Double-region synthesis device and method for InGaSb ternary alloy polycrystal

Abstract

The invention relates to the technical field of semiconductor material preparation, in particular to an InGaSb ternary alloy polycrystal double-zone synthesis device and method.The InGaSb ternary alloy polycrystal double-zone synthesis device comprises a synthesis cavity, a multi-section heater, a double-zone synthesis pipe, a synthesis cavity rotating mechanism and a synthesis cavity base; according to the invention, InGaSb polycrystal synthesis is carried out by adopting a double-region structure synthesis tube, firstly GaSb and InSb are synthesized in different temperature regions respectively, and then GaSb and InSb are fused to synthesize InGaSb. Compared with a method for synthesizing by directly adopting In, Ga and Sb elements, the method disclosed by the invention has the advantage that the element ratio in InGaSb can be effectively controlled by controlling the ratio of GaSb to InSb. And meanwhile, segregation of In in InGaSb in direct synthesis of In, Ga and Sb elements can be effectively avoided, and the uniformity of components is improved, so that the consistency of the material is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of semiconductor material preparation, in particular to a dual-zone synthesis device and method for InGaSb ternary alloy polycrystal. Background Art

[0002] Indium gallium antimony (InGaSb) is a ternary compound semiconductor material, considered a solid solution of InSb and GaSb. By varying the ratio of In to Ga, its bandgap and lattice constant can be tuned to lie between those of indium antimonide (InSb, bandgap: 0.17 eV, lattice constant: 0.64 nm) and gallium antimonide (GaSb, bandgap: 0.72 eV, lattice constant: 0.61 nm). Compared to GaSb and InSb, InGaSb crystals, as substrates, better match the lattices of ternary and quaternary compounds such as GaInSb, InAsSb, InGaAsSb, and AlGaAsSb. This makes it an ideal substrate for growing high-quality antimonide epitaxial materials, with significant potential applications in antimonide infrared lasers, detectors, and thermophotovoltaic cells.

[0003] InGaSb ternary polycrystalline alloys are the raw materials for growing InGaSb crystals. A suitably proportioned InGaSb polycrystalline alloy must first be synthesized, and then crystals are grown from this alloy using methods such as vertical directional solidification (VDS) and the Bridgman method (VB). Currently, InGaSb materials are primarily synthesized using In, Ga, and Sb elements via horizontal directional solidification or zone melting. Because the segregation coefficient of In in GaSb is only 0.2, far less than 1, In segregation can easily occur during the synthesis process, leading to imbalanced InGaSb ratios or significant compositional deviations. Therefore, we propose a dual-zone synthesis apparatus and method for InGaSb ternary alloy polycrystalline. Summary of the Invention

[0004] The object of the present invention is to provide a dual-zone synthesis device and method for InGaSb ternary alloy polycrystals to solve the problems raised in the above background technology.

[0005] To achieve the above-mentioned object, the present invention provides the following technical solutions: a dual-zone synthesis device for InGaSb ternary alloy polycrystals, comprising a synthesis cavity, a multi-segment heater, a dual-zone synthesis tube, a synthesis cavity rotation mechanism, and a synthesis cavity base; The synthesis cavity is used to support and fix the multi-stage heater and the dual-zone synthesis pipe and can be filled with inert gas to protect the synthesis device. The wall of the synthesis cavity is provided with a water cooling coil for cavity cooling; Each section of the multi-section heater is a resistance wire heater with independent temperature control and heating; A cooperating opening and closing mechanism is installed on the base of the synthesis cavity, and a barrier mechanism is provided on the dual-zone synthesis pipe. The barrier mechanism cooperates with the cooperating opening and closing mechanism to adjust the dual-zone synthesis pipe.

[0006] Furthermore, the dual-zone synthetic pipe includes a dual-zone synthetic pipe body and a dual-zone synthetic pipe cap, the dual-zone synthetic pipe body includes a dual-zone synthetic pipe synthesis zone 1, a dual-zone synthetic pipe necking zone and a dual-zone synthetic pipe synthesis zone 2, and the barrier mechanism is located at the dual-zone synthetic pipe necking zone; There are two double-zone synthetic pipe sealing caps, which are respectively welded to the openings of the double-zone synthetic pipe synthesis zone 1 and the double-zone synthetic pipe synthesis zone 2.

[0007] Furthermore, the synthetic cavity rotation mechanism includes a support shaft, a rotating shaft, a driving member and a swinging member. One end of the support shaft is rotatably connected to the bottom of the synthetic cavity, and the other end of the support shaft is fixedly connected to the synthetic cavity. The rotating shaft passes through the base of the synthetic cavity, and the rotating shaft is rotatably connected to the bottom of the synthetic cavity. The driving member is used to drive the rotating shaft, and the swinging member is installed at the other end of the rotating shaft. The swinging member is used to drive the synthetic cavity, and the synthetic cavity is rotationally driven by the provided synthetic cavity rotation mechanism.

[0008] Furthermore, the blocking mechanism includes a positioning rod, a first rotating sleeve, a second rotating sleeve, a closing plate and a reversing piece. One end of the positioning rod is fixedly connected to the inner wall of the necking area of the dual-zone synthetic pipe. The first rotating sleeve is rotatably sleeved on the outside of the positioning rod, and the first rotating sleeve is provided with a plurality of rotating grooves. The second rotating sleeve is provided with a plurality of second rotating sleeves, and the plurality of second rotating sleeves are respectively rotatably sleeved at the plurality of rotating grooves. There are two closing plates, and the two closing plates are respectively fixedly connected to the first rotating sleeve and the plurality of second rotating sleeves. One end of the first rotating sleeve extends to the outside of the necking area of the dual-zone synthetic pipe and is connected to the reversing piece, and one end of one of the second rotating sleeves extends to the necking area of the dual-zone synthetic pipe and is connected to the reversing piece. Through the blocking mechanism, the necking area of the dual-zone synthetic pipe is blocked.

[0009] Furthermore, the reversing member includes a movable plate, a pushing rod, a pushing plate and a limiting guide member. The movable plate is slidably connected to the outside of the necking area of the double-zone synthetic tube, and two pushing openings are provided on the movable plate. There are two pushing rods, and the two pushing rods slide through the pushing openings respectively. There are two pushing plates, and the two pushing plates are fixedly connected to the first rotating sleeve and the second rotating sleeve respectively, and the two pushing rods are fixedly connected to the two pushing plates respectively. The limiting guide member is installed on the outside of the necking area of the double-zone synthetic tube, and the limiting guide member is used to guide the movable plate, and through the provided reversing member, the function of synchronously driving one end of the first rotating sleeve and the second rotating sleeve is realized.

[0010] Furthermore, the limiting guide member includes a fixed rod, a fixed plate and a connecting spring. The fixed rod slides through one end of the movable plate, and both ends of the fixed plate are fixedly connected to the fixed plate, and the fixed plate is fixedly installed on the outside of the necking area of the dual-zone synthetic pipe. The connecting spring is sleeved on the outside of the fixed rod, and the two ends of the connecting spring are respectively fixedly connected to the movable plate and one of the fixed plates. Through the provided limiting guide member, the function of limiting and guiding the movable plate is realized.

[0011] Furthermore, the cooperative opening and closing mechanism includes a connecting sleeve, a synchronization block, a support adjustment member, a surrounding rod and a limit member. The connecting sleeve slides through one side of the synthetic cavity, and a connecting groove is provided on one end of the connecting sleeve close to the necking area of the dual-zone synthetic tube. The synchronization block is located in the connection groove and is fixedly connected to one end of the first rotating sleeve. The support adjustment member is located outside the synthetic cavity, and the support adjustment member is used to adjust the position of the connecting sleeve. One end of the surrounding rod is slidably connected to the inside of the connecting sleeve, and the other end of the surrounding rod is connected to the limit member. The limit member is connected to the base of the synthetic cavity, and the first rotating sleeve is driven by the cooperating opening and closing mechanism.

[0012] Furthermore, two raised strips are provided on the outside of the surrounding rod, and the connecting sleeve is provided with guide grooves at the positions corresponding to the two raised strips. The limiting member includes a limiting plate and a limiting rod. The limiting plate is fixedly installed on the end of the surrounding rod away from the connecting sleeve, and the limiting plate is slidably connected to the base of the synthetic cavity. The base of the synthetic cavity is provided with a limiting groove, and the limiting rod slides through the limiting groove. One end of the limiting rod is fixedly connected to the limiting plate, and the limiting rod deviates from the center of the limiting plate. The limiting member is provided to guide the surrounding rod.

[0013] Furthermore, the support adjustment member includes a support plate and an adjusting screw. One end of the support plate is rotatably sleeved on the outside of the connecting sleeve through a bearing, and a threaded hole is provided at the other end of the support plate. The adjusting screw passes through the threaded hole, and the adjusting screw is threadedly connected to the threaded hole. One end of the adjusting screw is rotatably connected to the outside of the synthetic cavity, and the connecting sleeve is adjusted through the support adjustment member.

[0014] A method for synthesizing an InGaSb ternary alloy polycrystal in a dual-zone synthesis device comprises the following steps: Step 1: weigh an appropriate amount of high-purity gallium and high-purity antimony in an atomic ratio of 1:1 and place them into a dual-zone synthesis tube to synthesize one zone; Step 2: weigh an appropriate amount of high-purity indium and high-purity antimony in an atomic ratio of 1:1 and load them into the second synthesis zone of the dual-zone synthesis tube; Step 3: Evacuate both ends of the dual-zone quartz tube and weld and seal them with the synthetic tube cap; Step 4: Place the sealed dual-zone quartz tube in the multi-segment heater in the synthesis chamber and fix it; Step 5: The purity of the high-purity gallium and high-purity antimony in step 1 is not less than 6N; the purity of the high-purity indium and high-purity antimony in step 2 is not less than 6N; the vacuum degree of the double-zone quartz tube in step 3 is less than 1×10-3Pa; Step 6: Control the multi-stage heater to heat up the first zone of the dual-zone synthesis tube to 800°C, and the second zone of the dual-zone synthesis tube to 600°C; Step 7: After the temperature of the first and second zones of the dual-zone synthesis tube is raised to the target temperature described in step 6, maintain the temperature for 3-5 hours to ensure sufficient synthesis; Step 8: The first synthesis zone of the dual-zone synthesis tube in step 6 is heated from room temperature to 800° C. at a heating rate of (5-10)° C. / min, and the second synthesis zone of the dual-zone synthesis tube in step 6 is heated from room temperature to 600° C. at a heating rate of (5-10)° C. / min; Step 9: The synthetic cavity is slowly rotated from a horizontal state to a vertical state by adjusting the synthetic cavity rotation mechanism that is connected to one end of the synthetic cavity and the cavity base; Step 10: During the process of the synthesis chamber rotating from the horizontal state to the vertical state in step 9, the barrier mechanism is opened by cooperating with the opening and closing mechanism, and the InSb melt in the synthesis zone 2 of the dual-zone synthesis tube flows through the necking zone to the synthesis zone 1 of the dual-zone synthesis tube to merge with the GaSb melt to form an InGaSb melt; Step 11: After step 9 is completed, the temperature is kept constant for 4-8 hours to allow the InSb melt and the GaSb melt to be fully mixed in the first zone of the dual-zone synthesis tube to synthesize the InGaSb melt; Step 12: Control the multi-stage heater to cool the first and second zones of the dual-zone synthesis tube from 800°C and 600°C to room temperature, respectively, at a cooling rate of (1-3)°C / min, so that the InGaSb melt is completely crystallized; Step 13: After step 12 is completed, the synthesis cavity is opened and the dual-zone synthesis tube is taken out to obtain an InGaSb ternary alloy polycrystal.

[0015] The present invention has at least the following beneficial effects: 1. The device and method of the present invention adopts a dual-zone structure synthesis tube to synthesize InGaSb polycrystals. First, GaSb and InSb are synthesized in different temperature zones respectively, and then GaSb and InSb are fused to synthesize InGaSb. Compared with the direct use of In, Ga, and Sb elements for synthesis, this method can effectively control the element ratio in InGaSb by controlling the ratio of GaSb and InSb. At the same time, it can effectively avoid the segregation of In in InGaSb in the direct synthesis using In, Ga, and Sb elements, improve the uniformity of the components, and thus ensure the consistency of the material; 2. The device and method of the present invention first synthesizes GaSb polycrystals and InSb polycrystals, and then performs InGaSb synthesis. This allows the three-step synthesis process to be completed in the same device, ensuring the material ratio while shortening the production process and improving efficiency. 3. The GaSb synthesis, InSb synthesis, and InGaSb synthesis methods of the present invention are all carried out in a vacuum-sealed quartz tube, isolated from the external environment and without the need for inert gas. The closed growth environment can effectively avoid impurity contamination, ensuring material purity and the electrical properties of the crystal; 4. The present invention is provided with a coordinated closing mechanism and a blocking mechanism to ensure that GaSb and InSb are independently heated at different temperature states to form a melt. When it is necessary to fuse and synthesize InGaSb, the synthesis cavity can rotate to connect the first zone of the dual-zone synthesis tube and the second zone of the dual-zone synthesis tube, so that InSb can fully enter the first zone of the dual-zone synthesis tube and be synthesized with the GaSb melt to form InGaSb. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram of the structure of the synthetic cavity base of the present invention; Figure 3 For the present invention Figure 2 Schematic diagram of the enlarged structure of area A in the middle; Figure 4 This is a schematic diagram of the structure of the synthetic cavity rotation mechanism of the present invention; Figure 5 Schematic diagram of the internal structure of the synthesis cavity of the present invention; Figure 6 This is a schematic diagram of the dual-zone synthesis tube structure of the present invention; Figure 7 This is a schematic diagram of the support shaft structure of the present invention; Figure 8 This is a top view of the double-zone synthetic tube sealing cap structure of the present invention; Figure 9 For the present invention Figure 8 Schematic diagram of the enlarged structure of the middle B area; Figure 10 This is a structural diagram of the connecting sleeve of the present invention; Figure 11 Schematic diagram of the synchronization block structure of the present invention; Figure 12 This is a schematic diagram of the reverse member structure of the present invention; Figure 13 This is a schematic diagram of the positioning rod structure of the present invention; Figure 14 It is a schematic diagram of the process of the present invention.

[0017] In the figure: 1-synthesis chamber; 2-multi-section heater; 3-dual-zone synthesis pipe; 31-dual-zone synthesis pipe body; 32-dual-zone synthesis pipe sealing cap; 33-dual-zone synthesis pipe synthesis zone 1; 34-dual-zone synthesis pipe necking zone; 35-dual-zone synthesis pipe synthesis zone 2; 4-synthesis chamber rotation mechanism; 41-support shaft; 42-rotation shaft; 43-drive member; 431-drive motor; 432-first drive gear; 433-second drive gear; 44-swing member; 441-swing support rod; 442-connecting shaft; 443-moving block; 444-guide rod; 5-synthesis chamber base; 51-limiting groove; 6-cooperating opening and closing mechanism; 61-connecting sleeve; 611-connecting groove; 612-guide groove; 62-synchronizing block; 63-support adjusting member; 631-support plate; 632-adjusting screw; 64-surrounding rod; 641-raised strip; 65-limiting member; 651-limiting plate; 652-limiting rod; 7-blocking mechanism; 71-positioning rod; 72-first rotating sleeve; 721-rotating groove; 73-second rotating sleeve; 74-closing plate; 75-reversing member; 751-moving plate; 7511-pushing port; 752-pushing rod; 753-pushing plate; 8-limiting guide member; 81-fixing rod; 82-fixing plate; 83-connecting spring. DETAILED DESCRIPTION

[0018] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention. Example

[0019] See also Figures 1 to 2 A dual-zone synthesis device for InGaSb ternary alloy polycrystals, comprising a synthesis cavity 1, a multi-segment heater 2, a dual-zone synthesis tube 3, a synthesis cavity rotating mechanism 4, and a synthesis cavity base 5; The synthesis chamber 1 is used to support and fix the multi-stage heater 2 and the dual-zone synthesis pipe 3 and can be filled with inert gas to protect the synthesis device. The wall of the synthesis chamber 1 is equipped with a water cooling coil for cooling the chamber. Each section of the multi-section heater 2 is a resistance wire heater with independent temperature control and heating; A cooperating opening and closing mechanism 6 is installed on the synthesis cavity base 5, and a barrier mechanism 7 is provided on the dual-zone synthesis pipe 3. The barrier mechanism 7 cooperates with the cooperating opening and closing mechanism 6 to adjust the dual-zone synthesis pipe 3.

[0020] See also Figures 5 and 6 In this embodiment, a mounting opening is provided at one end of the synthesis cavity 1, and the dual-zone synthesis pipe 3 is inserted into the synthesis cavity 1 through the mounting opening. The dual-zone synthesis pipe 3 includes a dual-zone synthesis pipe body 31 and a dual-zone synthesis pipe sealing cap 32. The dual-zone synthesis pipe body 31 includes a dual-zone synthesis pipe synthesis zone 1 33, a dual-zone synthesis pipe necking zone 34, and a dual-zone synthesis pipe synthesis zone 2 35. The barrier mechanism 7 is located at the dual-zone synthesis pipe necking zone 34. There are two double-zone synthetic pipe sealing caps 32 , which are respectively welded to the openings of the double-zone synthetic pipe synthetic zone 1 33 and the double-zone synthetic pipe synthetic zone 2 35 .

[0021] See also Figures 2 to 5 The synthesis cavity rotation mechanism 4 includes a support shaft 41, a rotating shaft 42, a driving member 43 and a swinging member 44. One end of the support shaft 41 is rotatably connected to the bottom of the synthesis cavity 1, and the other end of the support shaft 41 is fixedly connected to the synthesis cavity 1. The rotating shaft 42 passes through the synthesis cavity base 5 and is rotatably connected to the bottom of the synthesis cavity 1. The driving member 43 is used to drive the rotating shaft 42, and the swinging member 44 is installed at the other end of the rotating shaft 42. The swinging member 44 is used to drive the synthesis cavity 1; The driving member 43 includes a driving motor 431, a first driving gear 432 and a second driving gear 433. The driving motor 431 is mounted on the synthesis cavity base 5, and the output end of the driving motor 431 is fixedly connected to the first driving gear 432. The first driving gear 432 is meshed with the second driving gear 433. The second driving gear 433 is fixedly mounted on one end of the rotating shaft 42. Thus, by driving the motor 431, the first driving gear 432 drives the second driving gear 433 to rotate, and when the second driving gear 433 rotates, the rotating shaft 42 rotates synchronously; The swing member 44 includes a swing support rod 441, a connecting shaft 442, a moving block 443 and a guide rod 444. One end of the swing support rod 441 is fixedly connected to the rotating shaft 42, one end of the connecting shaft 442 is rotatably connected to the other end of the swing support rod 441, and the other end of the connecting shaft 442 is fixedly connected to the moving block 443. The moving block 443 is slidably sleeved on the outside of the guide rod 444, and both ends of the guide rod 444 are fixedly installed on the outside of the synthesis cavity 1: Specific implementation process: When the InSb melt and the GaSb melt are fully mixed in the dual-zone synthesis tube synthesis zone 33 to synthesize the InGaSb melt, the synthesis chamber 1 needs to be slowly rotated, and the driving motor 431 is operated to make the first driving gear 432 drive the second driving gear 433 to rotate slowly. When the second driving gear 433 rotates slowly, it drives the rotating shaft 42 to rotate slowly, and the rotating shaft 42 drives the swing support rod 441 to rotate. The swing support rod 441 is limited by the connecting shaft 442 at the other end and the moving block 443 of the guide rod 444, so that the swing support rod 441 slides relative to the guide rod 444 through the moving block 443, and at the same time, the synthesis chamber 1 is slowly rotated with the support shaft 41 as the rotation axis 42 until the synthesis chamber 1 is slowly rotated from a horizontal state to a vertical state, so that the InSb melt and the GaSb melt are fully mixed in the dual-zone synthesis tube synthesis zone 33 to synthesize the InGaSb melt.

[0022] See also Figures 10 to 13 The first and second rotating sleeves 73 are respectively rotatably connected to the plurality of rotating grooves 721. There are two closing plates 74, which are respectively fixed to the first rotating sleeve 72 and the plurality of second rotating sleeves 73. One end of the first rotating sleeve 72 extends to the outside of the dual-zone synthetic pipe necking area 34 and is connected to the reverse member 75. One end of one of the second rotating sleeves 73 extends to the dual-zone synthetic pipe necking area 34 and is connected to the reverse member 75. The second rotating sleeve 73 is rotatably connected to the dual-zone synthetic pipe necking area 34 through a sealed bearing. The reversing member 75 includes a movable plate 751, a pushing rod 752, a pushing plate 753 and a limiting guide member 8. The movable plate 751 is slidably connected to the outside of the necking area 34 of the dual-zone synthetic tube, and two pushing openings 7511 are provided on the movable plate 751. There are two pushing rods 752, and the two pushing rods 752 slide through the pushing openings 7511 respectively. There are two pushing plates 753, and the two pushing plates 753 are respectively fixedly connected to the first rotating sleeve 72 and the second rotating sleeve 73, and the two pushing rods 752 are respectively fixedly connected to the two pushing plates 753. The limiting guide member 8 is installed on the outside of the necking area 34 of the dual-zone synthetic tube, and the limiting guide member 8 is used to guide the movable plate 751.

[0023] The limiting guide 8 includes a fixed rod 81, a fixed plate 82 and a connecting spring 83. The fixed rod 81 slides through one end of the movable plate 751, and both ends of the fixed plate 82 are fixedly connected to the fixed plate 82, and the fixed plate 82 is fixedly installed on the outside of the necking area 34 of the dual-zone synthetic pipe. The connecting spring 83 is sleeved on the outside of the fixed rod 81, and the two ends of the connecting spring 83 are respectively fixedly connected to the movable plate 751 and one of the fixed plates 82.

[0024] Specific implementation process: When the first synthesis zone 33 of the dual-zone synthesis tube is loaded with high-purity gallium and high-purity antimony, and the second synthesis zone 35 of the dual-zone synthesis tube is loaded with high-purity indium and high-purity antimony respectively, then at the dual-zone synthesis tube necking zone 34 between the first synthesis zone 33 and the second synthesis zone 35, the two closing plates 74 are distributed 180 degrees to each other inside the dual-zone synthesis tube necking zone 34, that is, under the reverse elastic force of the connecting spring 83 at the movable plate 751, the movable plate 751 is fixed relative to the dual-zone synthesis tube necking zone 34, and then the first rotating sleeve 72 and the plurality of second rotating sleeves 73 respectively enable the closing plates 74 thereon to be relatively closed inside the dual-zone synthesis tube necking zone 34; The double-zone synthetic tube necking zone 34 is used to make the double-zone synthetic tube synthesis zone 1 33 and the double-zone synthetic tube synthesis zone 2 35 form a relatively independent state. Therefore, in the subsequent double-zone synthetic tube synthesis zone 1 33 and the double-zone synthetic tube synthesis zone 2 35 heating states of different temperatures, independent heating can be guaranteed.

[0025] See also Figure 4 and Figures 7 to 10 The cooperating opening and closing mechanism 6 includes a connecting sleeve 61, a synchronizing block 62, a supporting adjustment member 63, a surrounding rod 64 and a limiting member 65. The connecting sleeve 61 slides through one side of the synthesis cavity 1, and a connecting groove 611 is provided at one end of the connecting sleeve 61 close to the necking area 34 of the dual-zone synthesis pipe. The synchronizing block 62 is located in the connecting groove 611 and is fixedly connected to one end of the first rotating sleeve 72. The support adjustment member 63 is located outside the synthetic cavity 1, and the support adjustment member 63 is used to adjust the position of the connecting sleeve 61. One end of the surrounding rod 64 is slidably connected to the inside of the connecting sleeve 61, and the other end of the surrounding rod 64 is connected to the limit member 65, and the limit member 65 is connected to the synthetic cavity base 5.

[0026] Two raised strips 641 are provided on the outside of the surrounding rod 64, and a guide groove 612 is provided at the position of the connecting sleeve 61 corresponding to the two raised strips 641. The limiting member 65 includes a limiting plate 651 and a limiting rod 652. The limiting plate 651 is fixedly installed on the end of the surrounding rod 64 away from the connecting sleeve 61, and the limiting plate 651 is slidably connected to the synthetic cavity base 5. The synthetic cavity base 5 is provided with a limiting groove 51, and the limiting rod 652 slides through the limiting groove 51. One end of the limiting rod 652 is fixedly connected to the limiting plate 651, and the limiting rod 652 deviates from the center of the limiting plate 651.

[0027] The support adjustment member 63 includes a support plate 631 and an adjusting screw 632. One end of the support plate 631 is rotatably sleeved on the outside of the connecting sleeve 61 through a bearing, and the other end of the support plate 631 is provided with a threaded hole. The adjusting screw 632 passes through the threaded hole, and the adjusting screw 632 is threadedly connected to the threaded hole. One end of the adjusting screw 632 is rotatably connected to the outside of the synthetic cavity 1.

[0028] In this embodiment, when the dual-zone synthetic tube 3 is inserted into the synthetic cavity 1, the synthetic cavity 1 is correspondingly provided with a slide groove, and a slider is provided at the insertion end of the dual-zone synthetic tube 3. Even if the slider of the dual-zone synthetic tube 3 is aligned with the slide groove and inserted into the dual-zone synthetic tube 3, and before insertion, the connecting sleeve 61 deviates from the dual-zone synthetic tube 3, thereby ensuring that the dual-zone synthetic tube 3 is stably placed in the dual-zone synthetic tube 3, and then, the adjusting screw 632 is rotated, and when the adjusting screw 632 is rotated, a driving force is provided to the support plate 631, and the support plate 631 Under the limitation of the connecting sleeve 61, one end of the connecting groove 611 of the connecting sleeve 61 is further moved along the synchronization block 62 until the connecting groove 611 moves to the synchronization block 62 and is sleeved on the outside of the synchronization block 62. At the same time, in this embodiment, the synchronization block 62 is square in shape, thereby ensuring the stability of the connection of the synchronization block 62. At the same time, as the connecting sleeve 61 rotates, the synchronization block 62 can be driven to rotate synchronously, and the connecting sleeve 61 can then be rotated relative to the support plate 631 through the surrounding rod 64 and the raised strip 641.

[0029] Specific implementation process: After the heating is completed, when it is necessary to fully mix the InSb melt and the GaSb melt in the first synthesis zone 33 of the dual-zone synthesis tube to synthesize the InGaSb melt, the surrounding rod 64 rotates synchronously with the rotation of the synthesis cavity 1. Due to the limiting effect of the limiting rod 652 on the limiting plate 651 at one end of the surrounding rod 64 and the limiting effect of the limiting rod 652 in the limiting groove 51, the limiting rod 652 drives the limiting plate 651 to rotate. When the limiting plate 651 rotates, the surrounding rod 64 rotates slowly relative to the synthesis cavity 1. That is, when the surrounding rod 64 rotates, the connecting sleeve 61 drives the first rotating sleeve 72 to rotate due to the limiting effect of the two protruding strips 641. When the first rotating sleeve 72 rotates, the movable plate 751 moves along the direction of the first rotating sleeve 72 and the second rotating sleeve 73 through the limiting effect of the pushing rod 752. When the movable plate 751 moves, the other pushing rod 752 is pushed to rotate through the pushing port 7511, and the other pushing rod 752 is pushed through the pushing plate 753. Under the connecting action, the multiple second rotating sleeves 73 are pushed to rotate. At this time, the two closing plates 74 make the inside of the double-zone synthesis tube necking area 34 open, and the GaSb melt at the double-zone synthesis tube synthesis area 1 33 moves along the inside of the double-zone synthesis tube synthesis area 2 35. At the same time, as the inclination angle of the synthesis cavity 1 gradually increases, until the synthesis cavity 1 rotates to a vertical state, the two closing plates 74 rotate to a similar position, and the double-zone synthesis tube necking area 34 is opened to the maximum state, thereby ensuring that the GaSb melt can fully flow.

[0030] See also Figure 14 A method for synthesizing an InGaSb ternary alloy polycrystal in a dual-zone synthesis device is characterized by comprising the following steps: Step 1: weigh an appropriate amount of high-purity gallium and high-purity antimony in an atomic ratio of 1:1 and place them into a dual-zone synthesis tube to synthesize zone 33; Step 2: weigh an appropriate amount of high-purity indium and high-purity antimony in an atomic ratio of 1:1 and load them into the dual-zone synthesis tube to form the second zone 35; Step 3: Evacuate both ends of the dual-zone quartz tube and weld and seal them with the synthetic tube cap; Step 4: Place the sealed dual-zone quartz tube in the multi-segment heater 2 in the synthesis chamber 1 and fix it; Step 5: The purity of high-purity gallium and high-purity antimony in step 1 is not less than 6N; the purity of high-purity indium and high-purity antimony in step 2 is not less than 6N; the vacuum degree of the double-zone quartz tube in step 3 is less than 1×10-3Pa; Step 6: Control the multi-stage heater 2 to heat, raise the temperature of the first zone 33 of the dual-zone synthesis tube to 800° C., and raise the temperature of the second zone 35 of the dual-zone synthesis tube to 600° C.; Step 7: After the temperature of the first zone 33 and the second zone of the dual-zone synthesis tube is raised to the target temperature of step 6, the temperature is kept constant for 3h-5h to ensure sufficient synthesis; Step 8: The first synthesis zone 33 of the dual-zone synthesis tube in step 6 is heated from room temperature to 800° C. at a heating rate of (5-10)° C. / min, and the second synthesis zone 35 of the dual-zone synthesis tube in step 6 is heated from room temperature to 600° C. at a heating rate of (5-10)° C. / min; Step 9: The synthesis cavity 1 is slowly rotated from a horizontal state to a vertical state by adjusting the synthesis cavity rotation mechanism 4 that is connected to one end of the synthesis cavity 1 and the cavity base; Step 10: During the process of the synthesis chamber 1 rotating from the horizontal state to the vertical state in step 9, the opening and closing mechanism 6 is coordinated to open the barrier mechanism 7, and the InSb melt in the synthesis zone 2 35 of the dual-zone synthesis tube flows through the necking zone to the synthesis zone 1 33 of the dual-zone synthesis tube to merge with the GaSb melt to form an InGaSb melt; Step 11: After step 9 is completed, the temperature is kept constant for 4-8 hours to allow the InSb melt and the GaSb melt to be fully mixed in the first synthesis zone 33 of the dual-zone synthesis tube to synthesize the InGaSb melt; Step 12: Control the multi-stage heater 2 to cool the temperature of the first zone 33 and the second zone of the dual-zone synthesis tube from 800° C. and 600° C. to room temperature, respectively, at a cooling rate of (1-3)° C. / min, so that the InGaSb melt is completely crystallized; Step 13: After step 12 is completed, the synthesis cavity is opened and the dual-zone synthesis tube is taken out to obtain an InGaSb ternary alloy polycrystal. Example

[0031] The specifications of the dual-zone synthesis apparatus for the InGaSb ternary alloy in this embodiment are the same as those in Example 1. The method for synthesizing an In0.8Ga0.2Sb ternary alloy polycrystal with a Ga:In ratio of 2:8 using the above apparatus is as follows: Step 1: Weigh 4160g of high-purity indium and high-purity antimony at an atomic ratio of 1:1 and load them into a dual-zone synthesis tube for synthesis zone 1. Weigh 840g of high-purity gallium and high-purity antimony at an atomic ratio of 1:1 and load them into a dual-zone synthesis tube for synthesis zone 2. Evacuate both ends of the dual-zone quartz tube and weld the tube cap to seal it. Place the sealed dual-zone quartz tube in a multi-segment heater in the synthesis chamber and secure it. Step 2: Control the multi-stage heater to heat the first zone of the dual-zone synthesis tube from room temperature to 800°C at a heating rate of 5°C / min, and heat the second zone of the dual-zone synthesis tube from room temperature to 600°C at a heating rate of 5°C / min. After the first and second zones of the dual-zone synthesis tube reach the target temperature, the temperature is kept constant for 4 hours to ensure that InSb and GaSb are fully synthesized. Step 3: The synthesis cavity is slowly rotated from a horizontal state to a vertical state by adjusting the synthesis cavity rotation mechanism that telescopically connects one end of the synthesis cavity and the cavity base, and the temperature is maintained constant for 5 hours. During the process of the synthesis cavity rotating from the horizontal state to the vertical state, the GaSb melt in the synthesis zone 2 of the dual-zone synthesis tube flows through the necking zone to the synthesis zone 1 of the dual-zone synthesis tube and merges with the InSb melt to form an InGaSb melt; Step 4: Control the multi-stage heater to cool the first and second zones of the dual-zone synthesis tube from 800°C and 600°C respectively to room temperature at a cooling rate of 2°C / min to allow the InGaSb melt to completely crystallize. After step 12 is completed, open the synthesis chamber and take out the dual-zone synthesis tube to obtain a ternary alloy polycrystal with a ratio of In0.8Ga0.2Sb and a weight of 5 kg.

[0032] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0033] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A dual-zone synthesis device for InGaSb ternary alloy polycrystals, characterized by: It comprises a synthesis cavity (1), a multi-section heater (2), a dual-zone synthesis tube (3), a synthesis cavity rotating mechanism (4) and a synthesis cavity base (5); The synthesis cavity (1) is used to support and fix the multi-stage heater (2) and the dual-zone synthesis pipe (3) and can be filled with inert gas to protect the synthesis device. The wall of the synthesis cavity (1) is provided with a water cooling coil for cooling the cavity; Each section of the multi-section heater (2) is a resistance wire heater with independent temperature control and heating; A matching opening and closing mechanism (6) is installed on the synthesis cavity base (5), and a barrier mechanism (7) is provided on the dual-zone synthesis pipe (3). The barrier mechanism (7) cooperates with the matching opening and closing mechanism (6) to adjust the dual-zone synthesis pipe (3).

2. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 1, characterized in that: The dual-zone synthetic pipe (3) comprises a dual-zone synthetic pipe body (31) and a dual-zone synthetic pipe sealing cap (32); the dual-zone synthetic pipe body (31) comprises a dual-zone synthetic pipe synthesis zone 1 (33), a dual-zone synthetic pipe necking zone (34) and a dual-zone synthetic pipe synthesis zone 2 (35); the barrier mechanism (7) is located at the dual-zone synthetic pipe necking zone (34); Two double-zone synthetic pipe sealing caps (32) are provided, and the two double-zone synthetic pipe sealing caps (32) are respectively welded to the openings of the double-zone synthetic pipe synthetic zone 1 (33) and the double-zone synthetic pipe synthetic zone 2 (35).

3. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 2, characterized in that: The synthesis cavity rotation mechanism (4) comprises a support shaft (41), a rotation shaft (42), a driving member (43) and a swinging member (44); one end of the support shaft (41) is rotationally connected to the bottom of the synthesis cavity (1), and the other end of the support shaft (41) is fixedly connected to the synthesis cavity (1); the rotation shaft (42) passes through the synthesis cavity base (5), and the rotation shaft (42) is rotationally connected to the bottom of the synthesis cavity (1); the driving member (43) is used to drive the rotation shaft (42), and the swinging member (44) is installed at the other end of the rotation shaft (42); the swinging member (44) is used to drive the synthesis cavity (1).

4. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 3, characterized in that: The barrier mechanism (7) comprises a positioning rod (71), a first rotating sleeve (72), a second rotating sleeve (73), a closing plate (74) and a reverse member (75), one end of the positioning rod (71) is fixedly connected to the inner wall of the necking area (34) of the double-zone synthetic pipe, the first rotating sleeve (72) is rotatably sleeved on the outside of the positioning rod (71), and the first rotating sleeve (72) is provided with a plurality of rotating grooves (721), the second rotating sleeve (73) is provided with a plurality of second rotating sleeves, and the plurality of second rotating sleeves (73) are respectively rotatably sleeved at a plurality of rotating grooves (721), two closing plates (74) are provided, and the two closing plates (74) are respectively fixedly connected to the first rotating sleeve (72) and the plurality of second rotating sleeves (73), one end of the first rotating sleeve (72) extends to the outside of the double-zone synthetic pipe necking area (34) and is connected to the reverse member (75), and one end of one of the second rotating sleeves (73) extends to the double-zone synthetic pipe necking area (34) and is connected to the reverse member (75).

5. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 4, characterized in that: The reversing member (75) includes a movable plate (751), a pushing rod (752), a pushing plate (753) and a limiting guide member (8). The movable plate (751) is slidably connected to the outside of the double-zone synthetic tube necking region (34), and two pushing openings (7511) are provided on the movable plate (751). The pushing rod (752) is provided with two, and the two pushing rods (752) respectively slide through the pushing openings (7511). The pushing plates (753) are provided with two, and the two pushing plates (753) are respectively fixedly connected to the first rotating sleeve (72) and the second rotating sleeve (73), and the two pushing rods (752) are respectively fixedly connected to the two pushing plates (753). The limiting guide member (8) is installed on the outside of the double-zone synthetic tube necking region (34), and the limiting guide member (8) is used to guide the movable plate (751).

6. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 5, characterized in that: The limiting guide member (8) includes a fixed rod (81), a fixed plate (82) and a connecting spring (83), wherein the fixed rod (81) slides through one end of the movable plate (751), and both ends of the fixed plate (82) are fixedly connected to the fixed plate (82), and the fixed plate (82) is fixedly mounted on the outside of the necking area (34) of the double-zone synthetic pipe, and the connecting spring (83) is sleeved on the outside of the fixed rod (81), and the two ends of the connecting spring (83) are fixedly connected to the movable plate (751) and one of the fixed plates (82), respectively.

7. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 6, characterized in that: The cooperative opening and closing mechanism (6) comprises a connecting sleeve (61), a synchronizing block (62), a supporting adjusting member (63), a surrounding rod (64) and a limiting member (65); the connecting sleeve (61) slides through one side of the synthetic cavity (1), and a connecting groove (611) is provided at one end of the connecting sleeve (61) close to the necking area (34) of the double-zone synthetic pipe. The synchronizing block (62) is located at the connecting groove (611), and the synchronizing block (62) is fixedly connected to one end of the first rotating sleeve (72); The support adjustment member (63) is located outside the synthetic cavity (1), and the support adjustment member (63) is used to adjust the position of the connecting sleeve (61). One end of the surrounding rod (64) is slidably connected to the inside of the connecting sleeve (61), and the other end of the surrounding rod (64) is connected to the limiting member (65), and the limiting member (65) is connected to the synthetic cavity base (5).

8. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 7, characterized in that: Two raised strips (641) are provided on the outer side of the surrounding rod (64), and a guide groove (612) is provided at a position of the connecting sleeve (61) corresponding to the two raised strips (641). The limiting member (65) includes a limiting plate (651) and a limiting rod (652). The limiting plate (651) is fixedly mounted on an end of the surrounding rod (64) away from the connecting sleeve (61), and the limiting plate (651) is slidably connected to the synthetic cavity base (5). The synthetic cavity base (5) is provided with a limiting groove (51), and the limiting rod (652) slides through the limiting groove (51). One end of the limiting rod (652) is fixedly connected to the limiting plate (651), and the limiting rod (652) deviates from the center of the limiting plate (651).

9. The dual-zone synthesis device for InGaSb ternary alloy polycrystal according to claim 7, characterized in that: The support adjustment member (63) comprises a support plate (631) and an adjustment screw (632), one end of the support plate (631) being rotatably sleeved on the outside of the connecting sleeve (61) via a bearing, and the other end of the support plate (631) being provided with a threaded hole, the adjustment screw (632) passing through the threaded hole, and the adjustment screw (632) being threadedly connected to the threaded hole, and one end of the adjustment screw (632) being rotatably connected to the outside of the synthetic cavity (1).

10. A method for synthesizing an InGaSb ternary alloy polycrystal using a dual-zone synthesis device, characterized in that: The following steps are involved: Step 1: weigh an appropriate amount of high-purity gallium and high-purity antimony in an atomic ratio of 1:1 and place them into a double-zone synthesis tube to synthesize one zone (33); Step 2: weigh an appropriate amount of high-purity indium and high-purity antimony in an atomic ratio of 1:1 and place them into the dual-zone synthesis tube to synthesize the second zone (35); Step 3: Evacuate both ends of the dual-zone quartz tube and weld and seal them with the synthetic tube cap; Step 4: Place the sealed dual-zone quartz tube in the multi-segment heater (2) in the synthesis chamber (1) and fix it; Step 5: The purity of the high-purity gallium and high-purity antimony in step 1 is not less than 6N; the purity of the high-purity indium and high-purity antimony in step 2 is not less than 6N; the vacuum degree of the double-zone quartz tube in step 3 is less than 1×10-3Pa; Step 6: Control the multi-stage heater (2) to heat, raise the temperature of the first zone (33) of the double-zone synthesis tube to 800°C, and raise the temperature of the second zone (35) of the double-zone synthesis tube to 600°C; Step 7: After the temperature of the first zone (33) and the second zone of the dual-zone synthesis tube is raised to the target temperature in step 6, the temperature is kept constant for 3h-5h to ensure sufficient synthesis; Step eight: the first synthesis zone (33) of the dual-zone synthesis tube in step six is heated from room temperature to 800°C at a heating rate of (5-10)°C / min, and the second synthesis zone (35) of the dual-zone synthesis tube in step six is heated from room temperature to 600°C at a heating rate of (5-10)°C / min; Step nine: by adjusting the synthetic cavity rotating mechanism (4) that is connected to one end of the synthetic cavity (1) and the cavity base, the synthetic cavity (1) is slowly rotated from a horizontal state to a vertical state; Step 10: During the process of the synthesis cavity (1) rotating from the horizontal state to the vertical state in step 9, the opening and closing mechanism (6) is coordinated to open the barrier mechanism (7), and the InSb melt in the synthesis zone 2 (35) of the dual-zone synthesis tube flows through the necking zone to the synthesis zone 1 (33) of the dual-zone synthesis tube and merges with the GaSb melt to synthesize the InGaSb melt; Step 11: After step 9 is completed, continue to maintain the temperature constant for 4h-8h, so that the InSb melt and the GaSb melt are fully mixed in the first zone (33) of the dual-zone synthesis tube to synthesize the InGaSb melt; Step 12: Control the multi-stage heater (2) to cool the first zone (33) and the second zone of the dual-zone synthesis tube from 800°C and 600°C to room temperature, respectively, at a cooling rate of (1-3)°C / min, so that the InGaSb melt is completely crystallized; Step 13: After step 12 is completed, the synthesis cavity (1) is opened and the dual-zone synthesis tube (3) is taken out to obtain the InGaSb ternary alloy polycrystal.

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