An intelligent impurity removal vacuum distillation furnace

Abstract

The present invention belongs to the technical field of crude indium impurity removal, and the present invention discloses an intelligent impurity removal vacuum distillation furnace; comprising a primary cavity, and also comprising: a secondary cavity and a tertiary cavity, wherein the primary cavity, the secondary cavity and the tertiary cavity are sequentially connected, the primary cavity is used to remove cadmium impurities in the crude indium raw material, the secondary cavity is used to remove zinc impurities in the crude indium raw material, and the tertiary cavity is used to stabilize the state of the indium melt. The present invention achieves the purpose of step-by-step removal of cadmium and zinc impurities by setting three cavities with different temperatures and vacuum degrees, and the three cavities can avoid the problem of co-volatilization, multi-stage gradient temperature control reduces ineffective heating, and reduces comprehensive energy consumption. The pulse heating of the primary cavity increases the volatilization rate of cadmium, and the intermittent cooling of the secondary cavity reduces the co-volatilization amount of zinc, accurately controls the volatilization of zinc, and the constant temperature control module of the tertiary cavity stabilizes the purity of the indium melt. The LIBS probe monitors in real time during the impurity removal process so as to adjust the parameters in real time.

Description

Technical Field

[0001] The present invention relates to the technical field of crude indium impurity removal, and more particularly to an intelligent impurity removal vacuum distillation furnace. Background Art

[0002] Crude indium is an important raw material for manufacturing semiconductor materials, such as indium arsenide and indium antimonide. It is widely used in infrared detectors, high-speed electronic devices and other fields. At present, crude indium is mainly removed by vacuum distillation furnaces. Vacuum distillation furnaces use the different saturated gas pressures of different substances under a certain temperature and vacuum state to separate them, thereby achieving the purpose of impurity removal.

[0003] Existing vacuum distillation furnaces lack multi-stage gradient separation, in-situ element monitoring and dynamic control technologies when removing impurities from crude indium, resulting in high impurity removal costs and unstable purity. For example, the co-volatilization of cadmium and zinc in the crude indium raw material leads to low separation efficiency and the inability to perform gradient separation. In addition, the impurity removal degree detection of the material relies on offline testing, and process adjustments lag behind. Summary of the Invention

[0004] The present invention proposes an intelligent impurity removal vacuum distillation furnace to solve the problem that the existing vacuum distillation furnace in the background technology lacks multi-stage gradient separation, in-situ element monitoring and dynamic control technology when removing impurities from crude indium.

[0005] To achieve the above-mentioned object, the present invention provides the following technical solution: an intelligent impurity removal vacuum distillation furnace, comprising a first-level cavity, and further comprising:

[0006] The secondary cavity and the tertiary cavity are connected in sequence. The primary cavity is used to remove cadmium impurities in the crude indium raw material, the secondary cavity is used to remove zinc impurities in the crude indium raw material, and the tertiary cavity is used to stabilize the state of the indium melt.

[0007] LIBS probes are installed on the side walls of the primary, secondary and tertiary cavities to analyze materials and determine the types and concentrations of elements.

[0008] Furthermore, a pulse heating module is provided in the first-level cavity, which is used to quickly vaporize cadmium through short-term high temperature. An intermittent cooling module is provided in the second-level cavity, which is used to accurately control the volatilization of zinc. A constant temperature control module is provided in the third-level cavity, which is used to ensure that the high-purity indium melt remains liquid at low temperature.

[0009] Furthermore, the tops and bottoms of the primary cavity, the secondary cavity and the tertiary cavity are all connected and fixedly connected with connecting pipes, and the connecting pipes are each provided with a vacuum fine-tuning valve, and a bellows is fixedly connected between the corresponding two connecting pipes.

[0010] Furthermore, the inner walls of the primary cavity, the secondary cavity and the tertiary cavity are fixedly connected to a first box body facing the connecting pipe through a cross bar, the first box body is connected and fixedly connected to a spiral slide, the bottom end of the spiral slide is connected and fixedly connected to an inclined slide, the bottom of the inner walls of the primary cavity, the secondary cavity and the tertiary cavity are fixedly connected to a second box body connected to the corresponding connecting pipe, the inclined slide is connected and fixedly connected to the second box body, and the LIBS probe is facing the inside of the second box body.

[0011] Furthermore, the side walls of the primary cavity, the secondary cavity and the tertiary cavity are fixed with two transparent boxes, the LIBS probe is arranged in the corresponding transparent box, and the other transparent boxes are provided with a reflector, which is used to focus the scattered light and reflect it back to the direction of the LIBS probe.

[0012] Furthermore, an electric push rod is installed in the transparent box, the output end of the electric push rod is fixedly connected to a movable plate, a rack is fixedly connected to the movable plate, one side of the rack is engaged with a gear, the middle part of the gear is fixedly connected to a rotating shaft, the rotating shaft is rotatably connected to the inner wall of the transparent box, a mounting block is fixedly connected to the rotating shaft, and the LIBS probe and reflector are respectively installed on the corresponding mounting blocks.

[0013] Furthermore, a high-temperature exhaust gas discharge pipe is provided on the first-level cavity, and the high-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the high-temperature exhaust gas and uses it to preheat the second-level cavity. A medium-temperature exhaust gas discharge pipe is provided on the second-level cavity, and the medium-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the medium-temperature exhaust gas and uses it to preheat the third-level cavity. An annular pipeline is provided in the third-level cavity, and liquid is provided in the annular pipeline. The liquid enters the heat exchanger, and the heat exchanger recovers the heat of the liquid and uses it to preheat the crude indium raw material warehouse.

[0014] A method for using an intelligent impurity removal vacuum distillation furnace comprises the following steps:

[0015] S1: inject the crude indium raw material from the raw material bin into the first box of the first-level cavity, and evacuate the three cavities to a suitable state;

[0016] S2: The pulse heating module is started, and the raw material becomes liquid and enters the second box through the spiral slide and the inclined slide. The cadmium vapor in the crude indium raw material is discharged to the heat exchanger through the high-temperature exhaust gas exhaust pipe. The heat exchanger recovers the heat to preheat the secondary cavity;

[0017] S3: The material flows into the secondary cavity through the connecting pipe and the bellows. The intermittent cooling module is activated, and the zinc vapor in the material evaporates. The zinc vapor enters the heat exchanger through the medium-temperature exhaust gas discharge pipe. The heat exchanger recovers the heat to preheat the tertiary cavity.

[0018] S4: The material enters the tertiary cavity, the constant temperature control module is started, and a high-purity indium melt is produced in the second box. The waste heat of the tertiary cavity is recovered by the heat exchanger and preheated in the raw material bin;

[0019] S5: Three LIBS probes monitor the cadmium and zinc concentrations in the three chambers in real time, and provide feedback to the system to adjust the temperature and vacuum level of the chambers.

[0020] The technical effects and advantages of the intelligent impurity removal vacuum distillation furnace of the present invention are as follows:

[0021] (1) By setting three cavities with different temperatures and vacuum degrees, the purpose of removing cadmium and zinc impurities in steps is achieved. The three cavities can avoid the problem of co-volatilization. The multi-stage gradient temperature control reduces ineffective heating and reduces the overall energy consumption. The pulse heating of the first-stage cavity increases the volatilization rate of cadmium. The intermittent cooling of the second-stage cavity reduces the co-volatilization amount of zinc and accurately controls the volatilization of zinc. The constant temperature control module of the third-stage cavity stabilizes the purity of the indium melt. The LIBS probe monitors in real time during the impurity removal process so that parameters can be adjusted in real time.

[0022] (2) By recycling the waste heat of the three cavities, the high-temperature exhaust gas discharged from the first-stage cavity is used to preheat the second-stage cavity through a heat exchanger, the medium-temperature exhaust gas discharged from the second-stage cavity is used to preheat the third-stage cavity through a heat exchanger, and the waste heat generated by the first-stage cavity is used to preheat the crude indium raw material in the raw material bin through a heat exchanger, thereby achieving the purpose of significantly reducing energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0024] Figure 2 is a schematic cross-sectional view of the cavity in the present invention;

[0025] Figure 3 It is a first cross-sectional schematic diagram of the transparent box in the present invention;

[0026] Figure 4 It is a first cross-sectional schematic diagram of the transparent box in the present invention;

[0027] Figure 5 Schematic diagram of the system module structure in the present invention;

[0028] Figure 6 This is a schematic diagram of the waste heat recovery module structure in the present invention.

[0029] In the picture:

[0030] 1. First-stage cavity; 2. Second-stage cavity; 3. Third-stage cavity; 4. Connecting pipe; 5. Vacuum fine-tuning valve; 6. Bellows; 7. First box; 8. Spiral slide; 9. Inclined slide; 10. Second box; 11. Transparent box; 12. LIBS probe; 13. Reflector; 14. Electric push rod; 15. Moving plate; 16. Rack; 17. Gear; 18. Rotating shaft; 19. Mounting block. DETAILED DESCRIPTION

[0031] The following will provide a clear and complete description of 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. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0032] Reference Figures 1-6 , an intelligent impurity removal vacuum distillation furnace, comprising a first-level cavity 1, and further comprising:

[0033] The secondary cavity 2 and the tertiary cavity 3 are connected in sequence. The primary cavity 1, the secondary cavity 2 and the tertiary cavity 3 are connected in sequence. The primary cavity 1 is used to remove cadmium impurities in the crude indium raw material, the secondary cavity 2 is used to remove zinc impurities in the crude indium raw material, and the tertiary cavity 3 is used to stabilize the state of the indium melt.

[0034] LIBS probes 12 are provided on the side walls of the primary chamber 1, the secondary chamber 2, and the tertiary chamber 3, and are used to analyze the material and determine the element types and concentrations;

[0035] The first-stage chamber 1 is equipped with a pulse heating module, which is used to quickly vaporize cadmium through short-term high temperature. The second-stage chamber 2 is equipped with an intermittent cooling module, which is used to accurately control the volatilization of zinc. The third-stage chamber 3 is equipped with a constant temperature control module, which is used to ensure that the high-purity indium melt remains liquid at low temperatures.

[0036] During use, the three cavities are evacuated to a suitable state, and the crude indium raw material in the raw material bin is put into the first-level cavity 1. The first-level cavity 1 applies a high-temperature pulse through the pulse heating module, and uses the low activation energy characteristics of cadmium to volatilize preferentially. After passing through the first-level cavity 1, the material reaches the second-level cavity 2. The second-level cavity 2 is intermittently cooled by the intermittent cooling module to achieve precise control of zinc volatilization and reduce the amount of zinc co-volatilization. The material finally reaches the third-level cavity 3. The third-level cavity 3 is constant-temperature controlled by the constant temperature control module to stabilize the indium melt and suppress the re-volatilization of impurities. Cadmium and zinc impurities are removed in stages through the three cavities to avoid the problem of co-volatilization. By setting the LIBS probe 12, the LIBS probe 12 emits a laser beam focused on the surface of the indium melt to generate plasma. The scattered light is focused on the optical fiber bundle and transmitted to the spectrometer for analysis. The type and concentration of the material are analyzed so that the temperature and vacuum degree of the cavity can be adjusted in real time to assist in impurity removal.

[0037] Reference Figure 1 The tops and bottoms of the first-stage cavity 1, the second-stage cavity 2 and the third-stage cavity 3 are all connected and fixedly connected with connecting pipes 4, and vacuum fine-tuning valves 5 are provided on the connecting pipes 4. A bellows 6 is fixedly connected between the corresponding two connecting pipes 4; the vacuum degree of the cavity is maintained by setting the vacuum fine-tuning valve 5 to feedback dynamic opening and closing, and the thermal expansion deformation is compensated by setting the bellows 6.

[0038] Reference Figure 2 The inner walls of the primary cavity 1, the secondary cavity 2 and the tertiary cavity 3 are all fixedly connected to a first box body 7 facing the connecting pipe 4 through a cross bar. A spiral slide 8 is connected and fixed to the first box body 7. The bottom end of the spiral slide 8 is connected and fixed to an inclined slide 9. The bottom of the inner walls of the primary cavity 1, the secondary cavity 2 and the tertiary cavity 3 are all fixedly connected to a second box body 10 connected to the corresponding connecting pipe 4. The inclined slide 9 is connected and fixed to the second box body 10. The LIBS probe 12 is facing the inside of the second box body 10. The crude indium raw material entering the primary cavity 1 is located in the first box body 7. When the temperature in the primary cavity 1 increases, the crude indium raw material becomes liquid. The liquid indium will enter the second box body 10 along the spiral slide 8 and the inclined slide 9. By providing the spiral slide 8, the indium can be heated evenly, the heating area of ​​the indium can be increased, and the heating process can be accelerated, which is conducive to the volatilization of impurities. The indium in the second box body 10 will enter the next cavity.

[0039] Reference Figure 2 、 Figure 3 and Figure 4Two transparent boxes 11 are fixed to the side walls of the first-level cavity 1, the second-level cavity 2, and the third-level cavity 3. LIBS probes 12 are set in the corresponding transparent boxes 11. Reflectors 13 are set in the other transparent boxes 11. The reflectors 13 are used to focus and reflect scattered light back to the direction of the LIBS probe 12; the LIBS probe 12 monitors the indium in the second box body 10. The LIBS probe 12 emits laser energy to vaporize the surface of the indium material, forming a high-temperature plasma and generating an elemental characteristic spectrum. The light signal emitted by the plasma (including characteristic spectral lines of elements such as cadmium and zinc) is scattered in all directions, and the reflector 13 focuses and reflects the scattered light back to the direction of the LIBS probe 12.

[0040] Reference Figure 3 and Figure 4 , an electric push rod 14 is installed in the transparent box 11, and a moving plate 15 is fixedly connected to the output end of the electric push rod 14, and a rack 16 is fixedly connected to the moving plate 15, and a gear 17 is meshed on one side of the rack 16. A rotating shaft 18 is fixedly connected to the middle of the gear 17, and the rotating shaft 18 is rotatably connected to the inner wall of the transparent box 11. A mounting block 19 is fixedly connected to the rotating shaft 18, and the LIBS probe 12 and the reflector 13 are respectively mounted on the corresponding mounting blocks 19; when it is necessary to adjust the angle of the LIBS probe 12 and the reflector 13, the electric push rod 14 is started, and the electric push rod 14 drives the moving plate 15 to move, and the moving plate 15 drives the rack 16 to move, and the rack 16 drives the rotating shaft 18 and the mounting block 19 to rotate through the gear 17, and the mounting block 19 drives the LIBS probe 12 and the reflector 13 to rotate, thereby achieving the purpose of adjusting the angle of the LIBS probe 12 and the reflector 13.

[0041] Reference Figure 6 The first-level cavity 1 is provided with a high-temperature exhaust gas discharge pipe, and the high-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the high-temperature exhaust gas and uses it to preheat the second-level cavity 2. The second-level cavity 2 is provided with a medium-temperature exhaust gas discharge pipe, and the medium-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the medium-temperature exhaust gas and uses it to preheat the tertiary cavity 3. An annular pipeline is provided in the tertiary cavity 3, and liquid is provided in the annular pipeline. The liquid enters the heat exchanger, and the heat exchanger recovers the heat of the liquid and uses it to preheat the crude indium raw material warehouse; the high-temperature cadmium vapor generated in the first-level cavity 1 enters the corresponding heat exchanger, and the heat exchanger recovers the heat of the cadmium vapor for preheating the second-level cavity 2. The medium-temperature zinc vapor generated in the second-level cavity 2 enters the corresponding heat exchanger, and the heat exchanger recovers the heat of the zinc vapor for preheating the tertiary cavity 3. The waste heat of the tertiary cavity 3 is recovered through the liquid in the annular pipeline and used to preheat the crude indium raw material warehouse, reducing energy consumption.

[0042] A method for using an intelligent impurity removal vacuum distillation furnace comprises the following steps:

[0043] S1: inject the crude indium raw material from the raw material bin into the first box body 7 of the first-level chamber 1, and evacuate the three chambers to a suitable state;

[0044] S2: The pulse heating module is started, and the raw material becomes liquid and enters the second box body 10 through the spiral slide 8 and the inclined slide 9. The cadmium vapor in the crude indium raw material is discharged to the heat exchanger through the high-temperature exhaust gas exhaust pipe. The heat exchanger recovers the heat to preheat the secondary chamber 2;

[0045] S3: The material flows into the secondary cavity 2 through the connecting pipe 4 and the bellows 6. The intermittent cooling module is started, and the zinc vapor in the material evaporates. The zinc vapor enters the heat exchanger through the medium-temperature exhaust gas discharge pipe. The heat exchanger recovers the heat to preheat the tertiary cavity 3.

[0046] S4: The material enters the tertiary cavity 3, and the constant temperature control module is started to produce a high-purity indium melt in the second box body 10. The waste heat of the tertiary cavity 3 is recovered by the heat exchanger and preheated to the raw material bin;

[0047] S5: The three LIBS probes 12 monitor the cadmium and zinc concentrations in the three chambers in real time, and feed back to the system to adjust the temperature and vacuum degree of the chambers.

[0048] The above description is merely a specific embodiment of the present application, but the scope of protection of the present application is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in this application should be included in the scope of protection of this application. Therefore, the scope of protection of this application should be based on the scope of protection of the claims.

[0049] Finally: The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An intelligent impurity removal vacuum distillation furnace, comprising a first-level cavity (1), characterized in that: Also includes: The secondary cavity (2) and the tertiary cavity (3) are connected in sequence. The primary cavity (1), the secondary cavity (2) and the tertiary cavity (3) are connected in sequence. The primary cavity (1) is used to remove cadmium impurities in the crude indium raw material. The secondary cavity (2) is used to remove zinc impurities in the crude indium raw material. The tertiary cavity (3) is used to stabilize the state of the indium melt. LIBS probes (12) are arranged on the side walls of the first-stage cavity (1), the second-stage cavity (2), and the third-stage cavity (3) and are used to analyze the material and determine the type and concentration of elements; The first-stage cavity (1) is provided with a pulse heating module, which is used to quickly vaporize cadmium through short-term high temperature; the second-stage cavity (2) is provided with an intermittent cooling module, which is used to accurately control the volatilization of zinc; the third-stage cavity (3) is provided with a constant temperature control module, which is used to ensure that the high-purity indium melt remains in a liquid state at a low temperature; The inner walls of the first-stage cavity (1), the second-stage cavity (2) and the third-stage cavity (3) are all fixedly connected to a first box body (7) facing the connecting pipe (4) through a cross bar, the first box body (7) is connected and fixedly connected to a spiral slideway (8), the bottom end of the spiral slideway (8) is connected and fixedly connected to an inclined slideway (9), the bottom of the inner walls of the first-stage cavity (1), the second-stage cavity (2) and the third-stage cavity (3) are all fixedly connected to a second box body (10) connected to the corresponding connecting pipe (4), the inclined slideway (9) is connected and fixedly connected to the second box body (10), and the LIBS probe (12) faces the inside of the second box body (10); Two transparent boxes (11) are fixedly connected to the side walls of the primary cavity (1), the secondary cavity (2) and the tertiary cavity (3); the LIBS probe (12) is arranged in the corresponding transparent box (11); and the other transparent boxes (11) are each provided with a reflector (13); the reflector (13) is used to focus and reflect scattered light back in the direction of the LIBS probe (12).

2. The intelligent impurity removal vacuum distillation furnace according to claim 1, characterized in that: The tops and bottoms of the first-stage cavity (1), the second-stage cavity (2) and the third-stage cavity (3) are all connected and fixedly connected with connecting pipes (4), each of which is provided with a vacuum fine-tuning valve (5), and a bellows (6) is fixedly connected between two corresponding connecting pipes (4).

3. The intelligent impurity removal vacuum distillation furnace according to claim 2, characterized in that: An electric push rod (14) is installed in the transparent box (11), and the output end of the electric push rod (14) is fixedly connected to a moving plate (15), and a rack (16) is fixedly connected to the moving plate (15), and a gear (17) is meshed on one side of the rack (16), and a rotating shaft (18) is fixedly connected to the middle of the gear (17), and the rotating shaft (18) is rotatably connected to the inner wall of the transparent box (11), and a mounting block (19) is fixedly connected to the rotating shaft (18), and the LIBS probe (12) and the reflector (13) are respectively mounted on the corresponding mounting blocks (19).

4. The intelligent impurity removal vacuum distillation furnace according to claim 3, characterized in that: The first-stage cavity (1) is provided with a high-temperature exhaust gas discharge pipe, and the high-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the high-temperature exhaust gas and applies it to the preheating of the second-stage cavity (2). The second-stage cavity (2) is provided with a medium-temperature exhaust gas discharge pipe, and the medium-temperature exhaust gas enters the corresponding heat exchanger through the discharge pipe. The heat exchanger recovers the heat of the medium-temperature exhaust gas and applies it to the preheating of the third-stage cavity (3). The third-stage cavity (3) is provided with an annular pipeline, and liquid is provided in the annular pipeline. The liquid enters the heat exchanger, and the heat exchanger recovers the heat of the liquid and applies it to the preheating of the crude indium raw material bin.

5. A method for using an intelligent impurity removal vacuum distillation furnace, using the intelligent impurity removal vacuum distillation furnace according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1: injecting the crude indium raw material from the raw material bin into the first box body (7) of the first-level cavity (1), and evacuating the three cavities to a suitable state; S2: Start the pulse heating module, the raw material becomes liquid and enters the second box body (10) from the spiral slide (8) and the inclined slide (9), and the cadmium vapor in the crude indium raw material is discharged to the heat exchanger through the high-temperature exhaust gas discharge pipe. The heat exchanger recovers the heat to preheat the secondary cavity (2); S3: The material flows into the secondary cavity (2) through the connecting pipe (4) and the bellows (6), and the intermittent cooling module is started. The zinc vapor in the material evaporates and enters the heat exchanger through the medium-temperature exhaust gas discharge pipe. The heat exchanger recovers the heat to preheat the tertiary cavity (3); S4: The material enters the tertiary cavity (3), the constant temperature control module is started, and a high-purity indium melt is produced in the second box (10). The waste heat of the tertiary cavity (3) is recovered by the heat exchanger and the raw material bin is preheated; S5: Three LIBS probes (12) monitor the cadmium and zinc concentrations in the three chambers in real time, feed back to the system and adjust the temperature and vacuum degree of the chamber.

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