Indium antimonide crystal growth equipment and growth method
By introducing the control of the pot base lifting device and heater into the indium antimonide crystal growth equipment, the problem of crucible rupture during cooling is solved, and the reusable use of the equipment and the service life are extended.
Patent Information
- Application Number
- CN202411781515.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-05
- Publication Date
- 2025-03-25
AI Technical Summary
During the growth of indium antimonide crystals, the crucible is prone to rupture during cooling and cooling when using the lifting method, resulting in equipment damage and increased costs.
A crystal growth equipment of indium antimonide is designed, using a pot base lifting device and heater to ensure that all the pot base in the crucible is removed and the crucible is ruptured during the cooling process.
Through this equipment and method, the crucible can be effectively avoided, the service life of the equipment can be extended, and the crucible can be reused.
Smart Images
Figure CN119685921A_ABST
Abstract
Description
Technical Field
[0001] The present disclosure relates to the field of crystal growth, and more specifically to an indium antimonide crystal growth device and a growth method. Background Art
[0002] With the advancement and development of science and technology, more and more semiconductor crystals are gaining more and more attention due to their outstanding role in optoelectronic systems.
[0003] As a III-V semiconductor crystal material, indium antimonide crystal has extremely narrow bandgap, extremely small electron effective mass and extremely high electron mobility, and its physical and chemical properties are stable. Based on these excellent properties, it has been applied in important industrial technology fields such as magnetoresistive elements and Hall devices. It is particularly noteworthy that since indium antimonide has intrinsic absorption in the 3-5μm band, infrared detectors based on indium antimonide have extremely high quantum efficiency and response rate, so indium antimonide has become the preferred material for medium-wave infrared detectors.
[0004] At present, domestic and foreign companies and research institutions mainly use the Czochralski method (also known as the Czochralski method) to prepare InSb single crystals. Because the melt density of InSb material is greater than the solid density, the volume of InSb material increases during the solidification of the melt, which often damages the crucible that supports it. Especially during the cooling process after the growth of the Czochralski crystal, the solidification of the bottom material in the crucible is usually accompanied by the rupture of the crucible. Therefore, it is necessary to provide a new crystal growth technology. Summary of the invention
[0005] In view of the problems existing in the background technology, an object of the present disclosure is to provide an indium antimonide crystal growth device and a growth method, which can avoid the crucible from cracking during the cooling process after the indium antimonide crystal growth using the pulling method is completed, thereby allowing the crucible to be reused.
[0006] Thus, an indium antimonide crystal growth device includes a crucible containing an InSb melt, a heater for heating the crucible, a crystal pulling rod, and a seed crystal installed at the end of the crystal pulling rod; the indium antimonide crystal growth device also includes a crucible bottom material pulling device. The crucible bottom material pulling device includes a pulling rod and a seed crystal head installed at the end of the pulling rod, and the pulling rod, the seed crystal head and the heater are configured as follows: after the crystal pulling rod ends pulling the crystal through the seed crystal straight-pulling growth, the heater heats the crucible so that the crucible bottom material in the crucible maintains the liquid surface without floating InSb crystal blocks, the crucible bottom material pulling device works, the pulling rod together with the seed crystal head moves above the crucible and extends into the crucible, the seed crystal head contacts the liquid surface and starts to seed, the heater cools down to cool down the crucible, and when the crucible bottom material starts to crystallize, the crucible bottom material pulling device causes the pulling rod to pull so that the crucible bottom material is completely crystallized and pulled out of the crucible.
[0007] .A method for growing indium antimonide crystals adopts the aforementioned indium antimonide crystal growing equipment. The operation of the indium antimonide crystal growth method is as follows: after the crystal pulling rod finishes pulling the crystal through the seed crystal, the heater heats the crucible so that the bottom material in the crucible maintains the liquid surface without floating InSb crystal blocks, the bottom material pulling device works, the pulling rod together with the seed crystal head moves to the top of the crucible and extends into the crucible, the seed crystal head contacts the liquid surface and starts to seed, the heater is cooled to cool the crucible, and when the bottom material begins to crystallize, the bottom material pulling device causes the pulling rod to pull so that the bottom material is completely crystallized and pulled out of the crucible.
[0008] The beneficial effects of the present disclosure are as follows: in the indium antimonide crystal growth equipment and growth method according to the present disclosure, by adding a crucible bottom material pulling device and coordinating the heating and cooling of the heater, the crucible bottom material can be completely removed (i.e., pulled out) from the crucible after the crystal pulling rod has finished pulling the crystal through the seed crystal, thereby preventing the crucible bottom material remaining in the crucible after the crystal has finished pulling due to the cooling process, causing the crucible to break, thereby allowing the crucible to be reused. BRIEF DESCRIPTION OF THE DRAWINGS
[0009] Figure 1 It is a structural schematic diagram of the indium antimonide crystal growth equipment according to the present disclosure, wherein the crucible bottom material pulling device is in a position to pull the growing crystal away from the seed crystal at the end of the pulling rod, and the pulling rod is ready to directly pull the growing crystal through the seed crystal.
[0010] Figure 2 It is another structural schematic diagram of the indium antimonide crystal growth equipment according to the present disclosure, wherein, after the crystal pulling rod finishes pulling the grown crystal through the seed crystal, the crucible bottom material pulling device is in a position to prepare to pull the crucible bottom material in the crucible.
[0011] Figure 3 This is a photograph of the crucible bottom material pulled out in Example 1.
[0012] Figure 4 This is a photograph of the crucible of Comparative Example 1 when the crucible bottom material pulling device is not in operation.
[0013] The description of the accompanying drawings is as follows.
[0014] 100 InSb crystal growth equipment 154 Rotating mechanism
[0015] D1 vertical direction 154a motor
[0016] D2 Horizontal direction 154b rotation axis
[0017] 11 Crucible 154c connecting plate
[0018] 12 heater 155 translation mechanism
[0019] 121 graphite heater 16 top cover
[0020] 122 graphite double-layer insulation cover 17 middle tube
[0021] 122a inner layer 18 base
[0022] 122b outer layer 19 screw
[0023] 123 carbon felt 20 vacuum interface
[0024] 13 Crystal pulling rod 21 Gas inlet
[0025] 14 seed crystals 22 brackets
[0026] 15 Crucible Bottom Material Pulling Device 200InSb Melt
[0027] 151 lifting rod 300 crystal
[0028] 152 seed crystal head 400 crucible bottom material
[0029] 153 lifting mechanism DETAILED DESCRIPTION
[0030] 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.
[0031] [Indium Antimonide Crystal Growth Equipment]
[0032] Reference Figure 1 and Figure 2 According to the present disclosure, the indium antimonide crystal growth device 100 includes a crucible 11 for holding an InSb melt 200, a heater 12 for heating the crucible 11, a crystal pulling rod 13, and a seed crystal 14 installed at the end of the crystal pulling rod 13. The indium antimonide crystal growth device 100 also includes a crucible bottom material pulling device 15. The crucible bottom material pulling device 15 includes a pulling rod 151 and a seed crystal head 152 installed at the end of the pulling rod 151. The pulling rod 151, the seed crystal head 152 and the heater 12 are configured as follows: after the pulling rod 13 completes pulling the grown crystal 300 by directly pulling the seed crystal 14, the heater 12 heats the crucible 11 so that the bottom material 400 in the crucible 11 maintains no floating InSb crystal blocks on the liquid surface, the bottom material pulling device 15 works, the pulling rod 151 together with the seed crystal head 152 moves to the top of the crucible 11 and extends into the crucible 11, the seed crystal head 152 contacts the liquid surface and starts to induce crystal, the heater 12 cools down to cool down the crucible 11, and when the bottom material 400 starts to crystallize, the bottom material pulling device 15 causes the pulling rod 151 to pull so that the bottom material 400 is completely crystallized and completely pulled out of the crucible 11.
[0033] In the indium antimonide crystal growth equipment 100 according to the present disclosure, by adding a bottom material pulling device 15 and cooperating with the heating and cooling of the heater 12, the bottom material 400 can be completely removed (i.e. pulled out) from the crucible 11 after the crystal pulling rod 13 completes pulling of the grown crystal 300 through the seed crystal 14, thereby preventing the bottom material 400 remaining in the crucible 11 after the straight-pulling growth of the crystal is completed from breaking due to the cooling process, thereby allowing the crucible 11 to be reused.
[0034] In one example, the heater 12 heats the crucible 11 to increase the temperature by 5-20° C. The heater 12 cools the crucible 11 by 20-30° C. The lifting speed of the lifting rod 151 is 5-20 mm / h. For example, the crucible 11 is a quartz crucible.
[0035] like Figure 1 As shown, in one example, the heater 12 includes a graphite heater 121, a graphite double-layer heat-insulating cover 122, and a carbon felt 123; the graphite heater 121 is arranged around the crucible 11, and the graphite double-layer heat-insulating cover 122 is arranged around the graphite heater 121. Further, the graphite double-layer heat-insulating cover 122 includes an inner layer 122a and an outer layer 122b; the carbon felt 123 is filled between the inner layer 122a and the outer layer 122b of the graphite double-layer heat-insulating cover 122.
[0036] The crystal pulling rod 13 is disposed above the crucible 3. The crystal pulling rod 13 is connected to a corresponding rotating mechanism (not shown) and a corresponding lifting mechanism (not shown) so as to be able to reciprocate in the up and down directions while rotating. The crystal pulling rod 13 is configured to drive the seed crystal 14 to move downward into the crucible 11, immerse into the InSb melt 200 from the surface of the InSb melt, and then the crystal pulling rod 13 is pulled upward to grow the crystal 300.
[0037] The seed crystal 14 may be an InSb single crystal with a purity of 7N. Similarly, the seed crystal head 152 may be an InSb single crystal with a purity of 7N.
[0038] like Figure 1 and Figure 2 As shown, in one example, the crucible bottom material lifting device 15 further includes a lifting mechanism 153, which is connected to the lifting rod 151 and is used to drive the lifting rod 151 to move up and down in the vertical direction D1. Specifically, the lifting mechanism 153 is a telescopic cylinder, a hydraulic cylinder or a linear motor.
[0039] like Figure 1 and Figure 2As shown, in one example, the crucible bottom material pulling device 15 also includes a rotating mechanism 154, which is connected to the lifting mechanism 153. The rotating mechanism 154 is used to drive the lifting mechanism 153 together with the lifting rod 151 and the seed crystal head 152 to rotate, so as to drive the lifting mechanism 153 together with the lifting rod 151 and the seed crystal head 152 to rotate to avoid the seed crystal 14 at the end of the pulling rod 13 when the pulling rod 13 directly pulls the growing crystal 300 through the seed crystal 14, and to drive the lifting mechanism 153 together with the lifting rod 151 and the seed crystal head 152 to rotate above the crucible 11 after the pulling rod 13 directly pulls the growing crystal 300 through the seed crystal 14 and finishes pulling. So as to enable the lifting mechanism 153 to lift the lifting rod 151 and the seed crystal head 152 to pull the crucible bottom material 400.
[0040] Reference Figure 1 In one example, the indium antimonide crystal growth device 100 includes a top cover 16, and the rotating mechanism 154 includes a motor 154a, a rotating shaft 154b, and a connecting plate 154c. The motor 154a is fixed to the inner side of the top cover 16; the rotating shaft 154b is connected to the motor 154a and can rotate under the drive of the motor 154a; the connecting plate 154c is connected to the rotating shaft 154b to rotate under the drive of the rotating shaft 154b; the lifting mechanism 153 is fixedly connected to the connecting plate 154c, and the connection position of the lifting mechanism 153 and the connecting plate 154c is spaced apart from the connection position of the rotating shaft 154b and the connecting plate 154c in the horizontal direction D2 perpendicular to the vertical direction D1.
[0041] Reference Figure 1 In one example, the crucible bottom material lifting device 15 further includes a translation mechanism 155. The translation mechanism 155 is fixed to the inner side of the top cover 16; the motor 154a is connected to the translation mechanism 155 to reciprocate along the horizontal direction D2 under the drive of the translation mechanism 155. Specifically, the translation mechanism 155 is a telescopic cylinder, a hydraulic cylinder or a linear motor.
[0042] Reference Figure 1 In one example, the InSb crystal growth apparatus 100 further includes a middle cylinder 17 , a base 18 , and a plurality of screws 19 . The top cover 16 and the middle cylinder 17 are detachably assembled via the screws 19 , and the middle cylinder 17 and the base 18 are detachably assembled via the screws 19 .
[0043] Reference Figure 1In one example, the indium antimonide crystal growth device 100 further includes a vacuum interface 20, a gas inlet 21, and a bracket 22. The vacuum interface 20 is provided on the base 18. The gas inlet 21 is provided on the top cover 16, and the gas inlet 21 is used to introduce a purge gas (e.g., nitrogen) and a gas required for the crystal growth process (e.g., a nitrogen-hydrogen mixture). The bracket 22 is used to achieve fixed support for the crucible 11. The bracket 22 is connected to an external rotating mechanism (not shown) and an external lifting mechanism (not shown) so that it can rotate and rise simultaneously during crystal growth, so that the liquid level of the InSb melt in the crucible 11 is within the range heated by the heater 12, and the rotation of the crucible 11 is opposite to the rotation of the crystal pulling rod 13.
[0044] [Indium Antimonide Crystal Growth Method]
[0045] According to the indium antimonide crystal growth method disclosed in the present invention, the aforementioned indium antimonide crystal growth device 100 is used. The indium antimonide crystal growth method is operated as follows: after the crystal pulling rod 13 completes pulling the grown crystal 300 through the seed crystal 14, the heater 12 heats the crucible 11 so that the bottom material 400 in the crucible 11 maintains no floating InSb crystal blocks on the liquid surface, the bottom material pulling device 15 works, the pulling rod 151 together with the seed crystal head 152 moves to the top of the crucible 11 and extends into the crucible 11, the seed crystal head 152 contacts the liquid surface and starts to induce crystals, the heater 12 cools down to cool down the crucible 11, and when the bottom material 400 starts to crystallize, the bottom material pulling device 15 causes the pulling rod 151 to pull so that the bottom material 400 is completely crystallized and completely pulled out of the crucible 11.
[0046] The characteristics, effects and operations of the indium antimonide crystal growth device 100 used in the indium antimonide crystal growth method according to the present disclosure are described above and will not be repeated here.
[0047] [test]
[0048] Example 1
[0049] Example 1 uses a Figure 1 and Figure 2 The above-mentioned indium antimonide crystal growth equipment 100 of the crucible bottom material pulling device 15 of the entire structure, the crucible 11 is a quartz crucible, the seed crystal 14 is an indium antimonide single crystal with a purity of 7N, and the seed crystal head 152 is an indium antimonide single crystal with a purity of 7N.
[0050] The operation of the indium antimonide crystal growth method is as follows: after the crystal pulling rod 13 completes the pulling of the grown crystal 300 through the seed crystal 14, the heater 12 heats the crucible 11 to increase the temperature by 15°C, so that the bottom material 400 in the crucible 11 maintains a liquid surface without floating InSb crystal blocks, the bottom material pulling device 15 works, the pulling rod 151 together with the seed crystal head 152 moves to the top of the crucible 11 and extends into the crucible 11, the seed crystal head 152 contacts the liquid surface and starts to seed, the heater 12 cools down to cool the crucible 11 by 25°C, and when the bottom material 400 starts to crystallize, the bottom material pulling device 15 causes the pulling rod 151 to pull at a speed of 18 mm / h to make the bottom material 400 completely crystallize and be completely pulled out of the crucible 11.
[0051] Figure 3 This is a photograph of the crucible bottom material pulled out in Example 1.
[0052] Comparative Example 1
[0053] Comparative Example 1: Figure 1 and Figure 2 The above-mentioned indium antimonide crystal growth device 100 of the entire structure including the crucible bottom material pulling device 15, the crucible 11 is a quartz crucible, the seed crystal 14 is an indium antimonide single crystal with a purity of 7N, and the seed crystal head 152 is an indium antimonide single crystal with a purity of 7N. However, after the crystal pulling rod 13 completes the pulling of the grown crystal 300 by the seed crystal 14, the crucible bottom material pulling device 15 is not operated, and the crucible bottom material 400 is retained in the crucible 11. After that, the indium antimonide crystal growth device 100 is cooled to room temperature, and the gas in the indium antimonide crystal growth device 100 is replaced with nitrogen by a vacuum pump through the vacuum interface 20 and the gas inlet 21 again, and then the indium antimonide crystal growth device 100 is opened and the crucible 11 is taken out.
[0054] Figure 4 This is a photo of the crucible of Comparative Example 1 when the crucible bottom material pulling device is not in operation. Figure 4 It can be seen that the crucible is broken.
[0055] 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. An indium antimonide crystal growth device, comprising a crucible (11) containing an InSb melt (200), a heater (12) for heating the crucible (11), a crystal pulling rod (13), and a seed crystal (14) mounted at the end of the crystal pulling rod (13); It is characterized in that The indium antimonide crystal growing device (100) further comprises a crucible bottom material pulling device (15), The crucible bottom material lifting device (15) comprises a lifting rod (151) and a seed crystal head (152) installed at the end of the lifting rod (151). The pulling rod (151), the seed crystal head (152) and the heater (12) are configured such that: after the crystal pulling rod (13) stops pulling the growing crystal (300) through the seed crystal (14), the heater (12) heats the crucible (11) so that the bottom material (400) in the crucible (11) maintains a liquid surface without floating InSb crystal blocks, the bottom material pulling device (15) starts working, the pulling rod (151) together with the seed crystal head (152) moves to the top of the crucible (11) and extends into the crucible (11), the seed crystal head (152) contacts the liquid surface and starts seeding, the heater (12) cools down the crucible (11), and when the bottom material (400) starts to crystallize, the bottom material pulling device (15) causes the pulling rod (151) to pull so that the bottom material (400) is completely crystallized and completely pulled out of the crucible (11).
2. The indium antimonide crystal growth device according to claim 1, characterized in that: The heater (12) heats the crucible (11) to increase the temperature by 5-20°C; The heater (12) cools the crucible (11) by 20-30°C; The lifting speed of the lifting rod (151) is 5-20mm / h.
3. The indium antimonide crystal growth device according to claim 1, characterized in that: The crucible bottom material lifting device (15) further comprises a lifting mechanism (153). The lifting mechanism (153) is connected to the lifting rod (151), and the lifting mechanism (153) is used to drive the lifting rod (151) to rise and fall in the vertical direction (D1).
4. The indium antimonide crystal growth device according to claim 1, characterized in that: The crucible bottom material lifting device (15) further comprises a rotating mechanism (154). The rotating mechanism (154) is connected to the lifting mechanism (153). The rotating mechanism (154) is used to drive the lifting mechanism (153) together with the lifting rod (151) and the seed crystal head (152) to rotate, so as to drive the lifting mechanism (153) together with the lifting rod (151) and the seed crystal head (152) to rotate to the seed crystal (14) avoiding the end of the pulling rod (13) to lift the growing crystal (300) when the pulling rod (13) passes through the seed crystal (14) to pull the growing crystal (300); and after the pulling rod (13) passes through the seed crystal (14) to pull the growing crystal (300) and finishes pulling, drive the lifting mechanism (153) together with the lifting rod (151) and the seed crystal head (152) to rotate above the crucible (11) so that the lifting mechanism (153) lifts the lifting rod (151) and the seed crystal head (152) to lift the crucible bottom material (400).
5. The indium antimonide crystal growth device according to claim 4, characterized in that: The indium antimonide crystal growth apparatus (100) comprises a top cover (16), The rotating mechanism (154) includes a motor (154a), a rotating shaft (154b) and a connecting disk (154c). The motor (154a) is fixed to the inner side of the top cover (16); The rotating shaft (154b) is connected to the motor (154a) and can rotate under the drive of the motor (154a); The connecting disk (154c) is connected to the rotating shaft (154b) so as to rotate driven by the rotating shaft (154b); The lifting mechanism (153) is fixedly connected to the connecting disk (154c), and the connection position between the lifting mechanism (153) and the connecting disk (154c) is spaced apart from the connection position between the rotating shaft (154b) and the connecting disk (154c) in a horizontal direction (D2) perpendicular to the vertical direction (D1).
6. The indium antimonide crystal growth device according to claim 5, characterized in that: The crucible bottom material lifting device (15) further comprises a translation mechanism (155); The translation mechanism (155) is fixed to the inner side of the top cover (16); The motor (154a) is connected to the translation mechanism (155) so as to reciprocate along the horizontal direction (D2) under the drive of the translation mechanism (155).
7. The indium antimonide crystal growth device according to claim 6, characterized in that: The translation mechanism (155) is a telescopic cylinder, a hydraulic cylinder or a linear motor.
8. The indium antimonide crystal growth device according to claim 1, characterized in that: The crucible (11) is a quartz crucible.
9. The indium antimonide crystal growth device according to claim 1, characterized in that: The seed crystal (14) is an indium antimonide single crystal with a purity of 7N, and the seed crystal head (152) is an indium antimonide single crystal with a purity of 7N.
10. A method for growing indium antimonide crystals, characterized in that: An indium ion crystal growth device (100) according to any one of claims 1 to 9, The indium antimonide crystal growth method is operated as follows: after the crystal pulling rod (13) passes through the seed crystal (14) and the straight-pull growth crystal (300) is pulled off, the heater (12) heats the crucible (11) so that the bottom material (400) in the crucible (11) maintains a liquid surface without floating InSb crystal blocks, the bottom material pulling device (15) works, the pulling rod (151) together with the seed crystal head (152) moves to the top of the crucible (11) and extends into the crucible (11), the seed crystal head (152) contacts the liquid surface and starts seeding, the heater (12) cools down the crucible (11), and when the bottom material (400) starts to crystallize, the bottom material pulling device (15) causes the pulling rod (151) to pull so that the bottom material (400) is completely crystallized and completely pulled out of the crucible (11).