An electronic diborane purification apparatus

Abstract

The present application relates to diborane purification technical field, and disclose an electronic diborane purification device, including: base, the top of base is connected with reaction tube, the top of reaction tube is connected with top cover, the top of top cover is connected with pipeline, the pipeline is equipped with micro flow controller, the bottom of base is connected with cold trap equipment through connecting pipe, the outside of reaction tube is equipped with heating assembly. The present application can be automatically sealed when the reaction tube is broken during the reaction, so that the leaked diborane is isolated and sealed, avoiding the leakage of diborane to the outside to harm the staff, through the separation of driving heating tube and arc plate and reaction tube, the gap between multiple arc plates becomes larger, so that the diborane in the isolation sleeve can be extracted faster during subsequent processing, the speed of extracting diborane is improved, and the processing efficiency is improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of diborane purification, and particularly relates to an electronic diborane purification device. BACKGROUND

[0002] In the electronic field of semiconductors, microelectronics and the like, "electronic grade" generally refers to a chemical with extremely high purity (such as 99.999% or more, i.e. 5N grade, or even higher) and extremely low impurity content (metal ions, moisture, hydrocarbons and other impurities <1 ppm) to meet the stringent requirements of "no impurity interference" for electronic device preparation, and electronic grade diborane is just such high purity diborane.

[0003] The method for obtaining high-order boranes is generated by micro-thermal decomposition of high-purity diborane. In use of the existing electronic grade diborane purification device, the diborane is introduced into the heated reaction tube, catalyzed by the catalyst arranged in the reaction tube, decomposed under the synergistic action of heat and catalysis, then rapidly cooled by the cold trap equipment, and finally high-order boranes are obtained to realize the purification of electronic grade diborane. However, when the reaction tube breaks, the existing purification device lacks countermeasures, causing the diborane to leak to the outside and causing a series of problems.

[0004] Therefore, it is necessary to invent an electronic diborane purification device to solve the above problems. SUMMARY

[0005] In view of the above problems, the present application provides an electronic diborane purification device to solve the problems raised in the background art.

[0006] To achieve the above purpose, the present application provides the following technical scheme:

[0007] An electronic diborane purification device, comprising: a base, a reaction tube connected above the base, a top cover connected to the top of the reaction tube, a pipeline connected to the top of the top cover, a micro-flow controller arranged on the pipeline, a cold trap equipment connected to the bottom of the base through a connecting pipe, a heating assembly arranged outside the reaction tube, an isolation assembly arranged at the bottom of the top cover and capable of isolating the reaction tube when the reaction tube breaks, and a catalytic assembly arranged inside the reaction tube and capable of catalyzing the reaction.

[0008] The isolation assembly comprises: an isolation sleeve, a ring plate, a sealing gasket, an electromagnetic valve, and a driving assembly for driving the ring plate to descend.

[0009] One end of the isolation sleeve is fixedly installed at the bottom of the top cover, the ring plate is fixedly installed at the bottom of the isolation sleeve, the sealing gasket is fixedly connected at the bottom of the ring plate, and the electromagnetic valve is arranged on the pipeline and the connecting pipe, respectively.

[0010] Further, the driving assembly comprises a slide rod, a first spring, a first iron rod, a first electromagnet, and a control assembly for controlling the power-off of the first electromagnet.

[0011] The slide rods are fixedly installed at the bottom of the top cover in equal intervals, the ring plate is sleeved outside the slide rods, the first spring is sleeved outside the slide rods, two ends of the first spring are fixedly connected with the bottom of the top cover and the top of the ring plate respectively, the first electromagnet is fixedly connected with the bottom of the top cover, the first iron rod is fixedly installed at the top of the ring plate, and the first iron rod is fixedly connected with the first electromagnet.

[0012] Further, the control assembly comprises a sensor and a controller.

[0013] The sensor is arranged in multiple groups, each group of the sensor comprises multiple sensors arranged from top to bottom, and multiple groups of the sensor are arranged outside the heating assembly in equal intervals, the controller is arranged at the bottom of the base, and the controller can control the power-off of the first electromagnet.

[0014] Further, the heating assembly comprises an arc-shaped plate, a heating pipe, a vertical plate, a sliding block and a second spring.

[0015] The heating pipe is connected to the inner side of the arc-shaped plate in equal intervals, the top of the base is provided with a sliding groove in equal intervals, the sliding block is slidingly installed in the sliding groove, the sliding block is fixedly connected with the corresponding arc-shaped plate, the second spring is fixedly connected with the inner wall of the sliding groove on the side, away from the center of the base, of the sliding block, the arc-shaped plates are arranged outside the reaction tube in equal intervals, gaps are formed between adjacent arc-shaped plates, the vertical plate is fixedly installed outside the arc-shaped plate, the sensor is fixedly connected to the inner side of the vertical plate, and the position of the sensor corresponds to the gap.

[0016] Further, the second iron rod is fixedly installed on the side, away from the center of the base, of the sliding block, the recess is formed in the inner wall of the side, away from the sliding block, of the sliding groove, the second electromagnet is fixedly installed in the recess, and the controller can control the second electromagnet.

[0017] Further, the catalytic assembly comprises a net rack, a net plate, a fixing rod, a cushion block and a catalyst.

[0018] The net rack is arranged in two pieces and fixedly connected by the fixing rods, the net plate is arranged in the net rack, the cushion block is fixedly installed in the reaction tube in a symmetrical manner, the lower net rack is located on the cushion block, and the catalyst is arranged on the lower net plate.

[0019] Further, the isolation sleeve and the sealing gasket are made of fluorine rubber.

[0020] Furthermore, the reaction tube is threadedly connected to the base and the top cover.

[0021] The technical effects and advantages of this invention are as follows:

[0022] 1. This invention can automatically seal the reaction tube when it ruptures during the reaction process, so that the leaked borane is sealed by the isolation sleeve, preventing borane from leaking to the outside and harming the workers.

[0023] 2. This invention drives the separation of the heating tube and the arc plate from the reaction tube, thereby increasing the gap between the multiple arc plates. This allows for faster removal of the borane from the isolation sleeve, improving the speed of borane removal and increasing processing efficiency. Attached Figure Description

[0024] Figure 1 A schematic diagram of the electronic diborane purification apparatus according to an embodiment of the present invention is shown;

[0025] Figure 2 A cross-sectional schematic diagram of the electronic diborane purification apparatus according to an embodiment of the present invention is shown;

[0026] Figure 3 An embodiment of the present invention is shown. Figure 2 Enlarged structural diagram at point A in the middle;

[0027] Figure 4 An embodiment of the present invention is shown. Figure 2 Enlarged structural diagram at point B;

[0028] Figure 5 A schematic diagram of a portion of the structure of an embodiment of the present invention is shown. Figure 1 ;

[0029] Figure 6 A schematic diagram of a portion of the structure of an embodiment of the present invention is shown. Figure 2 ;

[0030] Figure 7 A physical diagram of the present invention is shown;

[0031] In the diagram: 1. Base; 2. Reaction tube; 3. Top cover; 4. Isolation sleeve; 5. Ring plate; 6. Sealing gasket; 7. Sliding rod; 8. First spring; 9. First iron rod; 10. First electromagnet; 11. Sensor; 12. Arc plate; 13. Heating tube; 14. Vertical plate; 15. Sliding block; 16. Second spring; 17. Second iron rod; 18. Second electromagnet; 19. Cold trap device; 20. Pipeline; 21. Solenoid valve; 22. Microflow controller; 23. Grid frame; 24. Grid plate; 25. Power transmission line. Detailed Implementation

[0032] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments.

[0033] This invention provides an electronic diborane purification device, such as... Figures 1 to 6 As shown, it includes: a base 1, a reaction tube 2 connected to the top of the base 1, the reaction tube 2 being a quartz glass tube, a top cover 3 connected to the top of the reaction tube 2, a pipe 20 connected to the top of the top cover 3, a micro-flow controller 22 installed on the pipe 20, a cold trap device 19 connected to the bottom of the base 1 via a connecting pipe, the cold trap device 19 being a cold trap device used in chemical experiments in the prior art, a heating component installed on the outside of the reaction tube 2, an isolation component installed at the bottom of the top cover 3 that can isolate the reaction tube 2 in the event of a rupture, a catalytic component installed inside the reaction tube 2 that can catalyze the reaction, and a suction pipe 26 installed at the top of the top cover 3, with a valve inside the suction pipe 26. By connecting the suction pipe 26 to an external extraction device, the diborane sealed in the isolation sleeve 4 can be extracted for processing.

[0034] The isolation assembly includes: an isolation sleeve 4, an annular plate 5, a sealing gasket 6, a solenoid valve 21, and a drive assembly for driving the annular plate 5 to descend;

[0035] One end of the isolation sleeve 4 is fixedly installed at the bottom of the top cover 3, the ring plate 5 is fixedly installed at the bottom of the isolation sleeve 4, the sealing gasket 6 is fixedly connected to the bottom of the ring plate 5, and the solenoid valve 21 is respectively installed on the pipe 20 and the connecting pipe.

[0036] In use, pipe 20 is connected to the device for introducing diborane. The amount of gas added during the reaction is strictly controlled by microflow controller 22 to meet the reaction requirements. The reaction tube 2 is heated by heating component, and the diborane introduced into the reaction tube 2 is heated and catalyzed by catalytic component. Under the synergistic effect of heat and catalysis, it decomposes. The decomposition product is rapidly cooled by cold trap device 19 to obtain higher-order borane, thus purifying electronic-grade diborane.

[0037] During the experiment, if a crack appears on the surface of the reaction tube 2, the drive assembly drives the ring plate 5 to descend rapidly with the sealing gasket 6, which pulls open the isolation sleeve 4 so that the isolation sleeve 4 covers the outside of the reaction tube 2. At the same time, the solenoid valve 21 seals the pipe 20 and the connecting pipe. At this time, the isolation sleeve 4, together with the base 1, the ring plate 5, the sealing gasket 6, and the top cover 3, isolates the reaction tube 2, so that the leaked borane is sealed by the isolation sleeve 4, preventing borane from leaking to the outside and harming the staff.

[0038] like Figures 1 to 3 As shown, the drive assembly includes: a slide bar 7, a first spring 8, a first iron rod 9, a first electromagnet 10, and a control assembly for controlling the first electromagnet 10 to be de-energized.

[0039] The slide rods 7 are fixedly installed at the bottom of the top cover 3 at equal intervals, the ring plate 5 is slidably sleeved outside the plurality of slide rods 7, the first spring 8 is sleeved outside the slide rod 7, the two ends of the first spring 8 are fixedly connected with the bottom of the top cover 3 and the top of the ring plate 5 respectively, the first electromagnet 10 is fixedly connected with the bottom of the top cover 3, the first iron rod 9 is fixedly installed at the top of the ring plate 5, and the first iron rod 9 is adsorptively fixed with the first electromagnet 10.

[0040] When the reaction tube 2 is broken, a small amount of borane leaking at this time triggers the control assembly, the control assembly controls the first electromagnet 10 in power to be powered off, so that the first electromagnet 10 loses magnetism and loses adsorptive fixation of the first iron rod 9, and the compressed first spring 8 pushes the ring plate 5 to quickly descend with the sealing gasket 6, so that the isolation sleeve 4 is quickly pulled open.

[0041] As shown in Figure 1 and Figure 5 , the control assembly comprises a sensor 11 and a controller (not shown in the figure);

[0042] The sensor 11 is provided in multiple groups, the sensor 11 is an electrochemical sensor, each group of sensors 11 comprises a plurality of sensors 11 distributed from top to bottom, and the multiple groups of sensors 11 are distributed at equal intervals outside the heating assembly. The controller is arranged at the bottom of the base 1, the controller can control the first electromagnet 10 to be powered off, and the controller is a PLC controller.

[0043] When the reaction tube 2 is broken, the borane leaking is monitored by the sensor 11, the sensor 11 cooperates with the controller to control the first electromagnet 10 to be powered off, and the electromagnetic valve 21 is controlled to be closed at the same time, so that the pipeline 20 and the connecting pipe are closed, and at this time, the worker stops injecting borane.

[0044] As shown in Figures 2 to 4 , the heating assembly comprises an arc plate 12, a heating pipe 13, a vertical plate 14, a sliding block 15 and a second spring 16.

[0045] The heating pipe 13 is connected to the inner side of the arc plate 12 at equal intervals, the top of the base 1 is provided with a sliding groove at equal intervals around, the sliding block 15 is slidably installed in the sliding groove, the sliding block 15 is fixedly connected with the corresponding arc plate 12, the second spring 16 is fixedly connected with the inner wall of the sliding groove on the side of the sliding block 15 away from the center of the base 1, the arc plate 12 is distributed at equal intervals outside the reaction tube 2, and gaps are formed between adjacent arc plates 12. The vertical plate 14 is fixedly installed outside the arc plate 12, the sensor 11 is fixedly connected to the inner side of the vertical plate 14, the position of the sensor 11 corresponds to the gap, the heating pipe 13 is an electric heating pipe, a plurality of heating pipes 13 are connected through a power transmission line 25, and the bottom end of the power transmission line 25 extends to the outside and is connected with a power supply device below the base 1.

[0046] In use, the heating tube 13 is powered, the heating tube 13 heats the reaction tube 2, the leaked diborane is monitored by the sensor 11 through the gap, when the reaction tube 2 needs to be taken out, the arc-shaped plate 12 is pulled to move along the sliding groove with the sliding block 15, so that the heating tube 13 is away from the reaction tube 2, then the reaction tube 2 can be taken out, the second spring 16 is compressed when the sliding block 15 moves, after the reaction tube 2 is reset, the arc-shaped plate 12 is reset, the presence of the second spring 16 can resist the sliding block 15 and the arc-shaped plate 12, so that the heating tube 13 is tightly attached to the surface of the reaction tube 2, and the heating effect is guaranteed.

[0047] As shown in Figure 4 , the second iron rod 17 is fixedly installed on the side of the sliding block 15 away from the center of the base 1, a groove is formed in the inner wall of the side of the sliding groove away from the sliding block 15, and the second electromagnet 18 is fixedly installed in the groove.

[0048] The controller controls the second electromagnet 18 to be powered to have magnetism, so that the second iron rod 17 is attracted to move with the sliding block 15, the arc-shaped plate 12 and the heating tube 13, and finally the second iron rod 17 is adsorbed and fixed to the second electromagnet 18. At this time, the arc-shaped plate 12 and the heating tube 13 are away from the reaction tube 2, so that the gap is enlarged due to the movement of the adjacent arc-shaped plate 12 when the diborane in the isolation sleeve 4 is subsequently pumped out and treated, so that the diborane can be pumped out faster, the pumping speed of the diborane is improved, and whether the diborane in the isolation sleeve 4 is completely pumped out can be judged through the monitoring of the sensor 11.

[0049] As shown in Figure 2 , the catalytic assembly comprises a net rack 23, a net plate 24, a fixing rod, a cushion block and a catalyst (not shown in the figure).

[0050] The net rack 23 is provided in two, and the two net racks 23 distributed above and below are fixedly connected through a plurality of fixing rods. The net plate 24 is arranged inside the net rack 23. The cushion block is fixedly installed symmetrically inside the reaction tube 2. The lower net rack 23 is located on the cushion block. The catalyst is laid on the lower net plate 24.

[0051] The top cover 3 is separated from the reaction tube 2, and the net rack 23 and the net plate 24 are taken out from the reaction tube 2, and then the catalyst can be replaced.

[0052] As shown in Figure 3 , the materials of the isolation sleeve 4 and the sealing gasket 6 are fluorine rubber.

[0053] So that the isolation sleeve 4 and the sealing gasket 6 can withstand the high temperature around the reaction tube 2 after isolating the reaction tube 2.

[0054] As shown in Figure 2 , the reaction tube 2 is in threaded connection with the base 1 and the top cover 3.

[0055] The top cover 3 is separated from the reaction tube 2 by rotating, and the reaction tube 2 is separated from the base 1 by rotating, so that the reaction tube 2 is disassembled and cleaned.

[0056] Working principle: in use, the pipeline 20 is connected with a device for introducing diborane, the strict control of the amount of gas added in the reaction process is realized through the micro-flow controller 22, the reaction required is met, the reaction tube 2 is heated through the heating pipe 13, the diborane introduced into the reaction tube 2 is heated, and is catalyzed through the catalytic assembly, is decomposed under the synergistic action of heat and catalysis, and the decomposed product is rapidly cooled through the cold trap device 19 to obtain high-order boranes, so that the purification of the electronic-grade diborane is realized.

[0057] In the experiment, if the reaction tube 2 is broken, a small amount of leaked diborane is monitored by the sensor 11, the sensor 11 cooperates with the controller to control the first electromagnet 10 to be powered off, so that it loses magnetism and loses the adsorption and fixation of the first iron rod 9, the compressed first spring 8 pushes the ring plate 5 with the sealing gasket 6 to quickly descend, so that the isolation sleeve 4 is quickly pulled open, so that the isolation sleeve 4 covers the outside of the reaction tube 2, and finally the sealing gasket 6 is in contact with the base 1, and the electromagnetic valve 21 is closed, so that the pipeline 20 and the connecting pipe are closed, at this time the worker stops the injection of diborane, at this time the isolation sleeve 4 cooperates with the base 1, the ring plate 5, the sealing gasket 6 and the top cover 3 to isolate the reaction tube 2, so that the leaked diborane is sealed by the isolation sleeve 4, to avoid the leakage of diborane to the outside to harm the worker, and then the pipe 26 is connected with the external extraction device to extract the diborane sealed in the isolation sleeve 4 for treatment.

[0058] When the reaction tube 2 is broken, the controller controls the second electromagnet 18 to be powered on to have magnetism, so that the second iron rod 17 is attracted to move with the sliding block 15, the arc-shaped plate 12 and the heating pipe 13, and finally the second iron rod 17 is adsorbed and fixed with the second electromagnet 18, at this time the arc-shaped plate 12 and the heating pipe 13 are away from the reaction tube 2, so that when the diborane in the isolation sleeve 4 is extracted for treatment, the gap is enlarged due to the movement of the adjacent arc-shaped plate 12, so that the diborane can be extracted faster, the extraction speed of the diborane is improved, and the treatment efficiency is improved.

[0059] The above examples are only used to illustrate the technical solutions of the present application, but not limit it.

Claims

1. An electronic diborane purification device, characterized in that, include: A base (1) is provided, above which a reaction tube (2) is connected. A top cover (3) is connected to the top of the reaction tube (2). A pipe (20) is connected to the top of the top cover (3). A micro-flow controller (22) is installed on the pipe (20). A cold trap device (19) is connected to the bottom of the base (1) via a connecting pipe. A heating assembly is provided outside the reaction tube (2). An isolation assembly is provided at the bottom of the top cover (3) to isolate the reaction tube (2) in the event of a rupture. The reaction tube (2) is equipped with a catalytic component that can catalyze the reaction; the isolation component includes: an isolation sleeve (4), an annular plate (5), a sealing gasket (6), a solenoid valve (21), and a drive component for driving the annular plate (5) to descend; one end of the isolation sleeve (4) is fixedly installed at the bottom of the top cover (3), the annular plate (5) is fixedly installed at the bottom of the isolation sleeve (4), the sealing gasket (6) is fixedly connected to the bottom of the annular plate (5), and the solenoid valve (21) is respectively installed on the pipe (20) and the connecting pipe; The driving assembly includes: a slide rod (7), a first spring (8), a first iron rod (9), a first electromagnet (10), and a control assembly for controlling the first electromagnet (10) to de-energize; the slide rod (7) is equidistantly and fixedly installed around the bottom of the top cover (3), the ring plate (5) is slidably sleeved on the outside of the multiple slide rods (7), the first spring (8) is sleeved on the outside of the slide rod (7), the two ends of the first spring (8) are fixedly connected to the bottom of the top cover (3) and the top of the ring plate (5) respectively, the first electromagnet (10) is fixedly connected to the bottom of the top cover (3), the first iron rod (9) is fixedly installed on the top of the ring plate (5), and the first iron rod (9) and the first electromagnet (10) are attracted and fixed.

2. The electronic diborane purification apparatus according to claim 1, characterized in that: The control component includes: a sensor (11) and a controller; the sensor (11) is configured in multiple groups, each group of the sensor (11) includes multiple sensors (11) distributed from top to bottom, and the multiple groups of the sensor (11) are equidistantly distributed around the outside of the heating component; the controller is located at the bottom of the base (1), and the controller can control the first electromagnet (10) to be de-energized.

3. The electronic diborane purification apparatus according to claim 2, characterized in that: The heating assembly includes: an arc plate (12), a heating tube (13), a vertical plate (14), a slider (15), and a second spring (16); the heating tube (13) is equidistantly connected to the inner side of the arc plate (12), the top of the base (1) is equidistantly surrounded by a sliding groove, the slider (15) is slidably installed in the sliding groove, the slider (15) is fixedly connected to the corresponding arc plate (12), the second spring (16) fixes the side of the slider (15) away from the center of the base (1) to the inner wall of the sliding groove, the arc plates (12) are equidistantly distributed around the outside of the reaction tube (2), there is a gap between adjacent arc plates (12), the vertical plate (14) is fixedly installed on the outside of the arc plate (12), the sensor (11) is fixedly connected to the inner side of the vertical plate (14), and the position of the sensor (11) corresponds to the gap.

4. The electronic diborane purification apparatus according to claim 3, characterized in that: A second iron rod (17) is fixedly installed on the side of the slider (15) away from the center of the base (1). A groove is provided on the inner wall of the slide groove away from the slider (15). A second electromagnet (18) is fixedly installed in the groove. The controller can control the second electromagnet (18).

5. The electronic diborane purification apparatus according to claim 4, characterized in that: The catalytic assembly includes: a mesh frame (23), a mesh plate (24), a fixing rod, a pad, and a catalyst; the mesh frame (23) is configured as two, and the two mesh frames (23) distributed vertically are fixedly connected by multiple fixing rods. The mesh plate (24) is set inside the mesh frame (23). The pad is symmetrically fixedly installed inside the reaction tube (2). The lower mesh frame (23) is located on the pad, and the catalyst is laid on the lower mesh plate (24).

6. The electronic diborane purification apparatus according to claim 5, characterized in that: The isolation sleeve (4) and the sealing gasket (6) are both made of fluororubber.

7. The electronic diborane purification apparatus according to claim 6, characterized in that: The reaction tube (2) is threadedly connected to the base (1) and the top cover (3).

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