Gallium antimonide single crystal growth apparatus and method

CN122833719APending Publication Date: 2026-09-29INST OF SEMICONDUCTORS - CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202510340182.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-21
Publication Date
2026-09-29

AI Technical Summary

Technical Problem

现有热场结构在维持大尺寸生长所需的温度梯度控制方面存在显著不足:纵向热流分布失衡加剧熔体对流紊乱,导致固液界面产生周期性振荡,直接影响晶体等径控制精度;横向温度场对称性失稳造成径向热应力积聚,在超过150mm的晶体截面内形成超过材料断裂强度的应力梯度,致使位错密度大幅增长

Benefits of technology

[0015]与现有技术相比较,本发明实施例所提供的大尺寸锑化镓单晶生长设备和方法,生长设备相对简单,便于随时观察坩埚内晶体生长情况,以及时调整晶体生长参数;基于该锑化镓单晶生长设备,通过在坩埚的侧壁和底部设置加热装置,籽晶夹和坩埚的侧壁之间设置热屏,炉壁、籽晶杆和坩埚杆等区域设置冷却管道等设计能够在晶体生长时形成合适的生长温度梯度,有效改善纵向热流分布失衡和横向温度场对称性失稳问题,从而生长出低位错密度、均匀性好的2-6英寸的锑化镓单晶。

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Abstract

This invention provides a gallium antimonide single crystal growth apparatus and method, which can be used to grow 2-6 inch gallium antimonide single crystals. The gallium antimonide single crystal growth apparatus includes: a furnace body, comprising a crucible rod, a seed crystal rod, and a seed crystal clamp, wherein the crucible rod is fixed to the bottom of the furnace body, the seed crystal rod is fixed to the top of the furnace body, and the seed crystal rod is connected to the seed crystal clamp; a crucible, supported in the furnace body by the crucible rod, with the opening of the crucible close to the seed crystal clamp; a heating device, disposed on the outside of the crucible, used to heat the sidewalls and bottom of the crucible; a heat preservation device, having an internal heat preservation space, wherein the crucible, the heating device, and the seed crystal clamp are located within the heat preservation space, and the heat preservation device includes a heat shield, which is located between the seed crystal clamp and the sidewall of the crucible; and multiple cooling pipes disposed in at least one of the furnace wall, the seed crystal rod, and the crucible rod.
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Description

Technical Field

[0001] This invention relates to the field of single crystal preparation technology, specifically to a gallium antimonide single crystal growth apparatus and method. Background Technology

[0002] Gallium antimonide (GaSb) is a typical III-V compound semiconductor material. Due to its narrow bandgap (0.726 eV), high electron mobility, and good lattice matching with other III-V materials, it has significant application value in infrared detection, semiconductor lasers, and high-frequency electronic devices, making it one of the most important materials in the semiconductor device field. Large-size, high-quality gallium antimonide single crystals are key materials for high-performance, large-scale infrared detectors with more than one million pixels. At the same time, large-size single-crystal substrates can effectively improve material utilization and reduce the manufacturing cost of semiconductor devices.

[0003] Currently, mature gallium antimonide single crystal growth technologies in the industry are mainly geared towards 2-4 inch crystal fabrication. When attempting to break through to the 6-inch scale, the limitations of traditional thermal field design become a core constraint. Existing thermal field structures have significant shortcomings in maintaining the temperature gradient control required for large-size growth: longitudinal heat flow imbalance exacerbates melt convection turbulence, leading to periodic oscillations at the solid-liquid interface, directly affecting the accuracy of crystal diameter control; transverse temperature field symmetry instability causes radial thermal stress accumulation, forming a stress gradient exceeding the material's fracture strength within a crystal cross-section exceeding 150 mm, resulting in a significant increase in dislocation density. This thermo-mechanical coupling instability phenomenon leads to a cracking rate of over 75% in 6-inch crystal growth experiments using traditional thermal field schemes, with the effective crystallization length less than 1 / 3 of the standard ingot. Therefore, reconstructing a gradient-controllable thermal field system adapted to large-size growth and designing one suitable for large-size growth processes have become the primary technological breakthroughs for achieving the commercial fabrication of 6-inch gallium antimonide single crystals. Summary of the Invention

[0004] In view of this, the present invention provides a gallium antimonide single crystal growth apparatus and method, which can achieve high-quality, large-size, commercially viable gallium antimonide single crystal growth.

[0005] This invention provides a gallium antimonide single crystal growth apparatus, comprising: a furnace body, including a crucible rod, a seed crystal rod, and a seed crystal clamp, wherein the crucible rod is fixed to the bottom of the furnace body, the seed crystal rod is fixed to the top of the furnace body, and the end of the seed crystal rod is connected to the seed crystal clamp; a crucible, supported in the furnace body by the crucible rod, with the opening of the crucible close to the seed crystal clamp; a heating device, disposed on the outside of the crucible, used to heat the sidewalls and bottom of the crucible; a heat preservation device, having a heat preservation space formed inside, wherein the crucible, the heating device, and the seed crystal clamp are located within the heat preservation space, the heat preservation device including a heat shield, the heat shield being located between the seed crystal clamp and the sidewall of the crucible; and multiple cooling pipes disposed in at least one of the furnace wall, the seed crystal rod, and the crucible rod.

[0006] According to an embodiment of the present invention, the crucible includes: a quartz crucible forming the inner wall of the crucible, the quartz crucible having a uniform thickness; and a graphite crucible forming the outer wall of the crucible, the thickness of the side wall of the graphite crucible being equal to the thickness of the quartz crucible, and the thickness of the bottom of the graphite crucible being greater than the thickness of the quartz crucible.

[0007] According to an embodiment of the present invention, the inner diameter of the quartz crucible is 200~350mm, the depth is 150~160mm, and the thickness is 3~5mm.

[0008] According to an embodiment of the present invention, the heating device includes: a first heater having a serpentine structure, the first heater surrounding the side wall of the crucible; a second heater having an annular structure, the second heater being disposed at the bottom of the crucible, and the second heater and the first heater being controlled by different power supplies.

[0009] According to an embodiment of the present invention, the heating device further includes: a graphite plate fixed to the bottom of the furnace body, a first heater, a second heater and a heat preservation device placed on the graphite plate; a plurality of electrodes uniformly embedded in the graphite plate, the plurality of electrodes being connected to the corresponding first heater and second heater, and each electrode having a cooling pipe.

[0010] According to an embodiment of the present invention, the heat preservation device includes: a graphite cover for enclosing the crucible, heating device and seed crystal in the heat preservation space; a heat screen in the shape of a funnel, the small opening of the heat screen extending into the interior of the crucible, and the large opening of the heat screen being movably connected to the top of the graphite cover, so that the heat screen and the surface of the free melt in the crucible maintain a relatively fixed distance during the rising or falling process.

[0011] According to an embodiment of the present invention, the interior of the graphite cover is filled with heat-insulating carbon felt, and the surface of the heat shield is coated with an anti-oxidation coating.

[0012] According to an embodiment of the present invention, the distance between the bottom of the heat shield and the surface of the free melt in the crucible is 10~15mm, and the tilt angle of the heat shield is 45°~60°.

[0013] According to an embodiment of the present invention, the cooling medium in the cooling pipe includes cooling water, the flow rate of the cooling water is 20~25L / min, and the inlet temperature is 24~28℃.

[0014] In another aspect, the present invention provides a gallium antimonide single crystal growth method, which is implemented using the gallium antimonide single crystal growth equipment of any of the above embodiments.

[0015] Compared with existing technologies, the large-size gallium antimonide single crystal growth equipment and method provided in this invention have relatively simple growth equipment, which facilitates observation of crystal growth in the crucible at any time and timely adjustment of crystal growth parameters. Based on this gallium antimonide single crystal growth equipment, by setting heating devices on the side wall and bottom of the crucible, setting a heat shield between the seed crystal clamp and the side wall of the crucible, and setting cooling pipes in areas such as the furnace wall, seed crystal rod and crucible rod, a suitable growth temperature gradient can be formed during crystal growth, effectively improving the problems of imbalance in longitudinal heat flow distribution and instability in lateral temperature field symmetry, thereby growing 2-6 inch gallium antimonide single crystals with low dislocation density and good uniformity. Attached Figure Description

[0016] The above and other objects, features and advantages of the present invention will become more apparent from the following description of embodiments of the invention with reference to the accompanying drawings, in which:

[0017] Figure 1 A schematic diagram of a gallium antimonide single crystal growth apparatus according to an embodiment of the present invention is shown.

[0018] Figure 2 A schematic diagram of the structure of a first heater according to an embodiment of the present invention is shown;

[0019] Figure 3 A schematic diagram of the structure of a second heater according to an embodiment of the present invention is shown;

[0020] Figure 4 A schematic diagram of a cooling pipe according to an embodiment of the present invention is shown.

[0021] Figure 5 A flowchart illustrating a gallium antimonide single crystal growth method according to an embodiment of the present invention is shown. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments and the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0023] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention. The terms “comprising,” “including,” etc., as used herein indicate the presence of features, steps, operations, and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, or components.

[0024] In the description of this invention, it should be understood that the terms "longitudinal", "length", "circumferential", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the subsystem or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0025] Throughout the accompanying drawings, identical elements are represented by the same or similar reference numerals. Conventional structures or configurations may be omitted where they might cause confusion in understanding the invention. Furthermore, the shapes, sizes, and positional relationships of the components in the drawings do not reflect actual size, scale, or actual positional relationships. Additionally, any reference numerals placed between parentheses in the claims should not be construed as limiting the claims.

[0026] Figure 1 A schematic diagram of a gallium antimonide single crystal growth apparatus according to an embodiment of the present invention is shown.

[0027] like Figure 1 As shown, the gallium antimonide single crystal growth equipment may include a furnace body 10, a crucible 20, a heating device 30, a heat preservation device 40, and multiple cooling pipes 50.

[0028] The furnace body 10 may include a crucible rod 11, a seed crystal rod 12, and a seed crystal clamp 13. The crucible rod 11 is fixed to the bottom of the furnace body 10, and the seed crystal rod 12 is fixed to the top of the furnace body 10. The end of the seed crystal rod 12 is connected to the seed crystal clamp 13. The crucible rod 11 supports the crucible 20 inside the furnace body 10. The opening of the crucible 20 is close to the seed crystal clamp 13, allowing the seed crystal clamp 13 to extract the gallium antimonide single crystal grown in the crucible 20. In this embodiment, the gallium antimonide single crystal is generated using the liquid-sealed Czochralski method, and this growth process will be described in detail later. In some embodiments, the seed crystal rod 12 and the crucible rod 11 may be connected to a lifting drive device, which can raise and lower the position of the crucible 20 according to the crystal length and the remaining melt, thereby improving the crystal extraction efficiency. A heating device 30 is disposed on the outer side wall and bottom of the crucible 20. The heating device 30 is used to heat the side wall and bottom of the crucible 20 to ensure the temperature required for crystal growth. The heat preservation device 40 has an internal heat preservation space, within which the crucible 20, heating device 30, and seed crystal clamp 13 are located. The heat preservation device 40 includes a heat shield 42, located between the seed crystal clamp 13 and the side wall of the crucible 20. Multiple cooling pipes 50 are disposed in at least one of the furnace wall of the furnace body 10, the seed crystal rod 12, and the crucible rod 11. For example, a cooling pipe 51 can be disposed between the inner furnace wall 15 and the outer furnace wall 14 of the furnace body 10, a cooling pipe 52 can be disposed in the seed crystal rod 12, and a cooling pipe 53 can be disposed in the crucible rod 11, respectively, to cool the furnace body 10, the seed crystal rod 12, and the crucible rod 11.

[0029] The gallium antimonide single crystal growth equipment provided in this embodiment is relatively simple. The crystal growth process within the crucible can be observed at any time through an observation window, allowing for timely adjustments to the crystal growth parameters. Based on this gallium antimonide single crystal growth equipment, by incorporating heating devices on the sidewalls and bottom of the crucible, a heat shield between the seed crystal clamp and the crucible sidewalls, and cooling pipes in the furnace wall, seed crystal rod, and crucible rod areas, a suitable growth temperature gradient can be formed during crystal growth. This effectively improves the imbalance in longitudinal heat flow distribution and the instability of lateral temperature field symmetry, thereby growing 2-6 inch gallium antimonide single crystals with low dislocation density and good uniformity.

[0030] Please continue reading. Figure 1 The crucible 20 may include a quartz crucible 21 and a graphite crucible 22. The quartz crucible 21 forms the inner wall of the crucible 20 and has a uniform thickness. The graphite crucible 22 forms the outer wall of the crucible 20, with the sidewall thickness equal to that of the quartz crucible 21, and the bottom thickness of the graphite crucible 22 greater than that of the quartz crucible 21. In some embodiments, the inner diameter of the quartz crucible 21 may be 200-350 mm, the depth may be 150-160 mm, and the thickness may be 3-5 mm, facilitating the growth of 2-6 inch gallium antimonide single crystals. Correspondingly, the sidewall thickness of the graphite crucible 22 may also be 3-5 mm to ensure uniform heating.

[0031] Figure 2 A schematic diagram of the structure of a first heater according to an embodiment of the present invention is shown; Figure 3 A schematic diagram of the structure of a second heater according to an embodiment of the present invention is shown.

[0032] Please continue reading. Figure 1 , Figure 2 and Figure 3 The heating device 30 may include a first heater 31 and a second heater 32.

[0033] like Figure 1 and Figure 2 As shown, the first heater 31 may have a serpentine structure, and the first heater 31 surrounds the sidewall of the crucible 20. For example... Figure 2 As shown, the first heater 31 may be equipped with a temperature-controlled thermocouple K1, and the heating method may be resistance heating. As an example, the inner diameter of the first heater 31 may be 220~380mm, the height may be 250~300mm, and the thickness may be 10~15mm. The first heater 31 can be considered as the main heater of the crystal growth equipment.

[0034] like Figure 1 and Figure 3 The second heater 32 can have a ring structure and is positioned at the bottom of the crucible 20. Understandably, the crucible rod 11 can pass through the central hole K2 of the second heater 32. The ring around the central hole K2 provides the required temperature to the bottom of the crucible 20. The second heater 32 can be considered an auxiliary heater in the crystal growth apparatus. As the crucible 20 moves up and down to generate crystals, the distance between the second heater 32 and the bottom of the crucible 20 changes accordingly. For example, the second heater 32 can be placed 10-20 mm below the crucible 20, with a thickness of 10-15 mm and a ring width of 120-180 mm. The second heater 32 and the first heater 31 can be controlled by different power supplies, achieving more precise temperature control through both main and auxiliary heaters. For example, the second heater 32 can be controlled by an independent power supply with a fixed power of 5-8 kW.

[0035] Please continue reading. Figures 1 to 3 The heating device 30 may further include a graphite plate 33 and multiple electrodes 34. The graphite plate 33 is fixed to the bottom of the furnace body 10, and the first heater 31, the second heater 32, and the heat preservation device 40 are placed on the graphite plate 33. Multiple electrodes 34 are evenly embedded in the graphite plate 33, and each electrode 34 is connected to a corresponding first heater 31 and second heater 32. For example, two electrodes 34 are connected to each of the first heater 31 and the second heater 32. In other words, the number of electrodes on the graphite plate 33 can be four. Figure 1 As shown, each electrode 34 can be connected to a cooling pipe 54 to cool the electrode 34.

[0036] Please continue reading. Figure 1 The heat preservation device 40 may further include a graphite cover 41. The graphite cover 41 can be a hollow cylindrical structure used to enclose the crucible 20, heating device 30, and seed crystal clamp 13 within the heat preservation space. The heat shield 42 can be funnel-shaped, with its large opening (i.e., the large opening of the funnel) movably fixed to the top of the graphite cover 41, and its small opening (i.e., the small opening of the funnel) extending into the interior of the crucible 20. The heat shield 42's movable connection to the top of the graphite cover 41 allows it to maintain a relatively fixed distance from the free melt surface in the crucible 20 during its rise or fall. In other words, the heat shield 42 can rise or fall synchronously with the free melt surface. This improves the radial temperature gradient and maintains a good interface morphology during the crystal growth process.

[0037] In some embodiments, the graphite cover 41 is filled with insulating carbon felt 43 for heat preservation. The inner diameter of the graphite cover 41 can be 260~420mm, and the width can be 15~20mm. The surface of the heat shield 42 can be coated with an anti-oxidation coating to improve oxidation resistance and extend service life. In some embodiments, the heat shield 42 surrounding the crystal can be designed to follow up, so that it is always 10~15mm above the free melt surface and tilted at an angle of 45°~60°. As an example, the follow-up design can be implemented by a lifting device for the heat shield 42. That is, the heat preservation device 40 can also include a lifting device for the heat shield 42. The present invention does not limit the specific type of lifting device, as long as it meets the requirements for precise lifting of the heat shield 42.

[0038] Figure 4 A schematic diagram of a cooling pipe 50 according to an embodiment of the present invention is shown.

[0039] like Figure 1 and Figure 4 As shown, the cooling medium in cooling pipes 51, 52, 53, and 54 can be cooling water. In the cooling pipe 51 built into the furnace wall, cooling water can enter from the bottom and exit from the top. The cooling circuits of cooling pipes 52, 53, and 54 in the seed crystal rod 12, electrode 34, and crucible rod 11 can be as follows: Figure 4 As shown, cooling water enters through the central pipe and exits through the side outlet. Throughout the crystal growth process, the cooling water flow rate can be 20~25 L / min, and the inlet temperature can be 24~28℃. By controlling the cooling water flow rate and temperature, the temperature changes inside the furnace can be controlled more precisely, resulting in the desired crystal.

[0040] Based on the gallium antimonide single crystal growth apparatus of the above embodiments, this invention also provides a corresponding gallium antimonide single crystal growth method. This gallium antimonide single crystal growth method can be implemented using the gallium antimonide single crystal growth apparatus of any of the above embodiments. Therefore, the gallium antimonide single crystal growth method has the same technical features and beneficial effects as the gallium antimonide single crystal growth apparatus, and will not be elaborated further here.

[0041] Figure 5 A flowchart illustrating a gallium antimonide single crystal growth method according to an embodiment of the present invention is shown.

[0042] like Figure 5 As shown, the gallium antimonide single crystal growth method may include steps S1 to S9.

[0043] In step S1, the dehydrated liquid sealant is obtained.

[0044] As an example, high-purity NaCl and KCl can be mixed in a 1:1 molar ratio and placed in a quartz crucible 20. The crucible 20 is then placed in a gallium antimonide single crystal growth apparatus, and the heating device 30 is turned on to heat to 550°C under vacuum conditions. Nitrogen gas is then filled in and maintained at one atmosphere. Heating continues to 950°C, then heating is stopped, and the temperature is maintained for 2 hours using a heat preservation device 40. After the NaCl and KCl mixture has completely melted and thoroughly mixed, it is cooled to 800°C through a cooling pipe 50. A vacuum pump is then turned on to evacuate the eutectic and maintain this state for 2 hours to remove as much water of crystallization as possible from the NaCl and KCl eutectic. The heating device 30 is then turned off, allowing the furnace body 10 to cool naturally to room temperature. A protective nitrogen gas is then filled into the furnace body 10, and the dehydrated liquid sealant is removed.

[0045] In step S2, the dehydrated liquid sealant and the pre-prepared raw materials are placed in the crucible 20.

[0046] Before adding the liquid sealant and raw materials, the crucible 20 can be pre-treated. For example, a quartz crucible 21 can be cleaned and dried with aqua regia, or a graphite crucible 22 can be vacuum-calcined to remove impurities. High-purity Ga and Sb raw materials are precisely weighed at a molar ratio of Ga:Sb = 1:1.05, and then evenly and flatly spread at the bottom of the quartz crucible 21. The dehydrated liquid sealant is then placed on top of the mixed raw materials. The entire quartz crucible 21 is placed on the graphite crucible 22, and a 10mm × 10mm × 12mm square seed crystal is clamped using the seed crystal clamp 12 before sealing the single crystal growth equipment.

[0047] In step S3, the gallium antimonide single crystal growth equipment containing liquid sealant and raw materials is subjected to gas washing treatment.

[0048] As an example, a vacuum pump can be turned on to evacuate the gallium antimonide single crystal growth equipment until the gas pressure reaches 1×10⁻⁶. -3After reaching a pressure of 1.2 × 10⁻⁶ Pa, nitrogen gas is introduced; wait until the pressure reaches 1.2 × 10⁻⁶ Pa. 5 Pa, then turn on the vacuum pump to evacuate the gas, repeating this process multiple times until the furnace pressure stabilizes at 1×10 Pa. 5 Pa.

[0049] In step S4, the liquid sealant and raw materials after the gas washing are heated and melted to generate crystals from the raw materials.

[0050] As an example, after gas washing, the feedstock is heated and hydrogen is introduced at a rate of 200 mL / min to reduce oxides and impurities in the furnace before the liquid sealant melts. Simultaneously, the exhaust valve can be opened to allow impurities to be expelled from the furnace with the hydrogen. After the liquid sealant has completely melted, the furnace pressure is controlled at 1.5 × 10⁻⁶. 5 Pa, stop the hydrogen supply and close the exhaust valve; raise the temperature of heating device 30 to 730℃, hold it for 1.5h through heat preservation device 40, and after the raw material mixture is completely melted, continue to raise the temperature to 740℃ and hold it for 1h to ensure that the raw material is completely melted and start the crystal growth process.

[0051] In step S5, the grown crystal is guided to form a crystal.

[0052] As an example, the seed crystal rod 12 can be slowly lowered to 15 mm above the melt in the crucible 20 for preheating for 10 minutes, stabilizing the seed crystal temperature at around the gallium antimonide melting point of 712°C. Then, it is lowered to contact the melt surface. Under good wetting conditions, the seed crystal is slowly pulled at a pulling rate of 12 mm / h. Simultaneously, the power of the first heater 31 is adjusted to control the temperature within the range of 725-730°C. As the seed crystal rises, the melt begins to crystallize at the point of contact with the seed crystal, growing small crystal segments with a diameter of approximately 5 mm and a length of 20 mm.

[0053] In step S6, the crystal is shouldered.

[0054] As an example, once the necking reaches the specified length, the crystal pulling rate is controlled at 10 mm / h within a temperature range of 720-730°C, allowing the crystal to begin growing to a diameter of 150 mm at a shoulder angle of 50°.

[0055] In step S7, the crystal is grown to the same diameter.

[0056] As an example, once the crystal diameter was observed to have increased to 150 mm in the observation window, the temperature was strictly controlled between 720-730 °C using the heating device 30. Simultaneously, the crystal pulling rate was fixed at 8 mm / h to prevent further increase in crystal diameter, thus initiating constant-diameter growth.

[0057] In step S8, the crystal is finished.

[0058] As an example, when the constant diameter growth reaches the point where the gallium antimonide melt is consumed in the variable diameter section of the quartz crucible 21, the power of the first heater 31 is increased, and the pulling rate is increased to 10 mm / h within the temperature range of 730-740°C, so that the crystal diameter becomes thinner until the crystal is completely pulled out of the melt. The crystal is then pulled 15 mm further away from the melt, and the power supply to the second heater 32 is turned off.

[0059] In step S9, the pulled-out crystal is annealed.

[0060] As an example, the crystal is further raised to 20 mm above the liquid surface and rotated at a rate of 2-3 r / min at 750°C for 2-2.5 h; the power of the first heater 31 is controlled to cool the crystal to 300°C at a cooling rate of 60°C / h and held for 1.5 h; the power of the first heater 31 is turned off and the crystal temperature is allowed to cool naturally to room temperature, and the grown crystal is then removed.

[0061] Compared with existing technologies, the large-size gallium antimonide growth process of this invention employs methods such as removing the liquid sealant's water of crystallization and introducing a hydrogen atmosphere to reduce oxide impurities. This effectively reduces the amount of oxide slag and Sb volatilization, significantly improving crystallization rate and crystal quality. The seeding process, to a certain extent, prevents dislocations in the seed crystal from extending into the pulled crystal material. The optimized shoulder-forming process reduces the probability of twin formation and the dislocation density in the head crystal. The annealing process achieves a low thermal stress distribution level in the crystal, reducing the probability of dislocation formation. The entire growth process controls heat exchange by adjusting the thermocouple temperature, improving the controllability of the large-size gallium antimonide crystal growth process.

[0062] It should be noted that the gallium antimonide single crystal growth equipment and method provided by this invention can be used to grow gallium antimonide single crystals, and can also be used to grow other similar crystals by changing the raw materials and process parameters. In other words, the growth of other crystals using the gallium antimonide single crystal growth equipment and method provided by this invention should also be included within the scope of protection of this invention.

[0063] The above specific embodiments further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A gallium antimonide single crystal growth apparatus, characterized in that, include: The furnace body includes a crucible rod, a seed crystal rod, and a seed crystal clamp. The crucible rod is fixed to the bottom of the furnace body, the seed crystal rod is fixed to the top of the furnace body, and the end of the seed crystal rod is connected to the seed crystal clamp. The crucible is supported in the furnace by the crucible rod, and the opening of the crucible is close to the seed crystal clamp. A heating device is disposed on the outside of the crucible, and the heating device is used to heat the side walls and bottom of the crucible; A heat preservation device has an internal heat preservation space. The crucible, the heating device, and the seed crystal clamp are located in the heat preservation space. The heat preservation device includes a heat shield, which is located between the side wall of the seed crystal clamp and the crucible. Multiple cooling pipes are provided in at least one of the furnace wall, the seed crystal rod, and the crucible rod.

2. The gallium antimonide single crystal growth apparatus according to claim 1, characterized in that, The crucible includes: A quartz crucible, forming the inner wall of the crucible, the quartz crucible having a uniform thickness; A graphite crucible forms the outer wall of the crucible, the thickness of the side wall of the graphite crucible is equal to the thickness of the quartz crucible, and the thickness of the bottom of the graphite crucible is greater than the thickness of the quartz crucible.

3. The gallium antimonide single crystal growth apparatus according to claim 2, characterized in that, The quartz crucible has an inner diameter of 200-350 mm, a depth of 150-160 mm, and a thickness of 3-5 mm.

4. The gallium antimonide single crystal growth apparatus according to claim 1, characterized in that, The heating device includes: A first heater, having a serpentine structure, surrounds the sidewall of the crucible; The second heater has a ring structure and is located at the bottom of the crucible. The second heater and the first heater are controlled by different power sources.

5. The gallium antimonide single crystal growth apparatus according to claim 4, characterized in that, The heating device also includes: A graphite plate is fixed to the bottom of the furnace body, and the first heater, the second heater, and the heat preservation device are placed on the graphite plate; Multiple electrodes are uniformly embedded in the graphite plate, and the multiple electrodes are connected to the corresponding first heater and second heater. Each electrode is provided with a cooling pipe.

6. The gallium antimonide single crystal growth apparatus according to claim 1, characterized in that, The heat preservation device also includes a graphite cover for enclosing the crucible, the heating device, and the seed crystal within the heat preservation space; The heat shield is funnel-shaped, with a small opening extending into the interior of the crucible and a large opening movably connected to the top of the graphite cover, so that the heat shield maintains a relatively fixed distance from the surface of the free melt in the crucible during its rising or falling process.

7. The gallium antimonide single crystal growth apparatus according to claim 6, characterized in that, The graphite cover is filled with heat-insulating carbon felt, and the surface of the heat shield is coated with an anti-oxidation coating.

8. The gallium antimonide single crystal growth apparatus according to claim 6, characterized in that, The bottom of the heat shield is 10-15 mm away from the surface of the free melt in the crucible, and the tilt angle of the heat shield is 45°-60°.

9. The gallium antimonide single crystal growth apparatus according to claim 1, characterized in that, The cooling medium in the cooling pipe includes cooling water, the flow rate of which is 20~25L / min and the inlet temperature is 24~28℃.

10. A method for growing gallium antimonide single crystals, characterized in that, The gallium antimonide single crystal growth method is implemented using the gallium antimonide single crystal growth equipment described in any one of claims 1 to 9.