阅读说明：本技术 一种晶体材料区熔提纯装置 (Crystal material zone melting purification device ) 是由 罗亚南 郭关柱 于 2020-12-31 设计创作，主要内容包括：本发明涉及一种晶体材料区熔提纯装置,属于晶体材料制备技术领域,包括机架、支撑板、丝杆、支撑滑座、伺服驱动装置、支撑座、移动式区熔加热装置、透明防护罩、密封法兰盘、石英管、分支管路、主控管路、支管开关阀、真空泵、真空开关阀、密封盖、真空管；本发明利用分凝现象将晶体材料局部熔化形成狭窄的熔区,并将其沿锭长方向由一端按预定速度缓慢地移动到另一端,重复移动多次(多次区熔)使杂质被驱赶集中在材料锭的尾部和头部,将材料锭的尾部和头部切除后,从而获得提纯后的高纯度材料。(The invention relates to a crystal material zone-melting purification device, which belongs to the technical field of crystal material preparation and comprises a frame, a support plate, a screw rod, a support sliding seat, a servo driving device, a support seat, a movable zone-melting heating device, a transparent protective cover, a sealing flange plate, a quartz tube, a branch pipeline, a main control pipeline, a branch tube switch valve, a vacuum pump, a vacuum switch valve, a sealing cover and a vacuum tube; the invention utilizes segregation phenomenon to melt crystal material locally to form a narrow melting zone, and the narrow melting zone is slowly moved from one end to the other end along the length direction of the ingot at a preset speed, and is repeatedly moved for a plurality of times (zone melting for a plurality of times) to drive impurities to be concentrated at the tail part and the head part of the material ingot, and the tail part and the head part of the material ingot are cut off, thereby obtaining the purified high-purity material.)

1. A crystal material zone melting purification device is characterized in that: the crystal material zone melting purification device comprises a rack (1), supporting plates (2), guide rods (3), supporting sliding seats (4), a servo driving device (5), a supporting seat (6), a movable zone melting heating device (7), a transparent protective cover (8), a sealing flange (9), a quartz tube (10), branch pipelines (11), a main pipeline (12), a branch pipe switch valve (13), a vacuum pump (14), a vacuum switch valve (15), a sealing cover (16) and a vacuum tube (17), wherein the top of the rack (1) is provided with two parallel supporting plates (2), the two supporting plates (2) are provided with two guide rods (3), the supporting sliding seats (4) are arranged on the guide rods (3), the supporting seats (6) are arranged on the two supporting sliding seats (4), the bottom of the supporting seats (6) is connected with the servo driving device (5) arranged on the top of the rack (1), at least two sets of movable zone-melting heating devices (7) are arranged at the top of the supporting seat (6), and a heating hole is formed in the middle of each movable zone-melting heating device (7); a transparent protective cover (8) is arranged at the top of the frame (1), a pair of sealing flange discs (9) which are right opposite to each set of movable zone-melting heating device (7) are arranged on two side walls of the transparent protective cover (8), the central holes of the pair of sealing flange discs (9) and the heating holes on the corresponding movable zone-melting heating devices (7) are on the same straight line, a quartz tube (10) penetrates through the two ends of the later period of the heating holes on the corresponding movable zone-melting heating devices (7) and is fixed on the sealing flange discs (9), a sealing cover (16) is arranged at the open end of the quartz tube (10), a branch pipeline (11) is arranged on the sealing cover (16), the branch pipeline (11) is communicated with a main pipeline (12), a branch switch valve (13) is arranged on the branch pipeline (11), the main pipeline (12) is connected with a vacuum tube (17), and the vacuum pump (, the vacuum pipe (17) is provided with a vacuum switch valve (15), the vacuum switch valve (15) and the branch pipe switch valve (13) are connected with a PLC (programmable logic controller) controller (22), and the PLC controller (22) is connected with the vacuum pump (14).

2. The apparatus of claim 1, wherein: the movable zone-melting heating device (7) comprises a heating cover body (18), a heat-insulating layer (19), a heating couple (20) and a heating sleeve (31), wherein the heating cover body (18) is installed on the supporting seat (6), a heating hole is formed in the middle of the heating cover body (18), the heating sleeve (31) is arranged on the inner wall, close to one side of the heating hole, of the inner cavity of the heating cover body (18), the heating sleeve (31) is fixed on the heating cover body (18), the heat-insulating layer (19) is arranged on the inner wall of the heating cover body (18), the heating couple (20) is installed in a cavity between the heat-insulating layer (19) and the heating sleeve (31), and heat-conducting holes (34) are formed in two end walls of the heating hole of the heating.

3. The apparatus of claim 2, wherein: a cavity between the temperature heat insulation layer (19) and the heating sleeve (31) is internally provided with a temperature sensor (32), the temperature sensor (32) is connected with a PLC (programmable logic controller) (22), and the PLC (22) is connected with a heating couple (20) through a relay.

4. A zone-melting purification apparatus for crystalline material as claimed in any one of claims 1 to 3, wherein: the hydrogen-supply device is characterized in that a hydrogen pipeline (23) is arranged on the main pipeline (12), the hydrogen pipeline (23) is connected with a hydrogen tank (24), a hydrogen switch valve (25) is arranged on the hydrogen pipeline (23), and the hydrogen switch valve (25) is controlled by a PLC (programmable logic controller) (22).

5. The apparatus for zone-melting purification of crystalline material as claimed in any one of claims 1 to 4, wherein: the main pipeline (12) is provided with a nitrogen pipeline (27), the nitrogen pipeline (27) is connected with a nitrogen tank (26), the nitrogen pipeline (27) is provided with a nitrogen switch valve (28), and the nitrogen switch valve (28) is in control connection with the PLC (22).

6. The apparatus for zone-melting purification of crystalline material as claimed in any one of claims 1 to 5, wherein: the hydrogen leakage sensor (36) is arranged nearby the inner cavity of the transparent protective cover (8), the connecting pipeline, the switch valve, the sealing flange and the like, the hydrogen leakage sensor (36) is connected with the PLC (programmable logic controller) (22), and the PLC (22) is connected with the alarm lamp (37).

Technical Field

The invention belongs to the technical field of crystal material preparation, and particularly relates to a crystal material zone melting purification device.

Background

When preparing multi-component crystal materials, other trace components or metal impurities contained in each component raw material can influence the growth and synthesis of the crystal materials, so that materials with excellent performance cannot be prepared, and each raw material needs to be purified.

When the high-performance multi-component single crystal material is prepared, raw materials are required to be purified, and the materials are directly collected after being volatilized in the purification process by the pre-purification equipment purchased in the current market, so that the purity of the materials purified by the purification equipment is not enough, and the final purity of the raw materials required by the growth of single crystals such as tellurium, zinc and cadmium reaches the standard of 7N (99.99999 percent), so that the growth requirement of the three-component tellurium, zinc and cadmium single crystal material can be met. The purity of the primarily purified components can reach the 5N (99.999%) standard, and the materials need to be purified again to meet the requirement of synthesizing high-performance materials on purity.

Disclosure of Invention

In order to overcome the problems in the prior art, the invention provides a crystal material zone melting and purifying device, which utilizes the segregation phenomenon to locally melt the material to form a narrow melting zone, slowly moves the material from one end to the other end along the length direction of an ingot at a preset speed, repeatedly moves for multiple times (zone melting) to enable impurities to be concentrated at the tail part and the head part of the material ingot, and obtains a purified high-purity material after cutting off the tail part and the head part of the material ingot.

In order to realize the purpose, the invention is realized by the following technical scheme:

a zone melting purification device for crystal materials comprises a frame 1, a support plate 2, a guide rod 3, a support slide 4, a servo drive device 5, a support seat 6, a movable zone melting heating device 7, a transparent protective cover 8, a sealing flange 9, a quartz tube 10, a branch pipeline 11, a main pipeline 12, a branch switch valve 13, a vacuum pump 14, a vacuum switch valve 15, a sealing cover 16 and a vacuum tube 17, the top of the rack 1 is provided with two sets of parallel supporting plates 2, the two supporting plates 2 are provided with two guide rods 3, the guide rods 3 are provided with a supporting slide seat 4, a supporting seat 6 is arranged on the two supporting slide seats 4, the bottom of the supporting seat 6 is connected with a servo driving device 5 arranged at the top of the rack 1, the top of the supporting seat 6 is provided with at least two sets of movable zone-melting heating devices 7, and the middle part of each movable zone-melting heating device 7 is provided with a heating hole; a transparent protective cover 8 is arranged at the top of the frame 1, a pair of sealing flange plates 9 which are opposite to each set of movable zone-melting heating device 7 are arranged on two side walls of the transparent protective cover 8, the central holes of the pair of sealing flange plates 9 and the heating holes on the corresponding movable zone-melting heating devices 7 are on the same straight line, the quartz tube 10 passes through the later two ends of the heating holes on the corresponding movable zone-melting heating devices 7 and is fixed on the sealing flange plates 9, a sealing cover 16 is arranged at the opening end of the quartz tube 10, a branch pipeline 11 is arranged on the sealing cover 16, the branch pipeline 11 is communicated with a main pipeline 12, a branch switch valve 13 is arranged on the branch pipeline 11, the main pipeline 12 is connected with a vacuum tube 17, the vacuum tube 17 is connected with a vacuum pump 14, a vacuum switch valve 15, the branch switch valve 13 is connected with a PLC 22, and the PLC 22 is connected with the vacuum pump 14.

Further, the movable zone-melting heating device 7 comprises a heating cover body 18, a heat insulation layer 19, a heating couple 20 and a heating sleeve 31, the heating cover body 18 is installed on the supporting seat 6, a heating hole is formed in the middle of the heating cover body 18, the heating sleeve 31 is arranged on the inner wall of the inner cavity of the heating cover body 18 close to the heating hole, the heating sleeve 31 is fixed on the heating cover body 18, the heat insulation layer 19 is arranged on the inner wall of the heating cover body 18, the heating couple 20 is installed in a cavity between the heat insulation layer 19 and the heating sleeve 31, and heat conduction holes 34 are formed in two end walls of the heating hole of the heating cover body 18.

Further, a temperature sensor 32 is installed in a cavity between the thermal insulation layer 19 and the heating jacket 31, the temperature sensor 32 is connected with the PLC controller 22, and the PLC controller 22 is connected with the heating couple 20 through a relay.

Further, a hydrogen pipeline 23 is arranged on the main pipeline 12, the hydrogen pipeline 23 is connected with a hydrogen tank 24, a hydrogen switch valve 25 is arranged on the hydrogen pipeline 23, and the hydrogen switch valve 25 is controlled by the PLC controller 22.

Further, the main pipeline 12 is provided with a nitrogen pipeline 27, the nitrogen pipeline 27 is connected with a nitrogen tank 26, the nitrogen pipeline 27 is provided with a nitrogen switch valve 28, and the nitrogen switch valve 28 is in control connection with the PLC controller 22.

Further, hydrogen leakage sensors 36 are arranged near the inner cavity of the transparent protective cover 8, the connecting pipeline, the switch valve, the sealing flange and the like, the hydrogen leakage sensors 36 are connected with the PLC 22, and the PLC 22 is connected with an alarm lamp 37.

The invention has the beneficial effects that:

the invention utilizes the segregation phenomenon to melt the material locally to form a narrow melting zone, and slowly moves the melting zone from one end to the other end along the length direction of the ingot at a preset speed, and repeatedly moves for a plurality of times (zone melting for a plurality of times) to concentrate impurities on the tail part and the head part of the material ingot, and after the tail part and the head part of the material ingot are cut off, the purified high-purity material is obtained.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is a front view of the present invention;

FIG. 3 is a schematic structural view of a mobile zone-melting heating apparatus according to the present invention;

FIG. 4 is a schematic diagram of a control circuit according to the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

As shown in fig. 1-4, a zone melting purification device for crystalline materials comprises a frame 1, a support plate 2, a guide rod 3, a support slide 4, a servo drive device 5, a support base 6, a movable zone melting heating device 7, a transparent shield 8, a sealing flange 9, a quartz tube 10, a branch pipeline 11, a main pipeline 12, a branch switch valve 13, a vacuum pump 14, a vacuum switch valve 15, a sealing cover 16 and a vacuum tube 17. The top of frame 1 install two sets of parallel backup pads 2, install two guide arms 3 on two backup pads 2, install a support slide 4 on the guide arm 3, supporting seat 6 installs on two support slides 4, the bottom of supporting seat 6 is connected with the servo drive device 5 who installs at frame 1 top, servo drive device 5 be lead screw nut mechanism, its actuating mechanism is servo motor, the bottom of supporting seat 6 is connected with the nut slider who installs on the lead screw. At least two sets of movable zone-melting heating devices 7 are arranged at the top of the supporting seat 6, and a heating hole is formed in the middle of each movable zone-melting heating device 7; a transparent protective cover 8 is arranged at the top of the frame 1, a pair of sealing flange plates 9 which are opposite to each set of movable zone-melting heating device 7 are arranged on two side walls of the transparent protective cover 8, the central holes of the pair of sealing flange plates 9 and the heating holes on the corresponding movable zone-melting heating devices 7 are on the same straight line, the quartz tube 10 passes through the later two ends of the heating holes on the corresponding movable zone-melting heating devices 7 and is fixed on the sealing flange plates 9, a sealing cover 16 is arranged at the opening end of the quartz tube 10, a branch pipeline 11 is arranged on the sealing cover 16, the branch pipeline 11 is communicated with a main pipeline 12, a branch switch valve 13 is arranged on the branch pipeline 11, the main pipeline 12 is connected with a vacuum tube 17, the vacuum tube 17 is connected with a vacuum pump 14, a vacuum switch valve 15, the branch switch valve 13 is connected with a PLC 22, and the PLC 22 is connected with the vacuum pump 14. Putting a material to be purified into a quartz tube 10, then penetrating the quartz tube 10 through a heating hole on a corresponding movable zone melting heating device 7, installing two ends of the quartz tube on a pair of sealing flange plates 9 which are opposite to two side walls on a transparent protective cover 8, supporting and fixing the quartz tube 10, packaging the quartz tube 10 through a sealing cover 16, opening a vacuum switch valve 15 and a branch switch valve 13 after the quartz tube 10 is packaged, and vacuumizing the inner cavity of the quartz tube 10 by a vacuum pump 14 by opening the vacuum switch valve 15 and the branch switch valve 13. After the inner cavity of the quartz tube 10 is in a vacuum state, the hydrogen switch valve 25 is opened, high-purity hydrogen in the hydrogen tank 24 is injected into the inner cavity of the quartz tube 10 through the hydrogen pipeline 23, and residual trace oxygen in the inner cavity of the quartz tube 10 is discharged, so that the phenomenon that oxidation reaction between the trace oxygen and a crystal material affects the purity of the material is prevented; the movable zone melting heating device 7 is controlled to heat to the melting temperature of the crystal material, and the supporting slide seat 4 drives the movable zone melting heating device 7 to do linear reciprocating motion along the guide rod 3 through the supporting seat 6 under the driving control of the servo driving device 5. Therefore, the material is locally melted to form a narrow melting zone by utilizing the segregation phenomenon, the movable zone-melting heating device 7 slowly moves from one end to the other end along the length direction of the crystal material ingot, and the movable zone-melting heating device repeats zone melting for multiple times to ensure that impurities in the crystal material are concentrated at the tail part and the head part of the quartz tube 10, and the tail part and the head part of the crystal material are cut off, so that the aim of purifying the crystal material is fulfilled.

In the invention, the movable zone-melting heating device 7 comprises a heating cover body 18, a heat-insulating layer 19, a heating couple 20 and a heating sleeve 31, wherein the heating cover body 18 is arranged on a supporting seat 6, the middle part of the heating cover body 18 is provided with a heating hole, the heating sleeve 31 is arranged on the inner wall of one side of the inner cavity of the heating cover body 18 close to the heating hole, the heating sleeve 31 is fixed on the heating cover body 18, the heat-insulating layer 19 is arranged on the inner wall of the heating cover body 18, the heating couple 20 is arranged in a cavity between the heat-insulating layer 19 and the heating sleeve 31, and heat-conducting holes 34 are arranged on two end walls of the heating hole. The heating sleeve 31 is heated by electrifying the heating couple 20, the heat-insulating layer 19 can prevent the temperature from diffusing outwards, after the heating sleeve 31 is heated, the heating sleeve 31 heats the crystal material in the quartz tube 10, under the drive control of the servo driving device 5, the supporting slide seat 4 drives the movable zone-melting heating device 7 to do linear reciprocating motion along the guide rod 3 through the supporting seat 6, the crystal material of the quartz tube 10 is locally melted to form a narrow melting zone by utilizing the segregation phenomenon, the movable zone-melting heating device 7 slowly moves from one end to the other end along the length direction of the crystal material ingot, and the impurities in the crystal material are concentrated on the tail part and the head part of the quartz tube 10 repeatedly. Because the heat conduction holes 34 are formed on the two end walls of the heating hole of the heating cover body 18, the heat dissipation of the temperature at the two ends of the heating cover body 18 can be faster than the heat dissipation of the temperature at the middle part, so that a temperature interval reduced from the middle part to the two ends is established, the formation of a narrow melting area required by zone melting is facilitated, the movable zone melting heating device 7 is slowly moved from one end to the other end along the length direction of a crystal material ingot, and the impurities in the crystal material can be concentrated at the tail part and the head part of the crystal material ingot purified in the quartz tube 10 by repeating (zone melting for multiple times), so that the purification of the crystal material is realized.

In the invention, a temperature sensor 32 is arranged in a cavity between the temperature heat insulation layer 19 and the heating jacket 31, the temperature sensor 32 is connected with the PLC 22, and the PLC 22 is connected with the heating couple 20 through a relay. Because the heating temperatures of different components in the material are different, the heating temperature is within the range of 300-1300 ℃ after the heating couple 20 is electrified; the temperature sensor 32 detects the temperature in real time, transmits a temperature signal to the PLC 22, and the PLC 22 controls the heating couple 20 to realize heating, so that different impurities in the material can be driven to be concentrated on the tail and the head of the quartz tube 10.

The main pipeline 12 is provided with a hydrogen pipeline 23, the hydrogen pipeline 23 is connected with a hydrogen tank 24, the hydrogen pipeline 23 is provided with a hydrogen switch valve 25, and the hydrogen switch valve 25 is controlled by a PLC 22. Flowing high-purity hydrogen is introduced into the chamber of the quartz tube 10 to remove trace oxygen in the chamber and prevent the material in the quartz tube 10 from being oxidized.

The main pipeline 12 is provided with a nitrogen pipeline 27, the nitrogen pipeline 27 is connected with a nitrogen tank 26, the nitrogen pipeline 27 is provided with a nitrogen switch valve 28, and the nitrogen switch valve 28 is controlled by the PLC 22. The transparent protective cover 8 inner chamber, connecting line and ooff valve and sealing flange etc. near be provided with hydrogen leakage sensor 36, hydrogen leakage sensor 36 is connected with PLC controller 22, PLC controller 22 is connected with alarm lamp 37. When the hydrogen leakage sensor 36 detects hydrogen leakage, an alarm signal is sent to the PLC controller 22, an alarm lamp 37 gives an alarm, meanwhile, the PLC controller 22 automatically controls to close the heating couple 20 and the hydrogen switch valve 25, open the nitrogen switch valve 28 and introduce flowing high-purity nitrogen into the cavity of the quartz tube 10 so as to prevent the hydrogen mixed gas from burning and exploding in the zone melting purification device.

Finally, it is noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.