl+KCl mixed solid particles; S2, loading the liquid sealing agent NaCl+KCl solid particles into the feeding crucible (111); S3, vacuuming, degassing, and leak detection; S4, filling the furnace body (16) with nitrogen until the pressure in the furnace body (16) reaches 0.1 MPa, and then stopping filling the furnace body (16); S5, raising the temperature so that the temperature of the crystal growth crucible (13) reaches the melting temperature of the gallium antimonide polycrystal, and the temperature of the feed crucible (111) reaches the melting temperature; S6, after the temperature is stabilized, the seed crystal rod (15) drives the seed crystal (14) to extend under the liquid sealant on the surface of the crystal growth crucible (13), and the liquid seal Czochralski method is started to grow the crystal; S7, as the crystal growth proceeds, the flow switch (114) is adjusted to allow the liquid sealing agent in the feed crucible (111) to continuously flow into the crystal growth crucible (13), The flow rate L of the liquid sealing agent, the pulling speed V of the crystal, the diameter d of the crystal during the pulling process, and the inner diameter D of the crystal growth crucible (13) have the following relationship: S8, after the crystal growth is completed, the crystal growth crucible (13) starts a cooling procedure, and until the cooling is completed, the feeding crucible (111) stops replenishing the liquid sealing agent to the crystal growth crucible (13); S9, evacuate the furnace body (16) and inject air, then open the furnace body (16) and cut the crystal rod off the lifting rod (15).

7. The gallium antimonide crystal growth method according to claim 6, characterized in that: In step S1, the initial thickness of the liquid sealant in the crystal growth crucible (13) is 10 mm; and / or In step S1, in the crystal growth crucible (13), the liquid sealing agent is finally spread on the gallium antimonide polycrystal and the dopant; and / or In step S1, the dopant is gallium telluride, and the mass fraction of the dopant relative to the gallium antimonide polycrystal is 10-100 ppm; in step S1 and step S2, the molar ratio of NaCl to KCl is 1:

1.

8. The gallium antimonide crystal growth method according to claim 6, characterized in that: Step S3 is: Vacuuming and degassing The furnace body (16) is evacuated by a vacuum pump and nitrogen is filled into the furnace body (16) alternately 2-3 times. The vacuuming reaches a pressure of 10Pa, and nitrogen is used for degassing.

9. The gallium antimonide crystal growth method according to claim 6, characterized in that: In step S5, the temperature of the crystal growth crucible (13) reaches 712° C., and the temperature of the feed crucible (111) is the same as the temperature of the crystal growth crucible (13); In step S6, the temperature is stabilized for 10 h.

10. The gallium antimonide crystal growth method according to claim 6, characterized in that: The flow switch (114) is a pipeline flow meter and is communicatively connected to the controller (12); and / or In step S7, the pulling speed V of the crystal is determined by measuring the speed of the pulling rod (15) with a speed meter, and the diameter d of the crystal and the inner diameter D of the crystal growth crucible (13) during the pulling process are monitored by an infrared measuring instrument.

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