Preparation device and preparation method of high-purity antimony dopant

Abstract

The invention discloses a preparation device and a preparation method of a high-purity antimony dopant, and relates to the technical field of metal processing. The preparation device of the high-purity antimony doping agent comprises a base and a fixing clamp, a heat preservation device is arranged on the upper surface of the base, a supporting frame is fixedly connected to the upper surface of the base, a connecting rod is fixedly connected to the outer surface of the fixing clamp, a connecting frame is fixedly connected to the outer surface of the connecting rod, and a supporting iron ring is fixedly connected to the bottom of the connecting frame. A quartz crucible is arranged at the top of the supporting iron ring, a cover plate is arranged at the top of the quartz crucible, a seed crystal dismounting opening is formed in the top of the cover plate, the heat preservation device comprises a base, a control box and a telescopic air cylinder are fixedly connected to the upper surface of the base, a heat preservation shell is fixedly connected to the top end of the telescopic air cylinder, and a vacuum cavity is formed in the heat preservation shell; the heating coil is arranged in the inner cavity of the heat preservation shell, the heat preservation function can be provided in the preparation process, and low-power-consumption single-time preparation of a large amount of high-purity antimony dopant is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of metal processing, and in particular to a preparation device and a preparation method of a high-purity antimony dopant. Background Art

[0002] High-purity antimony is mainly used in the semiconductor manufacturing industry. Indium antimonide and gallium antimonide are typical antimonide semiconductors formed by high-purity antimony. In addition, high-purity antimony can be used as a dopant for semiconductor silicon and germanium to improve their performance. It can also be used to prepare thermoelectric conversion elements, cooling elements, piezoelectric bodies and infrared detectors. With the development of modern information materials, the use of high-purity antimony is becoming more and more extensive. With the needs of equipment renewal and process development, the growth of heavily antimony-doped single-crystalline silicon by the CZ method is developing in the direction of larger diameter and lower resistivity, which means that the amount of high-purity antimony dopant required for a single doping is increasing. The existing preparation device for high-purity antimony dopant lacks heat preservation function, resulting in rapid heat loss during heating, which increases power consumption and takes a long time for high-purity antimony to melt, or even fails to melt, resulting in device failure. Summary of the invention

[0003] In view of the deficiencies of the existing problems, the present invention provides a preparation device and a preparation method of a high-purity antimony dopant to solve the existing problems raised in the above background technology.

[0004] To solve the above problems, the present invention is implemented through the following technical solutions: a preparation device for high-purity antimony dopant, comprising a base and a fixing clamp, the upper surface of the base is provided with a heat preservation device, the upper surface of the base is fixedly connected to a support frame, the outer surface of the fixing clamp is fixedly connected to a connecting rod, the outer surface of the connecting rod is fixedly connected to a connecting frame, the bottom of the connecting frame is fixedly connected to a supporting iron ring, the top of the supporting iron ring is provided with a quartz crucible, the top of the quartz crucible is provided with a cover plate, the top of the cover plate is provided with a seed crystal disassembly and assembly port, the top of the cover plate is provided with an air inlet pipe and an exhaust pipe, the heat preservation device comprises a base, the upper surface of the base is fixedly connected to a control box and a telescopic cylinder, the top of the telescopic cylinder is fixedly connected to a heat preservation shell, a vacuum chamber is provided inside the heat preservation shell, the inner cavity of the heat preservation shell is provided with a heating coil, and the outer surface of the heat preservation shell is fixedly connected to an electromagnetic heating controller.

[0005] Preferably, the fixing clip is arranged on the outer surface of the support frame, and high-purity antimony particles are arranged inside the quartz crucible.

[0006] Preferably, a sealing cover is provided inside the seed crystal disassembly and assembly port, and the outer surfaces of the air inlet pipe and the exhaust pipe penetrate the cover plate and extend to the inner cavity of the quartz crucible.

[0007] Preferably, the telescopic cylinder, the heat-insulating shell and the quartz crucible are arranged on the same central axis, and the supporting iron ring and the quartz crucible are arranged in a cavity inside the heating coil.

[0008] Preferably, a connecting terminal is fixedly connected to the top of the electromagnetic heating controller, the number of the connecting terminals is two, and the inside of the connecting terminal is fixedly connected to the two ends of the heating coil.

[0009] Preferably, a connecting wire is fixedly connected to the bottom of the electromagnetic heating controller, and one end of the connecting wire away from the electromagnetic heating controller is fixedly connected to the inside of the control box.

[0010] Preferably, a display screen is fixedly connected to the upper surface of the control box, and a first switch key and a second switch key are provided on the upper surface of the control box.

[0011] Preferably, a temperature sensor is fixedly connected to the bottom of the inner surface of the heat-insulating shell, and the telescopic cylinder, the electromagnetic heating controller and the temperature sensor are all electrically connected to the control box.

[0012] A preparation method of a preparation device for a high-purity antimony dopant comprises the following steps: placing a heat-insulating shell directly below a quartz crucible, adding high-purity antimony particles and seed crystals into the quartz crucible, covering the quartz crucible with a cover plate, introducing argon gas into the quartz crucible through an air inlet pipe, pressing a first switch key to control the extension of a telescopic cylinder, driving the heat-insulating shell to move upward until the quartz crucible is in the inner cavity of a heating coil, pressing a second switch key to energize the heating coil for heating, heating and melting the high-purity antimony particles, pressing the second switch key to stop heating, and pressing the first switch key to move the heat-insulating shell downward until the quartz crucible leaves the interior of the heating coil, and after the quartz crucible is cooled, removing the seed crystal and the antimony block and turning off the argon gas.

[0013] The present invention provides a device and method for preparing a high-purity antimony dopant. The device and method have the following beneficial effects:

[0014] 1. The preparation device of the high-purity antimony dopant, through the heat preservation device, is arranged in a liftable manner, so that the quartz crucible can be located in the inner cavity of the heating coil in the heat preservation shell during the preparation process, and the vacuum cavity in the heat preservation shell is used to achieve good heat preservation capacity. After the preparation is completed, the heat preservation shell is lowered by using a telescopic cylinder until the main body of the quartz crucible is exposed outside the heat preservation shell, thereby achieving good heat dissipation capacity, thereby realizing a single preparation of a large amount of high-purity antimony dopant with low power consumption.

[0015] 2. The preparation device of high-purity antimony dopant has an observation function realized through the cover plate and the seed crystal disassembly and assembly port if the quartz crucible is made of transparent quartz material. If the quartz crucible is made of non-transparent material, the seed crystal disassembly and assembly port serves as an observation window, thereby improving the practicability of the device and avoiding the situation inside the quartz crucible being opaque and unable to be observed. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0017] Figure 2 It is a schematic diagram of the structure of the entire preparation state of the present invention;

[0018] Figure 3 It is a schematic cross-sectional structure diagram of the present invention as a whole;

[0019] Figure 4 It is a partial structural schematic diagram of the present invention;

[0020] Figure 5 It is a schematic structural diagram of a quartz crucible of the present invention;

[0021] Figure 6 It is a schematic structural diagram of the heat preservation device of the present invention.

[0022] In the figure: 1. base; 2. support frame; 3. insulation device; 301. pedestal; 302. control box; 303. telescopic cylinder; 304. insulation shell; 305. vacuum chamber; 306. heating coil; 307. electromagnetic heating controller; 308. connecting terminal; 309. temperature sensor; 310. connecting line; 311. display screen; 312. first switch; 313. second switch; 4. fixing clip; 5. connecting rod; 6. connecting frame; 7. supporting iron ring; 8. quartz crucible; 9. cover plate; 10. seed crystal disassembly and assembly port; 11. sealing cover; 12. air inlet pipe; 13. exhaust pipe; 14. high purity antimony particles. DETAILED DESCRIPTION

[0023] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The embodiments of the present invention are provided for the purpose of illustration and description, and are not intended to be exhaustive or to limit the present invention to the disclosed forms. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments are selected and described in order to better illustrate the principles and practical applications of the present invention, and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific uses.

[0024] Example 1

[0025] like Figure 1-Figure 6As shown, the present invention provides a technical solution: a preparation device for a high-purity antimony dopant, comprising a base 1 and a fixing clamp 4, the upper surface of the base 1 is provided with a heat preservation device 3, the upper surface of the base 1 is fixedly connected with a support frame 2, the outer surface of the fixing clamp 4 is fixedly connected with a connecting rod 5, the outer surface of the connecting rod 5 is fixedly connected with a connecting frame 6, the bottom of the connecting frame 6 is fixedly connected with a supporting iron ring 7, the top of the supporting iron ring 7 is provided with a quartz crucible 8, the top of the quartz crucible 8 is provided with a cover plate 9, the top of the cover plate 9 A seed crystal disassembly and assembly port 10 is provided, an air inlet pipe 12 and an exhaust pipe 13 are arranged on the top of the cover plate 9, the insulation device 3 comprises a base 301, a control box 302 and a telescopic cylinder 303 are fixedly connected to the upper surface of the base 301, an insulation shell 304 is fixedly connected to the top of the telescopic cylinder 303, a vacuum chamber 305 is provided inside the insulation shell 304, a heating coil 306 is arranged in the inner cavity of the insulation shell 304, and an electromagnetic heating controller 307 is fixedly connected to the outer surface of the insulation shell 304.

[0026] The fixing clip 4 is arranged on the outer surface of the support frame 2 , and high-purity antimony particles 14 are arranged inside the quartz crucible 8 .

[0027] A sealing cover 11 is disposed inside the seed crystal disassembly and assembly port 10 . The outer surfaces of the air inlet pipe 12 and the air outlet pipe 13 penetrate the cover plate 9 and extend to the inner cavity of the quartz crucible 8 .

[0028] The telescopic cylinder 303 , the heat-insulating shell 304 and the quartz crucible 8 are arranged on the same central axis, and the supporting iron ring 7 and the quartz crucible 8 are arranged in a cavity inside the heating coil 306 .

[0029] A connection terminal 308 is fixedly connected to the top of the electromagnetic heating controller 307 . There are two connection terminals 308 . The inside of the connection terminal 308 is fixedly connected to the two ends of the heating coil 306 .

[0030] A connecting wire 310 is fixedly connected to the bottom of the electromagnetic heating controller 307 , and one end of the connecting wire 310 away from the electromagnetic heating controller 307 is fixedly connected to the inside of the control box 302 .

[0031] A display screen 311 is fixedly connected to the upper surface of the control box 302 , and a first switch key 312 and a second switch key 313 are disposed on the upper surface of the control box 302 .

[0032] A temperature sensor 309 is fixedly connected to the bottom of the inner surface of the heat-insulating shell 304 , and the telescopic cylinder 303 , the electromagnetic heating controller 307 and the temperature sensor 309 are all electrically connected to the control box 302 .

[0033] A preparation method of a preparation device for a high-purity antimony dopant comprises the following steps: placing a heat-insulating shell 304 directly below a quartz crucible 8, adding high-purity antimony particles 14 and seed crystals into the quartz crucible 8, covering the cover plate 9, introducing argon gas into the quartz crucible 8 through an air inlet pipe 12, pressing a first switch key 312 to control the extension of a telescopic cylinder 303, driving the heat-insulating shell 304 to move upward until the quartz crucible 8 is in the inner cavity of a heating coil 306, then pressing a second switch key 313 to energize and heat the heating coil 306, heating and melting the high-purity antimony particles 14, pressing the second switch key 313 to stop heating, and then pressing the first switch key 312 to move the heat-insulating shell 304 downward until the quartz crucible 8 leaves the interior of the heating coil 306, and after the quartz crucible 8 cools down, removing the seed crystal and the antimony block and turning off the argon gas.

[0034] When in use, a cover plate 9 is arranged above the quartz crucible 8, and a seed crystal disassembly port 10 is arranged on the cover plate 9. If the quartz crucible 8 is made of transparent quartz material, the observation function is realized. If the quartz crucible 8 is made of non-transparent material, the seed crystal disassembly port 10 serves as an observation window. The heat preservation device 3 is arranged in a liftable manner. During preparation, the fixing clip 4 is clamped at a suitable position on the support frame 2, so that the support iron ring 7 is at a suitable height, the quartz crucible 8 is placed on the support iron ring 7, and the heat preservation device 3 is in the quartz crucible. The quartz crucible 8 is placed below the quartz crucible 8, high-purity antimony particles 14 and seed crystals are added into the quartz crucible 8, the cover plate 9 is covered, argon gas is introduced into the quartz crucible 8 through the air inlet pipe 12, the first switch key 312 is pressed to control the extension of the telescopic cylinder 303, and the heat-insulating shell 304 is driven to move upward until the quartz crucible 8 is in the inner cavity of the heating coil 306, and the vacuum cavity 305 in the heat-insulating shell 304 is used to achieve good heat-insulating ability, and then the second switch key 313 is pressed to make the heating coil 306 in cooperation with the electromagnetic heating controller 307. 6 is powered on for heating, so that the high-purity antimony particles 14 are heated and melted. During the heating process, the temperature sensor 309 monitors the heating temperature in real time, and the temperature value is displayed on the display screen 311, so that the staff can understand the heating temperature in real time and achieve accurate heating. After the heating process is completed, the second switch key 313 is pressed to stop heating, and then the first switch key 312 is pressed to shorten the telescopic cylinder 303 to drive the insulation shell 304 to move downward until the quartz crucible 8 leaves the interior of the heating coil 306, so that the quartz crucible 8 is outside the insulation shell 304, achieving good heat dissipation capacity. After the quartz crucible 8 is cooled, the seed crystal and the antimony block are removed and the argon gas is turned off. The above process flow ensures that there is argon protection throughout the heating process, and ensures that the seed crystal and the high-purity antimony block are located above the insulation device 3 during the disassembly and assembly process, thereby protecting the seed crystal and the high-purity antimony. In addition, the quartz crucible 8 and the insulation shell 304 are both selected from the same grade of raw and auxiliary materials used for growing single crystal silicon by the Czochralski method, and the cover plate 9 is selected from quartz material or polytetrafluoroethylene material.

[0035] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field and related fields without creative work should fall within the scope of protection of the present invention. The structures, devices and operating methods not specifically described and explained in the present invention are implemented according to the conventional means in the field unless otherwise specified and limited.

Claims

1. A device for preparing a high-purity antimony dopant, comprising a base (1) and a fixing clamp (4), characterized in that: The upper surface of the base (1) is provided with a heat preservation device (3), the upper surface of the base (1) is fixedly connected to a support frame (2), the outer surface of the fixing clamp (4) is fixedly connected to a connecting rod (5), the outer surface of the connecting rod (5) is fixedly connected to a connecting frame (6), the bottom of the connecting frame (6) is fixedly connected to a supporting iron ring (7), the top of the supporting iron ring (7) is provided with a quartz crucible (8), the top of the quartz crucible (8) is provided with a cover plate (9), the top of the cover plate (9) is provided with a seed crystal disassembly port (10), and the cover plate (9) is provided with a seed crystal disassembly port (10). An air inlet pipe (12) and an exhaust pipe (13) are arranged at the top, and the heat preservation device (3) comprises a base (301), the upper surface of the base (301) is fixedly connected with a control box (302) and a telescopic cylinder (303), the top end of the telescopic cylinder (303) is fixedly connected with a heat preservation shell (304), a vacuum chamber (305) is provided inside the heat preservation shell (304), a heating coil (306) is arranged in the inner cavity of the heat preservation shell (304), and an electromagnetic heating controller (307) is fixedly connected to the outer surface of the heat preservation shell (304).

2. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: The fixing clamp (4) is arranged on the outer surface of the support frame (2), and high-purity antimony particles (14) are arranged inside the quartz crucible (8).

3. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: A sealing cover (11) is provided inside the seed crystal disassembly and assembly port (10), and the outer surfaces of the air inlet pipe (12) and the exhaust pipe (13) penetrate the cover plate (9) and extend to the inner cavity of the quartz crucible (8).

4. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: The telescopic cylinder (303), the heat-insulating shell (304) and the quartz crucible (8) are arranged on the same central axis, and the supporting iron ring (7) and the quartz crucible (8) are arranged in a cavity inside the heating coil (306).

5. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: A connecting terminal (308) is fixedly connected to the top of the electromagnetic heating controller (307), the number of the connecting terminals (308) is two, and the inside of the connecting terminal (308) is fixedly connected to the two ends of the heating coil (306).

6. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: A connecting wire (310) is fixedly connected to the bottom of the electromagnetic heating controller (307), and one end of the connecting wire (310) away from the electromagnetic heating controller (307) is fixedly connected to the inside of the control box (302).

7. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: A display screen (311) is fixedly connected to the upper surface of the control box (302), and a first switch key (312) and a second switch key (313) are provided on the upper surface of the control box (302).

8. The device for preparing a high-purity antimony dopant according to claim 1, characterized in that: A temperature sensor (309) is fixedly connected to the bottom of the inner surface of the heat-insulating shell (304), and the telescopic cylinder (303), the electromagnetic heating controller (307) and the temperature sensor (309) are all electrically connected to the control box (302).

9. A method for preparing a high-purity antimony dopant preparation device, characterized in that: The following steps are involved: The heat-insulating shell (304) is placed directly below the quartz crucible (8), high-purity antimony particles (14) and seed crystals are added into the quartz crucible (8), the cover plate (9) is covered, argon gas is introduced into the quartz crucible (8) through the air inlet pipe (12), the first switch key (312) is pressed to control the extension of the telescopic cylinder (303), and the heat-insulating shell (304) is driven to move upward until the quartz crucible (8) is in the inner cavity of the heating coil (306), and the second switch key (313) is pressed to energize the heating coil (306) for heating, so that the high-purity antimony particles (14) are heated and melted, the second switch key (313) is pressed to stop heating, and the first switch key (312) is pressed to move the heat-insulating shell (304) downward until the quartz crucible (8) leaves the interior of the heating coil (306), and after the quartz crucible (8) is cooled, the seed crystal and the antimony block are removed and the argon gas is turned off.

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