A diborane production synthesis device and synthesis process

Abstract

The present application relates to the field of semiconductor technology, and discloses a diborane production synthesis device and synthesis process. The production synthesis device includes a reaction tank body, a first rotating plate is provided at the bottom of the reaction tank body, the first rotating plate and the bottom wall of the reaction tank body are surrounded by a first gas collecting chamber, the first rotating plate and the side wall of the reaction tank body are surrounded by a reaction chamber, a vertical first air duct is provided on the side of the first rotating plate close to the reaction chamber, the first air duct is connected to the first gas collecting chamber, and a plurality of air holes for boron trichloride gas to pass through are opened on the periphery of the first air duct; a driving component is provided on the periphery of the reaction tank body, and the driving component drives the first rotating plate and the first air duct to revolve around the central axis of the reaction tank body. In the present application, the driving component drives the first rotating plate and the first air duct to rotate around the central axis of the reaction tank body, so that boron trichloride can contact with a larger range of sodium borohydride, thereby improving the production efficiency of diborane.

Description

Technical Field

[0001] The present application relates to the field of semiconductor technology, and in particular to a diborane production synthesis device and synthesis process. Background Art

[0002] Diborane is an inorganic compound that plays an important role in the semiconductor industry, especially as a P-type doping source for silicon materials. In the semiconductor production process, diborane is used in the epitaxial growth, passivation, diffusion and ion implantation of silicon and germanium. Therefore, diborane is widely used in the production of semiconductor integrated circuits, semiconductor light-emitting devices and other fields.

[0003] There are several different methods for the industrial production of diborane. For example, diborane (B2H6) can be produced by reacting sodium borohydride (NaBH4) with boron trichloride (BCl3). Sodium borohydride (solid) reacts with boron trichloride (gas) in a solvent (liquid) to produce diborane (B2H6). The above method produces fewer by-products and is suitable for the preparation of high-purity diborane.

[0004] Sodium borohydride is a solid white crystal, and boron trichloride is a gas. To make the two react, sodium borohydride needs to be dissolved in a certain solvent to form a mixed solution. Subsequently, the boron trichloride gas is introduced into the mixed solution through a pipe, so that the boron trichloride and sodium borohydride come into contact and react to generate diborane gas.

[0005] However, after boron trichloride is introduced into the mixed solution, it will move upward along a stable moving path after coming out of the pipeline outlet; that is, boron trichloride gas reacts more with sodium borohydride in a small range around the moving path, while sodium borohydride far away from the pipeline outlet is difficult to react with boron trichloride; thereby affecting the synthesis efficiency of diborane and the concentration of synthesized diborane. Summary of the invention

[0006] In order to improve the production efficiency of diborane, the present application provides a diborane production synthesis device and a synthesis process.

[0007] The present application provides a diborane production synthesis device and synthesis process, which adopts the following technical scheme:

[0008] A diborane production and synthesis device comprises a mixing tank body, a reaction tank body, a boron trichloride storage tank, a protective gas storage tank, a vacuum component and a collecting component connected by pipelines; the mixing tank body is used to mix sodium borohydride and a solvent into a mixed solution, the reaction tank body is connected to the mixing tank body, the reaction tank body is provided with a liquid inlet for the mixed solution to be added, the reaction tank body is provided with a first air inlet and a second air inlet, the first air inlet is connected to the protective gas storage tank, the second air inlet is connected to the boron trichloride storage tank, the reaction tank body is also provided with a first air outlet and a second air outlet, the first air outlet is connected to the vacuum component, the vacuum component is used to evacuate the reaction tank body, the second air outlet is connected to the collecting component, the collecting component is used to collect the diborane generated in the reaction tank body; the bottom of the reaction tank body is provided with a A first rotating plate is provided, and the first rotating plate and the side wall of the reaction tank body are arranged to form a reaction chamber, and the reaction chamber is used to accommodate a mixed solution. The first rotating plate and the bottom wall of the reaction tank body are arranged to form a first gas collecting chamber, and the first gas collecting chamber is connected with a first air inlet. A vertical first air duct is provided on the side of the first rotating plate close to the reaction chamber, and the first air duct is connected with the first gas collecting chamber. A plurality of air holes for boron trichloride gas to pass through are opened on the periphery of the first air duct; a driving assembly is provided on the periphery of the reaction tank body, and the driving assembly includes a rotating motor, a first gear and a first gear ring, the first gear ring is coaxially fixed with the first rotating plate, the first gear is fixedly connected to the driving end of the rotating motor, the first gear is meshed with the first gear ring, and the driving assembly drives the first air duct to revolve around the central axis of the reaction tank body.

[0009] By adopting the above technical solution, boron trichloride gas enters the first gas collecting chamber through the first gas inlet and is transported to the mixed solution in the reaction chamber through the first gas duct, so that boron trichloride reacts with sodium borohydride in the mixed solution to generate diborane.

[0010] Since the driving component drives the first rotating plate and the first air duct to rotate around the central axis of the reaction tank body, after the boron trichloride gas is discharged from the first air duct, the boron trichloride gas is spirally distributed in the mixed solution, so that the gas discharged from the first air duct can be diffused in a larger range in the mixed solution, so that the boron trichloride can contact with a larger range of sodium borohydride, thereby improving the production efficiency of diborane.

[0011] Optionally, the outer periphery of the first air guide tube is fixed to a gas-liquid separation membrane, the gas-liquid separation membrane covers the air holes, and the boron trichloride gas passes through the gas-liquid separation membrane into the reaction chamber.

[0012] By adopting the above technical solution, a gas-liquid separation membrane is arranged on the periphery of the first gas duct, so that only boron trichloride gas is allowed to expand from the first gas collecting chamber to the reaction chamber, while the mixed solution is prevented from flowing from the reaction chamber to the first gas collecting chamber, thereby facilitating the input of boron trichloride.

[0013] Optionally, the first air duct includes a spiral pipe segment and a straight pipe segment, the spiral pipe segment and the straight pipe segment are integrally formed, the spiral pipe segment is arranged in the reaction chamber, and the straight pipe segment passes through the first rotating plate and extends into the first gas collecting chamber; the air holes are arranged at intervals along the outer circumference of the spiral pipe.

[0014] By adopting the above technical solution, when boron trichloride diffuses from the air holes of the first air duct into the reaction chamber, the boron trichloride moves along a specific route. By configuring the first air duct to be a spiral tube segment and a straight tube segment, and providing the air holes on the spiral tube segment, when the boron trichloride moves upward, the overlapping portion of the boron trichloride on the vertical projection surface can be reduced; that is, the diffusion range of the boron trichloride on the horizontal projection surface is expanded, so that the boron trichloride can react with a wider range of sodium borohydride, so as to further improve the production efficiency of diborane.

[0015] Optionally, the outer diameter of the spiral tube segment increases or decreases along a direction away from the first gas collecting chamber.

[0016] By adopting the above technical solution, the outer diameter of the spiral pipe section increases or decreases, thereby further improving the diffusion range of boron trichloride gas in the horizontal direction, further promoting the reaction of boron trichloride and sodium borohydride, and further improving the production efficiency of diborane.

[0017] Optionally, the first air duct is rotatably connected to the first rotating plate, and a sealing ring is provided between the straight pipe section and the first rotating plate; a second gear ring is fixedly provided on the inner side of the bottom wall of the reaction tank body, and a second gear is fixedly provided at the end of the straight pipe section, and the second gear is meshed with the inner ring of the second gear ring; the second gear ring is located on the vertical projection plane of the revolution trajectory of the first air duct, and the second gear ring is used to drive the first air duct to rotate; the straight pipe section is provided with an air inlet channel for gas to enter and exit, and the air inlet channel is arranged in the first gas collecting chamber.

[0018] By adopting the above technical solution, when the driving component drives the first air duct to rotate around the central axis of the reaction tank body, the second gear on the outer periphery of the straight pipe segment meshes with the second gear ring, thereby driving the first air duct to rotate; thereby, the boron trichloride gas can be fully mixed with the mixed solution on the outer periphery of the first air duct, so as to further improve the reaction of the boron trichloride gas and sodium borohydride, and improve the synthesis efficiency of diborane.

[0019] Optionally, the reaction tank body is further provided with a second rotating plate, a partition plate, a second air duct and an air collecting pipe, and the second rotating plate and the tank top of the reaction tank body are surrounded by a second air collecting chamber; the driving components are provided with two, and the two driving components drive the first rotating plate and the second rotating plate to rotate respectively, and the first rotating plate and the second rotating plate rotate at the same frequency, the partition plate is fixedly arranged on the side of the second rotating plate close to the first rotating plate, and the partition plate is vertically arranged, the partition plate is inserted into the mixed solution, the partition plate divides the second rotating plate into a first component and a second component, the first component is arranged opposite to the first air duct, and the partition plate divides the reaction chamber into a first reaction chamber and a second reaction chamber; the first component is provided with a breathable mesh hole, and the breathable mesh hole is used for allowing the gas in the first reaction chamber to enter the second gas collecting chamber; the second air duct is fixedly arranged on the side of the second component close to the first rotating plate, the first end of the second air duct is communicated with the second gas collecting chamber, the second end of the second air duct is inserted into the mixed solution, and an avoidance gap is provided between the second end of the second air duct and the first rotating plate; the gas collecting pipe is fixedly arranged on the side of the second component away from the first rotating plate, one end of the gas collecting pipe is communicated with the second reaction chamber, and the other end of the gas collecting pipe is externally connected to the collection component.

[0020] By adopting the above technical solution, the partition plate divides the reaction chamber into the first reaction chamber and the second reaction chamber, so that the boron trichloride flows through the first gas collecting chamber, the first reaction chamber, the second gas collecting chamber, the second gas guide pipe, the second reaction chamber in sequence, and finally discharges from the reaction tank from the gas collecting pipe. Thus, the adsorption path of boron trichloride is extended, the dissolution effect of boron trichloride in the mixed solution is improved, and the synthesis efficiency of boron trichloride and sodium borohydride is further improved.

[0021] Optionally, an aerator is fixedly provided at the second end of the second air guide pipe.

[0022] By adopting the above technical solution, the aerator can improve the dispersion degree of boron trichloride gas in the second reaction chamber to further promote the reaction of boron trichloride and sodium borohydride.

[0023] Optionally, a stainless steel blade is fixedly provided on the outer periphery of the second air duct, and the stainless steel blade is spirally wrapped around the outer peripheral wall of the second air duct at 45 degrees.

[0024] By adopting the above technical solution, the stainless steel blade can disturb the mixed solution to promote the uniform distribution of sodium borohydride in the mixed solution, so as to facilitate the full reaction of boron trichloride and sodium borohydride.

[0025] A diborane production synthesis process comprises the following steps:

[0026] Gas environment preparation: The vacuum component evacuates the reaction tank, and the protective gas storage tank delivers protective gas to the reaction tank to displace the impurity gas in the reaction tank and pipelines;

[0027] Preparation of mixed solution: weigh sodium borohydride solid powder and solvent according to the formula ratio, stir the sodium borohydride and solvent in a mixing tank to dissolve the sodium borohydride in the solvent, and transport the mixed solution to the reaction chamber of the reaction tank;

[0028] Reaction temperature preparation: adjust the temperature inside the reaction tank;

[0029] Preparation of boron trichloride gas: Place the boron trichloride storage tank on an electronic scale, and determine the input amount of boron trichloride gas according to the value change on the electronic scale. The input amount of boron trichloride matches the amount of boron hydrogen warner added to meet the diborane synthesis formula;

[0030] Preparation of diborane gas: the driving assembly drives the first rotating plate and the first air guide pipe to rotate, and the boron trichloride storage tank transports boron trichloride gas to the reaction tank body; the boron trichloride gas flows through the first gas collecting chamber, the first air guide pipe, and the reaction chamber in sequence, and the boron trichloride reacts with sodium borohydride to synthesize diborane;

[0031] Diborane gas transportation: The gas in the reaction tank is transported to the collecting component, which separates and purifies the diborane gas in the gas and then fills the diborane gas into a steel cylinder.

[0032] A diborane production synthesis process comprises the following steps:

[0033] Preparation of diborane gas: the driving assembly synchronously drives the first rotating plate, the first air duct, the second rotating plate and the second air duct to rotate, and the boron trichloride storage tank transports boron trichloride gas to the reaction tank body; the boron trichloride gas flows through the first gas collecting chamber, the first air duct, the first reaction chamber, the second gas collecting chamber, the second air duct and the second reaction chamber in sequence, and boron trichloride reacts with sodium borohydride to synthesize diborane.

[0034] In summary, the present application includes at least one of the following beneficial technical effects:

[0035] The driving assembly drives the first rotating plate and the first air guide pipe to rotate around the central axis of the reaction tank body, so that when the boron trichloride gas is discharged from the first air guide pipe, the boron trichloride gas is distributed in a spiral shape in the mixed solution, so that the gas discharged from the first air guide pipe can be diffused in a larger range in the mixed solution, so that the boron trichloride can contact with a larger range of sodium borohydride, thereby improving the production efficiency of diborane;

[0036] When the driving assembly drives the first air guide tube to rotate around the central axis of the reaction tank body, the second gear on the outer periphery of the straight tube segment meshes with the second gear ring, thereby driving the first air guide tube to rotate; thereby, the boron trichloride gas can be fully mixed with the mixed solution on the outer periphery of the first air guide tube, so as to further improve the reaction of the boron trichloride gas and sodium borohydride, and improve the synthesis efficiency of diborane;

[0037] The partition plate divides the reaction chamber into a first reaction chamber and a second reaction chamber, so that the boron trichloride flows through the first gas collecting chamber, the first reaction chamber, the second gas collecting chamber, the second gas guide pipe, the second reaction chamber in sequence, and finally discharges from the reaction tank from the gas collecting pipe. Thus, the adsorption path of the boron trichloride is extended, and the dissolution effect of the boron trichloride in the mixed solution is improved, so as to further improve the synthesis efficiency of the boron trichloride and the sodium borohydride. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 It is a schematic diagram showing the structure of the diborane production synthesis device in Example 1.

[0039] Figure 2 It is a cross-sectional view showing the structure of the reaction tank in Example 1.

[0040] Figure 3 yes Figure 2 Enlarged view of point A in the middle.

[0041] Figure 4 yes Figure 2 Enlarged view of point B in the middle.

[0042] Figure 5 It is a cross-sectional view showing the structure of the reaction tank in Example 3.

[0043] Figure 6 It is a cross-sectional view showing the structure of the reaction tank in Example 4.

[0044] Figure 7 yes Figure 6 Enlarged view of point C in the middle.

[0045] Explanation of reference numerals: 1, mixing tank; 11, first delivery pipeline; 12, first valve; 13, circular track; 14, avoidance gap; 15, first gas collection chamber; 16, reaction chamber; 161, first reaction chamber; 162, second reaction chamber; 17, second gas collection chamber; 18, sealing sleeve; 19, second gear; 20, second gear ring; 2, reaction tank; 21, first rotating plate; 22, first air guide pipe; 221, air vent; 222, spiral pipe section; 223, straight pipe section; 2231, air inlet channel; 23, second rotating plate; 231, first component; 2311, air mesh; 232, second component; 24, partition plate; 25, second guide Gas pipe; 26, gas collecting pipe; 27, gas-liquid separation membrane; 3, protective gas storage tank; 31, second delivery pipeline; 32, second valve; 4, boron trichloride storage tank; 41, third delivery pipeline; 42, third valve; 5, vacuum assembly; 51, fourth delivery pipeline; 52, fourth valve; 6, collecting assembly; 61, fifth delivery pipeline; 62, fifth valve; 7, drainage pipeline; 71, sixth valve; 8, driving assembly; 81, rotating motor; 82, first gear; 83, first gear ring; 9, containing shell; 100, temperature control jacket; 1001, medium chamber; 110, insulation jacket; 120, temperature control delivery pipe; 130, aerator; 140, stainless steel blade. DETAILED DESCRIPTION

[0046] The following is combined with Figure 1-7 This application is described in further detail.

[0047] Example 1

[0048] The present application embodiment discloses a diborane production synthesis device. Figure 1 The diborane production synthesis device comprises a mixing tank body 1, a reaction tank body 2, a protective gas storage tank 3, a boron trichloride storage tank 4, a vacuum component 5 and a collection component 6 connected by pipelines. For the convenience of description, the arrow direction of the drawings in the specification is the flow direction of the gas.

[0049] Sodium borohydride is a solid white crystal, and boron trichloride is a gas. To make the two react, sodium borohydride must be dissolved in a certain solvent to form a mixed solution; then, boron trichloride gas is introduced into the mixed solution, so that boron trichloride and sodium borohydride synthesize diborane gas at a specific temperature. Ethylene glycol dimethyl ether is a water-white neutral liquid with an ether smell, which is stable in nature, not easy to react, and can dissolve sodium borohydride; therefore, this embodiment uses ethylene glycol dimethyl ether as a solvent to dissolve sodium borohydride solid powder.

[0050] Reference Figure 1 and Figure 2The mixing tank 1 is used to mix sodium borohydride and solvent into a mixed solution. The reaction tank 2 is connected to the mixing tank 1 through a first delivery pipe 11. The reaction tank 2 is provided with a liquid inlet for the mixed solution. At the same time, the first delivery pipe 11 is provided with a first valve 12 for controlling the on-off of the first delivery pipe 11 and the flow rate of the mixed solution. A stirrer is provided in the mixing tank 1 for stirring and mixing ethylene glycol dimethyl ether and sodium borohydride so that sodium borohydride is fully dissolved in the ethylene glycol dimethyl ether solution; the stirrer can be a common stirrer such as an electromagnetic stirrer.

[0051] Reference Figure 1 and Figure 2 The reaction tank body 2 is the place where sodium borohydride and boron trichloride synthesize diborane, and is also the main invention of this application. In this embodiment, the reaction tank body 2 is cylindrical. The bottom of the reaction tank body 2 is connected to the protective gas storage tank 3 through the second delivery pipeline 31. The tank body is provided with a first air inlet connected to the second delivery pipeline 31. The second delivery pipeline 31 is provided with a second valve 32, and the second valve 32 is used to control the opening and closing of the second delivery pipeline 31. The protective gas can be an inactive gas such as nitrogen and argon. In this embodiment, the protective gas is nitrogen.

[0052] Reference Figure 1 and Figure 2 At the same time, the bottom of the reaction tank body 2 is connected to the boron trichloride storage tank 4 through the third delivery pipe 41. The tank body is provided with a second air inlet connected to the third delivery pipe 41. The third delivery pipe 41 is provided with a third valve 42, and the third valve 42 is used to control the on-off of the second delivery pipe 31.

[0053] Reference Figure 1 and Figure 2 The reaction tank body 2 is also provided with a first gas outlet and a second gas outlet. The first gas outlet is connected to the vacuum assembly 5 through a fourth delivery pipe 51. The vacuum assembly 5 is used to evacuate the reaction tank body 2. The fourth delivery pipe 51 is provided with a fourth valve 52. The fourth valve 52 is used to control the on-off of the second delivery pipe 31. The second gas outlet is connected to the collection assembly 6 through a fifth delivery pipe 61. The collection assembly 6 is used to collect the diborane generated in the reaction tank body 2. The fifth delivery pipe 61 is provided with a fifth valve 62. The fifth valve 62 is used to control the on-off of the second delivery pipe 31.

[0054] Reference Figure 1 and Figure 2 The reaction tank body 2 is also provided with a drain port, which is connected to the sewage treatment equipment through a drain pipe 7; after the boron trichloride reacts with the sodium borohydride, the drain pipe 7 is used to discharge the remaining liquid in the reaction tank body 2. The drain pipe 7 is provided with a sixth valve 71, which is used to control the on-off of the drain pipe 7.

[0055] It is worth noting that the reaction tank body 2 is also provided with several conventional devices in the chemical industry, such as temperature detectors, pressure detectors, pressure reducing valves, etc., to facilitate the synthesis of diborane, which are not indicated in the drawings of the specification of this application.

[0056] Reference Figure 2 and Figure 3 The inner chamber of the reaction tank body 2 is provided with a first rotating plate 21, a first air guide tube 22, a second rotating plate 23, a partition plate 24, a second air guide tube 25 and an air collecting tube 26. A driving assembly 8 is provided outside the reaction tank body 2, and two driving assemblies 8 are provided, and the two driving assemblies 8 drive the first rotating plate 21 and the second rotating plate 23 to rotate respectively.

[0057] Reference Figure 2 , the first rotating plate 21 and the second rotating plate 23 are arranged horizontally, the first rotating plate 21 is arranged at the bottom area of ​​the reaction tank body 2, and the second rotating plate 23 is arranged at the upper area of ​​the reaction tank body 2. The first rotating plate 21 and the second rotating plate 23 are both rotatably connected with the reaction tank body 2, and the first rotating plate 21 and the second rotating plate 23 rotate synchronously. This embodiment takes the first rotating plate 21 as an example for explanation. The inner circumferential wall of the reaction tank body 2 is provided with a circumferential track 13, and the first rotating plate 21 cooperates with the circumferential track 13 to realize the rotatable connection between the first rotating plate 21 and the reaction tank body 2, and the inner circumference of the reaction tank body 2 is also provided with an avoidance ring groove for accommodating the first rotating plate 21. The first rotating plate 21 is connected to the inner circumferential wall of the reaction tank body 2 through a sealing ring to improve the sealing between the first rotating plate 21 and the reaction tank body 2.

[0058] Reference Figure 2 The first rotating plate 21 and the bottom wall of the reaction tank body 2 are surrounded by a first gas collecting chamber 15 , and the second delivery pipeline 31 for delivering protective gas and the third delivery pipeline 41 for delivering boron trichloride are both connected to the first gas collecting chamber 15 .

[0059] Reference Figure 2 The first rotating plate 21, the second rotating plate 23 and the reaction tank body 2 are surrounded by a reaction chamber 16, and the reaction chamber 16 provides a reaction space for the reaction of boron trichloride and sodium borohydride. The first delivery pipeline for delivering the mixed solution is connected to the reaction chamber 16 to achieve the purpose of delivering the mixed solution into the reaction tank body 2.

[0060] Reference Figure 2 and Figure 3The first air guide pipe 22 is vertically arranged and fixed to the side of the first rotating plate 21 close to the reaction chamber 16. The first air guide pipe 22 is connected to the first gas collecting chamber 15. The outer periphery of the first air guide pipe 22 is provided with a plurality of air holes 221 for the boron trichloride gas to pass through. In this embodiment, two second air guide pipes 25 are arranged at intervals along the radial direction of the reaction tank body 2.

[0061] Reference Figure 2 and Figure 4 In this embodiment, the outer periphery of the first air duct 22 is fixed to the gas-liquid separation membrane 27 (also called gas selective permeation membrane or gas separation membrane), the gas-liquid separation membrane 27 covers the air permeability 221, and the boron trichloride gas passes through the gas-liquid separation membrane 27 to enter the reaction chamber 16; the gas-liquid separation membrane 27 only allows the boron trichloride gas to expand from the first gas collecting chamber 15 to the reaction chamber 16, and prevents the mixed solution from flowing from the reaction chamber 16 to the first gas collecting chamber 15, thereby facilitating the input of the boron trichloride gas.

[0062] Reference Figure 2 , the second rotating plate 23 and the tank top of the reaction tank body 2 are surrounded to form a second gas collecting chamber 17, the partition plate 24 is fixedly arranged on the side of the second rotating plate 23 close to the first rotating plate 21, and the partition plate 24 is arranged vertically. Under normal conditions, the partition plate 24 is inserted into the mixed solution (the horizontal dotted line in the figure is the liquid surface of the mixed solution). The partition plate 24 divides the reaction chamber 16 into a first reaction chamber 161 and a second reaction chamber 162. The partition plate 24 can abut against the inner circumferential wall of the reaction tank body 2, or an avoidance distance is provided between the partition plate 24 and the inner circumferential wall of the reaction tank body 2, so that the partition plate 24 can rotate with the second rotating plate 23. The partition plate 24 divides the second rotating plate 23 into a first part 231 and a second part 232. The first part 231 is arranged opposite to the first air duct 22, that is, the first air duct 22 is arranged on the vertical projection surface of the first part 231. The first component 231 is provided with a plurality of air-permeable mesh holes 2311 , and the air-permeable mesh holes 2311 are used to allow the gas in the first reaction chamber 161 to enter the second gas collecting chamber 17 .

[0063] Reference Figure 2 The second air duct 25 is fixedly disposed on a side of the second component 232 close to the first rotating plate 21 , a first end of the second air duct 25 is communicated with the second gas collecting chamber 17 , a second end of the second air duct 25 is inserted into the mixed solution, and an avoidance gap is provided between the second end of the second air duct 25 and the first rotating plate 21 .

[0064] Reference Figure 2The gas collecting pipe 26 is fixedly arranged on the side of the second component 232 away from the first rotating plate 21. One end of the gas collecting pipe 26 is connected to the second reaction chamber 162. The other end of the gas collecting pipe 26 is connected to the vacuum component 5 and the collecting component 6 through a pipeline. The collecting component 6 is used to collect and separate the generated diborane.

[0065] Reference Figure 2 and Figure 3 The two driving components 8 drive the first rotating plate 21 and the second rotating plate 23 to rotate respectively, and the first rotating plate 21 rotates at the same frequency as the second rotating plate 23. This embodiment takes the driving component 8 driving the first rotating plate 21 as an example to explain the specific structure of the driving component 8.

[0066] Reference Figure 2 and Figure 3 The main body of the driving assembly 8 is fixedly arranged on the outer periphery of the reaction tank body 2, and a housing 9 is arranged on the outer periphery of the reaction tank body 2, and the driving assembly 8 is fixedly arranged in the housing 9. The driving assembly 8 includes a rotating motor 81, a first gear 82 and a first gear ring 83. The first gear ring 83 is fixedly arranged on the outer periphery of the first rotating plate 21, and the first gear ring 83 is coaxially fixed with the first rotating plate 21. The first gear 82 is fixedly connected to the driving end of the rotating motor 81. The reaction tank body 2 is provided with an avoidance notch 14. The first gear 82 is meshed with the first gear ring 83 through the avoidance notch 14. The driving assembly 8 drives the first air duct 22 to revolve around the central axis of the reaction tank body 2.

[0067] Reference Figure 2 and Figure 3 , the outer periphery of the reaction tank body 2 is also provided with a temperature control jacket 100 and a heat preservation jacket 110, and the temperature control jacket 100 and the heat preservation jacket 110 are arranged between the two driving components 8. The temperature control jacket 100 is sleeved on the outer periphery of the reaction tank body 2, and the temperature control jacket 100 is used to control the temperature in the reaction tank body 2, so that boron trichloride and sodium borohydride can react under specific reaction temperature conditions to improve the production quality of diborane. In this embodiment, a medium chamber 1001 is provided in the temperature control jacket 100 for accommodating fluid media of different temperatures. The medium chamber 1001 is connected to an external temperature control device through a temperature control delivery pipe 120, and the temperature control device can transport fluid media of different temperatures into the medium chamber 1001 to control the temperature in the reaction tank body 2. Temperature detectors are provided in the medium chamber 1001 and the reaction tank body 2, and are connected to the back-end terminal computer, and the back-end terminal computer controls the temperature of the fluid medium flowing in and out, as well as the flow rate of the fluid medium, to control the temperature in the reaction tank body 2. The fluid medium can be heat transfer medium such as heat transfer oil and nitrogen, and this embodiment does not limit the fluid medium. The insulation jacket 110 is made of insulation materials such as rock wool and composite silicate, and this embodiment does not limit the specific material and specific structure of the insulation jacket 110.

[0068] The implementation principle of a diborane production synthesis device in the embodiment of the present application is:

[0069] Reference Figures 1 to 4 The vacuum component 5 is a vacuum component including a vacuum pump, and the vacuum component 5 performs vacuum treatment on the reaction tank body 2 and the pipeline. Subsequently, the protective gas storage tank 3 delivers protective gas to the reaction tank body 2, thereby completing the gas replacement in the reaction tank body 2 and several pipelines. In this embodiment, the protective gas is nitrogen to reduce the production cost of diborane; in other embodiments, the protective gas can also be an inert gas such as argon.

[0070] Subsequently, the mixed solution in the mixing tank body 1 is transported to the reaction tank body 2 through the first transport pipe 11, and the pressure of the reaction tank body 2 is controlled between the working pressures. At the same time, the reaction tank body 2 and the mixed solution in the reaction tank body 2 are heated by the temperature control jacket 100, so that the temperature in the reaction tank body 2 reaches the temperature required for the reaction of boron trichloride and sodium borohydride.

[0071] Next, the driving assembly 8 drives the first rotating plate 21 , the first air duct 22 , the second rotating plate 23 , the partition plate 24 , and the second air duct 25 to rotate around the central axis of the reaction tank body 2 .

[0072] Finally, the boron trichloride gas enters the first gas collecting chamber 15 through the third delivery pipe 41 and is delivered to the mixed solution in the reaction chamber 16 through the first gas guide pipe 22, so that the boron trichloride reacts with the sodium borohydride in the mixed solution to generate diborane.

[0073] Since the driving assembly 8 drives the first rotating plate 21 and the first air duct 22 to rotate continuously around the central axis of the reaction tank body 2, the first air duct 22 continuously performs a circular motion. Therefore, after the boron trichloride gas is discharged from the first air duct 22, the boron trichloride gas is distributed in a spiral shape in the mixed solution, so that the boron trichloride gas discharged from the first air duct 22 can be diffused in a larger range in the mixed solution, so that the boron trichloride can contact with a larger range of sodium borohydride, thereby improving the production efficiency of diborane.

[0074] At the same time, the partition plate 24 divides the reaction chamber 16 into the first reaction chamber 161 and the second reaction chamber 162, so that the boron trichloride flows through the first gas collecting chamber 15, the first reaction chamber 161, the second gas collecting chamber 17, the second gas guide pipe 25, the second reaction chamber 162 in sequence, and finally discharges the reaction tank body 2 from the gas collecting pipe 26. Thereby, the adsorption path of the boron trichloride is extended, and the dissolution effect of the boron trichloride in the mixed solution is improved, so as to further improve the synthesis efficiency of the boron trichloride and the sodium borohydride; that is, the production efficiency of diborane and the synthesis purity of diborane are improved.

[0075] It is worth noting that after boron trichloride and sodium borohydride synthesize diborane in the first reaction chamber 161, a small amount of diborane will escape into the second reaction chamber 162, while most of the diborane will escape into the cavity at the top of the first reaction chamber 161, and flow along the second gas collecting chamber 17 and the second gas duct 25 together with the remaining boron trichloride in the reaction, and finally flow into the mixed solution in the second reaction chamber 162. Since the diborane generated in the first reaction chamber 161 flows back into the second reaction chamber 162, the mixed solution in the second reaction chamber 162 has a higher solubility of diborane. Therefore, when boron trichloride and sodium borohydride produce new diborane in the second reaction chamber 162, the diborane generated in the previous stage can inhibit the generation of methanol impurities, so as to further improve the purity of the diborane synthesis.

[0076] When the synthesized diborane and other gases flow to the collection assembly 6 through the gas collecting pipe 26, the collection assembly 6 can separate the diborane and fill the diborane into a steel cylinder. In the prior art, cold hydrazine can be used to cool and separate other impurities in diborane; the embodiment of the present application can collect diborane through existing technical means, so the specific structure of the collection assembly 6 is not described in detail in this embodiment. Example 2

[0077] Reference Figures 1 to 4 , this embodiment 2 discloses a diborane production synthesis process, and the diborane synthesis process in this embodiment is implemented using the diborane production synthesis device in embodiment 1. The diborane production synthesis process includes the following steps:

[0078] Gas environment preparation: the vacuum component 5 evacuates the reaction tank body 2, and the protective gas storage tank 3 delivers protective gas to the reaction tank body 2 to replace the impurity gas in the reaction tank body 2 and the pipeline.

[0079] Preparation of mixed solution: Sodium borohydride solid powder and solvent are weighed according to the formula ratio, and the sodium borohydride and solvent are stirred in a mixing tank 1 to dissolve the sodium borohydride in the solvent, and the mixed solution is transported to the reaction chamber 16 of the reaction tank 2.

[0080] Reaction temperature preparation: adjust the temperature inside the reaction tank 2.

[0081] Preparation of boron trichloride gas: Place the boron trichloride storage tank 4 on an electronic scale, and determine the input amount of boron trichloride gas according to the numerical changes on the electronic scale. The input amount of boron trichloride matches the amount of borohydride Warner added to comply with the diborane synthesis formula.

[0082] Preparation of diborane gas: The driving assembly 8 drives the first rotating plate 21, the first air duct 22, the second rotating plate 23, the partition plate 24, and the second air duct 25 to rotate, and the boron trichloride storage tank 4 transports boron trichloride gas to the reaction tank body 2; the boron trichloride gas flows through the first gas collecting chamber 15, the first air duct 22, the first reaction chamber 161, the second gas collecting chamber 17, the second air duct 25, and the second reaction chamber 162 in sequence. During the movement of boron trichloride, boron trichloride reacts with sodium borohydride to synthesize diborane.

[0083] Diborane gas delivery: The gas in the reaction tank 2 is delivered to the collecting component 6, and the collecting component 6 separates and purifies the diborane gas in the gas, and then fills the diborane gas into a steel cylinder. Example 3

[0084] This embodiment 3 discloses a diborane production synthesis device. The difference between this embodiment 3 and embodiment 1 is that:

[0085] Reference Figure 5 The second end of the second air guide tube 25 is fixed to the aerator 130, and the aerator 130 is used to disperse the gas into a large number of tiny bubbles to improve the solubility and dispersion of the gas in the solution. The aerator 130 can be one of a rotary mixing aerator 130, a microporous aerator 130, a jet aerator 130, etc., to improve the dispersion of the boron trichloride gas in the second reaction chamber 162, so as to further promote the reaction of boron trichloride and sodium borohydride, improve the production efficiency of diborane, and the concentration of synthesized diborane. A stainless steel blade 140 is fixed on the periphery of the second air guide tube 25, and the stainless steel blade 140 is wrapped around the outer peripheral wall of the second air guide tube 25 in a 45° spiral shape; so that when the second rotating plate 23 rotates with the second air guide tube 25, the second air guide tube 25 and the stainless steel blade 140 can disturb the mixed solution to promote the uniform distribution of sodium borohydride in the mixed solution, so as to facilitate the full reaction of boron trichloride and sodium borohydride. Example 4

[0086] This embodiment 4 discloses a diborane production synthesis device. The difference between this embodiment 4 and embodiment 3 is that:

[0087] Reference Figure 6 and Figure 7The first air guide pipe 22 includes a spiral pipe section 222 and a straight pipe section 223, which are integrally formed. The spiral pipe section 222 is disposed in the first reaction chamber 161, and the straight pipe section 223 passes through the first rotating plate 21 and extends into the first gas collecting chamber 15. The straight pipe section 223 is provided with an air inlet channel 2231 for gas to enter and exit, and the air inlet channel 2231 is disposed in the first gas collecting chamber 15. The air holes 221 are arranged at intervals along the outer circumference of the spiral pipe. Along the direction away from the first gas collecting chamber 15, the outer diameter of the spiral pipe section 222 increases or decreases. In this embodiment, along the direction away from the first gas collecting chamber 15, the outer diameter of the spiral pipe section 222 increases.

[0088] Reference Figure 6 and Figure 7 , the straight pipe section 223 of the first air duct 22 is rotatably connected to the first rotating plate 21, and a sealing sleeve 18 is provided between the straight pipe section 223 and the first rotating plate 21. A second gear ring 20 is fixedly provided on the inner side of the bottom wall of the reaction tank body 2, and a second gear 19 is fixedly provided at the end of the straight pipe section 223, and the second gear 19 is meshed with the inner ring of the second gear ring 20. The second gear ring 20 is located on the vertical projection plane of the orbital trajectory of the first air duct 22. When the driving assembly 8 drives the first rotating plate 21 to rotate, the second gear 19 rotates along the inner ring of the second gear ring 20, thereby realizing the self-rotation of the first air duct 22. The number of second gear rings 20 corresponds to the number of first air ducts 22. In the present embodiment, two second gear rings 20 are provided inside and outside.

[0089] The implementation principle of a diborane production synthesis device in the embodiment of the present application is:

[0090] Reference Figure 6 and Figure 7 When the driving assembly 8 drives the first air duct 22 to rotate around the central axis of the reaction tank body 2, the second gear 19 on the outer periphery of the straight pipe section 223 meshes with the second gear ring 20, thereby driving the first air duct 22 to rotate.

[0091] That is, when the driving assembly 8 drives the first air guide tube 22 to rotate around the center of the reaction tank body 2, the first air guide tube 22 will also rotate around its own central axis, so that the boron trichloride gas can be fully mixed with the mixed solution on the periphery of the first air guide tube 22, so as to further improve the reaction between the boron trichloride gas and sodium borohydride and improve the synthesis efficiency of diborane.

[0092] Specifically, when boron trichloride diffuses from the air holes 221 of the first air duct 22 into the reaction chamber 16, the boron trichloride moves along a specific route. By setting the first air duct 22 in the spiral tube section 222 and the straight tube section 223, and opening the air holes 221 on the spiral tube section 222, when the boron trichloride moves upward, the diffusion range of the boron trichloride on the horizontal projection plane is expanded, so that the boron trichloride can react with a larger range of sodium borohydride to further improve the production efficiency of diborane. The outer diameter of the spiral tube section 222 increases or decreases, which can reduce the overlapping part of the boron trichloride on the vertical projection plane, thereby further increasing the diffusion range of the boron trichloride gas in the horizontal direction, so as to further promote the reaction of boron trichloride and sodium borohydride, and further improve the production efficiency of diborane. Example 5

[0093] Reference Figure 6 and Figure 7 , this embodiment 5 discloses a diborane production synthesis process, and the synthesis process of this embodiment is realized by the diborane production synthesis device in embodiment 4, and the difference between the production process in this embodiment 5 and that in embodiment 2 mainly lies in the diborane gas preparation link, and the difference is as follows:

[0094] Preparation of diborane gas: The driving assembly 8 synchronously drives the first rotating plate 21, the first air duct 22, the second rotating plate 23 and the second air duct 25 to rotate, and the boron trichloride storage tank 4 delivers boron trichloride gas to the reaction tank body 2; the boron trichloride gas flows through the first gas collecting chamber 15, the first air duct 22, the first reaction chamber 161, the second gas collecting chamber 17, the second air duct 25 and the second reaction chamber 162 in sequence, and the boron trichloride reacts with sodium borohydride to synthesize diborane. At the same time, the second gear 19 on the outer periphery of the straight pipe section 223 meshes with the second gear ring 20, thereby driving the first air duct 22 to rotate.

[0095] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.

Claims

1. A diborane production synthesis device, characterized in that: The invention comprises a mixing tank body (1), a reaction tank body (2), a protective gas storage tank (3), a boron trichloride storage tank (4), a vacuum component (5) and a collecting component (6) which are connected by pipelines; the mixing tank body (1) is used to mix sodium borohydride and a solvent into a mixed solution; the reaction tank body (2) is connected to the mixing tank body (1); the reaction tank body (2) is provided with a liquid inlet for feeding the mixed solution; the reaction tank body (2) is provided with a first air inlet and a second air inlet; the first air inlet is connected to the protective gas storage tank (3); the second air inlet is connected to the boron trichloride storage tank (4); The reaction tank body (2) is further provided with a first gas outlet and a second gas outlet, the first gas outlet being in communication with the vacuum component (5), the vacuum component (5) being used for evacuating the reaction tank body (2), the second gas outlet being in communication with the collection component (6), the collection component (6) being used for collecting diborane generated in the reaction tank body (2); a first rotating plate (21) is provided at the bottom of the reaction tank body (2), the first rotating plate (21) and the side wall of the reaction tank body (2) forming a reaction chamber (16), the reaction chamber (16) being used for containing a mixed solution, the first rotating plate (21) A first gas collecting chamber (15) is formed with the bottom wall of the reaction tank body (2), the first gas collecting chamber (15) is connected to the first gas inlet, a first vertical gas guide pipe (22) is provided on the side of the first rotating plate (21) close to the reaction chamber (16), the first gas guide pipe (22) is connected to the first gas collecting chamber (15), and a plurality of gas holes (221) for boron trichloride gas to pass through are opened on the outer periphery of the first gas guide pipe (22); a driving assembly (8) is provided on the outer periphery of the reaction tank body (2), the driving assembly (8) comprising a rotating motor (81), a first gear (82) and a first gear ring (83) ), the first gear ring (83) is coaxially fixed with the first rotating plate (21), the first gear (82) is fixedly connected to the driving end of the rotating motor (81), the first gear (82) is meshed with the first gear ring (83), the driving assembly (8) drives the first air guide pipe (22) to revolve around the central axis of the reaction tank body (2); the reaction tank body (2) is further provided with a second rotating plate (23), a partition plate (24), a second air guide pipe (25) and an air collecting pipe (26), the second rotating plate (23) and the tank top of the reaction tank body (2) are arranged to form a second air collecting chamber (17);The driving components (8) are provided with two, and the two driving components (8) respectively drive the first rotating plate (21) and the second rotating plate (23) to rotate, and the first rotating plate (21) and the second rotating plate (23) rotate at the same frequency, the partition plate (24) is fixedly arranged on a side of the second rotating plate (23) close to the first rotating plate (21), and the partition plate (24) is arranged vertically, the partition plate (24) is inserted into the mixed solution, the partition plate (24) divides the second rotating plate (23) into a first part (231) and a second part (232), the first part (231) and the first air guide tube (22) are arranged opposite to each other, and the partition plate (24) divides the reaction chamber (16) into a first reaction chamber (161) and a second reaction chamber (162); the first part (231) is provided with a breathable mesh The second gas collecting chamber (17) is provided with a hole (2311), wherein the gas permeable mesh hole (2311) is used for allowing the gas in the first reaction chamber (161) to enter the second gas collecting chamber (17); the second gas guide pipe (25) is fixedly arranged on the side of the second component (232) close to the first rotating plate (21), the first end of the second gas guide pipe (25) is connected to the second gas collecting chamber (17), the second end of the second gas guide pipe (25) is inserted into the mixed solution, and an escape gap is provided between the second end of the second gas guide pipe (25) and the first rotating plate (21); the gas collecting pipe (26) is fixedly arranged on the side of the second component (232) away from the first rotating plate (21), one end of the gas collecting pipe (26) is connected to the second reaction chamber (162), and the other end of the gas collecting pipe (26) is externally connected to the collecting assembly (6). ; 2. The diborane production synthesis device according to claim 1, characterized in that: A gas-liquid separation membrane (27) is fixedly arranged on the outer periphery of the first gas guide tube (22), the gas-liquid separation membrane (27) covers the air permeable hole (221), and the boron trichloride gas passes through the gas-liquid separation membrane (27) and enters the reaction chamber (16).

3. The diborane production synthesis device according to claim 1, characterized in that: The first air guide pipe (22) comprises a spiral pipe section (222) and a straight pipe section (223); the spiral pipe section (222) and the straight pipe section (223) are integrally formed; the spiral pipe section (222) is arranged in the reaction chamber (16); the straight pipe section (223) passes through the first rotating plate (21) and extends into the first gas collecting chamber (15); the air holes (221) are arranged at intervals along the outer circumference of the spiral pipe section (222).

4. The diborane production synthesis device according to claim 3, characterized in that: Along the direction away from the first gas collecting chamber (15), the outer diameter of the spiral tube section (222) increases or decreases.

5. The diborane production synthesis device according to claim 3, characterized in that: The first air guide pipe (22) is rotatably connected to the first rotating plate (21), and a sealing sleeve (18) is provided between the straight pipe section (223) and the first rotating plate (21); a second gear ring (20) is fixedly provided on the inner side of the bottom wall of the reaction tank body (2), and a second gear (19) is fixedly provided at the end of the straight pipe section (223), and the second gear (19) is meshed with the inner ring of the second gear ring (20); the second gear ring (20) is located on the vertical projection plane of the orbital trajectory of the first air guide pipe (22), and the second gear ring (20) drives the first air guide pipe (22) to rotate through the second gear (19); the straight pipe section (223) is provided with an air inlet channel (2231) for gas to enter and exit, and the air inlet channel (2231) is arranged in the first gas collecting chamber (15).

6. The diborane production and synthesis device according to claim 1, characterized in that: An aerator (130) is fixedly disposed at the second end of the second air guide pipe (25).

7. The diborane production and synthesis device according to claim 1, characterized in that: A stainless steel blade (140) is fixedly provided on the outer circumference of the second air guide tube (25), and the stainless steel blade (140) is wrapped around the outer circumferential wall of the second air guide tube (25) in a 45-degree spiral shape.

8. A process for producing and synthesizing diborane, characterized in that: The method of synthesizing diborane using the diborane production synthesis device described in any one of claims 1 to 7 comprises the following steps: Preparation of gas environment: the vacuum component (5) evacuates the reaction tank (2), and the protective gas storage tank (3) delivers protective gas to the reaction tank (2) to displace impurity gases in the reaction tank (2) and pipelines; Preparation of mixed solution: weighing sodium borohydride solid powder and solvent according to the formula ratio, stirring the sodium borohydride and solvent in a mixing tank (1) to dissolve the sodium borohydride in the solvent, and conveying the mixed solution to the reaction chamber (16) of the reaction tank (2); Reaction temperature preparation: adjusting the temperature in the reaction tank (2); Preparation of boron trichloride gas: Place the boron trichloride storage tank (4) on an electronic scale, and determine the input amount of boron trichloride gas according to the value change on the electronic scale. The input amount of boron trichloride matches the input amount of sodium borohydride to meet the diborane synthesis formula; Preparation of diborane gas: the driving component (8) synchronously drives the first rotating plate (21), the first air guide pipe (22), the second rotating plate (23) and the second air guide pipe (25) to rotate, and the boron trichloride storage tank (4) transports boron trichloride gas to the reaction tank body (2); the boron trichloride gas flows through the first gas collecting chamber (15), the first air guide pipe (22), the first reaction chamber (161), the second gas collecting chamber (17), the second air guide pipe (25) and the second reaction chamber (162) in sequence, and the boron trichloride reacts with sodium borohydride to synthesize diborane; Diborane gas transportation: The gas in the reaction tank (2) is transported to the collecting component (6), and the collecting component (6) separates and purifies the diborane gas in the gas, and then fills the diborane gas into a steel cylinder.

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