Electronic-grade phosphine synthesizing and refining device

Abstract

The utility model relates to the technical field of reaction kettles, and particularly discloses an electronic-grade phosphine synthesizing and refining device which comprises a reaction kettle, a conveying pipe and a communicating pipe are arranged at the top of the reaction kettle, the reaction kettle is communicated with a water inlet pipe, a discharging pipe is arranged at the bottom of the reaction kettle, and a rotating shaft is rotatably mounted on a bottom plate of the reaction kettle. The rotating shaft and the material conveying pipe are coaxially arranged, an umbrella-shaped flow guide table is arranged on the rotating shaft, the discharging end of the material conveying pipe faces the flow guide table, the rotating shaft is driven by a first driving source to rotate, the flow guide table is driven by the rotating shaft to rotate, and an electric air cylinder used for driving the flow guide table to ascend and descend is arranged in the rotating shaft. According to the invention, the flow guide table is arranged, so that the speed of phosphide falling into water from the edge of the flow guide table is slowed down, the generation speed of phosphine can be effectively controlled, the risk of sudden pressure increase caused by a large amount of gas generated due to too high speed is avoided, and the phosphide falls to the flow guide table and is dispersed around, so that the phosphide falls into water in a dispersed manner, and the contact surface area of the phosphide and the water is increased.

Description

Technical Field

[0001] The utility model relates to the technical field of reaction kettles, and specifically designs an electronic-grade phosphine synthesis and refining device. Background Art

[0002] Phosphine is a colorless and highly toxic gas at room temperature. It is widely used in semiconductors, solar cells, grain fumigation and other fields. As an important N-type doping source in semiconductor manufacturing, phosphine is also used in ion implantation processes, epitaxial GAP materials and polysilicon chemical vapor deposition. It is an important electronic specialty gas. The main methods for synthesizing phosphine are chemical method, electrolysis method and microwave method. The chemical method mainly includes thermal decomposition method, acid method, alkali method and hydrolysis method.

[0003] In the prior art, the hydrolysis method only requires mixing a phosphide such as aluminum phosphide or zinc phosphide with water to produce phosphine gas at room temperature and pressure. This method is simple to operate, relatively low in cost, and suitable for large-scale production. However, if the phosphide is added to the water too quickly, the phosphine gas will be released quickly, causing a sudden increase in the pressure in the reactor, which poses a production risk. Therefore, in the existing reactor, a metering pump or regular addition of phosphide is usually used to deal with this problem. This method mainly controls the maximum amount of phosphine gas released at a time, that is, a small amount of phosphide is added into the water at a time for reaction. Although this can avoid the instantaneous release of a large amount of phosphine gas, the problem of sudden release of a large amount of gas due to the excessively fast water entry speed still exists. Moreover, the addition of a small amount of phosphide at a time means that the synthesized phosphine gas will be reduced, and the phosphide enters the water in an aggregated form, so that the internal phosphide cannot contact the water at the first time, which prolongs the time for synthesizing gas and reduces the production efficiency. Based on this, the inventor purposefully provides an electronic-grade phosphine synthesis and refining device that can reduce the speed at which the raw material enters the water and ensure the phosphine synthesis rate. Utility Model Content

[0004] The utility model aims to solve the problems in the prior art by providing an electronic grade phosphine synthesis and refining device which can reduce the speed of raw materials entering water and ensure the synthesis rate of phosphine, so as to solve the problem in the prior art that the phosphide enters water quickly and a large amount of phosphine gas is suddenly released.

[0005] The purpose of the utility model can be achieved through the following technical solutions:

[0006] An electronic grade phosphine synthesis and refining device comprises a reactor, wherein a feed pipe and a connecting pipe are arranged on the top of the reactor, the reactor is connected with a water inlet pipe, a discharge pipe is arranged at the bottom of the reactor, a rotating shaft is rotatably mounted on the bottom plate of the reactor, and the rotating shaft is coaxially arranged with the feed pipe, an umbrella-shaped guide platform is arranged on the rotating shaft, a discharge end of the feed pipe faces the guide platform, the rotating shaft is driven to rotate by a first driving source, the guide platform is driven to rotate by the rotating shaft, an electric cylinder for driving the guide platform to rise and fall is arranged in the rotating shaft, a water level monitoring component is arranged in the reactor, the water level monitoring component and the electric cylinder are both connected to a control box, when the water level in the reactor changes, the electric cylinder will drive the guide platform to rise and fall, so that the height at the edge of the guide platform is higher than the water level in the reactor.

[0007] As a further optimization or improvement of this solution.

[0008] A through hole is provided on the rotating shaft, a connecting rod is slidably installed in the through hole, the connecting rod is fixedly connected to the guide platform, and the connecting rod is driven to rise and fall by an electric cylinder.

[0009] As a further optimization or improvement of this solution.

[0010] The guide platform is provided with a plurality of discharge holes in an arc shape, and the discharge holes are located in the middle of the umbrella surface of the guide platform.

[0011] As a further optimization or improvement of this solution.

[0012] One end of the rotating shaft close to the material conveying pipe is arranged as a dome.

[0013] As a further optimization or improvement of this solution.

[0014] Two stirring rods are fixedly connected to the surface of the rotating shaft, and the two stirring rods are symmetrically arranged.

[0015] As a further optimization or improvement of this solution.

[0016] An auger blade is rotatably installed in the feed pipe and is coaxially arranged with the rotating shaft. The auger blade is driven to rotate by a second driving source, and the edge of the auger blade is slidably matched with the inner wall of the feed pipe.

[0017] As a further optimization or improvement of this solution.

[0018] The feed pipe is connected to the feed pipe, the discharge end of the feed pipe faces the auger blade, and the height of the discharge end of the feed pipe is not lower than the height of the auger blade.

[0019] Beneficial effects of the utility model:

[0020] 1. Before feeding, the utility model adds water into the reactor through the water inlet pipe as a reaction medium. The control box monitors the water level through the water level sensor, and drives the guide table to rise and fall through the electric cylinder, so that the edge of the guide table is slightly higher than the water level, which can adapt to different water level changes and meet different production needs. Since the edge of the guide table is slightly higher than the water level, the phosphide does not have enough distance for acceleration, avoiding the risk of a sudden pressure increase caused by a large amount of gas suddenly generated due to the phosphide entering the water too quickly.

[0021] 2. The utility model drives the guide table to rotate through the rotation of the rotating shaft. When the phosphide is transported to the reactor through the feed pipe, it will first fall onto the guide table and slide along the plate surface of the guide table and fall into the water from its edge. The phosphide will spread out to the surroundings when it falls onto the guide table, so that the phosphide is dispersed and falls into the water, preventing local phosphides from gathering together, resulting in the phosphide wrapped therein being unable to react with water in time, and falling into the water in a dispersed manner, thereby ensuring that the phosphide can be fully mixed with water and react with water as soon as it falls into the water, thereby shortening the time for synthesizing gas.

[0022] 3. According to the characteristic that the particle phosphide will be differentiated by size during grinding, the utility model opens a plurality of discharge holes on the guide table, and cooperates with the function of the rotating shaft to drive the guide table to rotate. When the particle phosphide falls on the guide table, it will slide to its edge. In this process, due to the rotation of the guide table and its own gravity, the large particle phosphide will not fall from the discharge hole due to its inertia, but fall into the water from the edge of the guide table, while the small particle phosphide will fall from the discharge hole and directly enter the water, thereby dividing the area where the phosphide falls into the water, making the distribution of the phosphide in the water more dispersed and avoiding excessive local concentration. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The utility model is further described below in conjunction with the accompanying drawings.

[0024] Figure 1 It is a schematic diagram of the overall structure of the utility model.

[0025] Figure 2 It is a schematic diagram of the cross-sectional structure of the reactor.

[0026] Figure 3 It is a schematic diagram of the connection structure between the rotating shaft and the connecting rod.

[0027] The figure shows:

[0028] 1. Reactor; 2. Feed pipe; 3. Connecting pipe; 4. Water inlet pipe; 5. Rotating shaft; 6. Guide platform; 7. Discharge hole; 8. Stirring rod; 9. Through hole; 10. Connecting rod; 11. Electric cylinder; 12. Dome; 13. Auger blade; 14. Feed pipe; 15. Discharge pipe. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0030] See also Figure 1-Figure 3 , an electronic grade phosphine synthesis and refining device, comprising a reactor 1, a feed pipe 2 and a connecting pipe 3 are arranged on the top of the reactor 1, the reactor 1 is connected to a water inlet pipe 4, a discharge pipe 15 is arranged at the bottom of the reactor 1, a rotating shaft 5 is rotatably installed on the bottom plate of the reactor 1, and the rotating shaft 5 is coaxially arranged with the feed pipe 2, an umbrella-shaped guide platform 6 is arranged on the rotating shaft 5, the discharge end of the feed pipe 2 faces the guide platform 6, the rotating shaft 5 is driven to rotate by a first driving source, the guide platform 6 is driven to rotate by the rotating shaft 5, an electric cylinder 11 for driving the guide platform 6 to rise and fall is arranged in the rotating shaft 5, a water level monitoring component is arranged in the reactor 1, the water level monitoring component and the electric cylinder 11 are both connected to the control box, when the water level in the reactor 1 changes, the electric cylinder 11 will drive the guide platform 6 to rise and fall, so that the height at the edge of the guide platform 6 is higher than the water level in the reactor 1.

[0031] In a specific embodiment, the first driving source can be set to a first motor, the water level monitoring component includes a water level sensor, a data storage disk, a data transmitter, etc., the control box includes a PLC control system, a networking module, a control switch, etc., and the connecting pipe 3 is connected to the phosphine gas purification device. The above components are all prior arts. The specific models are not disclosed in the present utility model, which does not affect the integrity of the present utility model.

[0032] The working principle of the utility model is as follows: water is added into the reactor 1 through the water inlet pipe 4 as a reaction medium; the control box monitors the water level through the water level sensor, and drives the guide platform 6 to rise and fall through the electric cylinder 11, so that the edge of the guide platform 6 is slightly higher than the water level, which can adapt to different water level changes and meet different production needs.

[0033] The granular phosphide is transported through the feed pipe 2. As a reaction raw material, the phosphide first falls onto the guide table 6 and slides along the plate surface of the guide table 6. Then, the first motor drives the rotating shaft 5 to rotate, thereby driving the guide table 6 to rotate synchronously. The rotation of the guide table 6 causes the phosphide to spread around on the plate surface and slide into the water from the edge. Since the edge is slightly higher than the water level, the phosphide does not have enough distance for acceleration, thereby avoiding the risk of a sudden increase in pressure caused by a large amount of gas suddenly generated due to the phosphide entering the water too quickly. At the same time, the phosphide is changed from entering the water in one place to falling into the water in a dispersed manner from the plate surface of the guide table 6, thereby preventing local phosphides from being concentrated together, resulting in the phosphide wrapped therein being unable to react with water in time, and falling into the water in a dispersed manner, thereby ensuring that the phosphide can be fully mixed with water and can react with water as soon as it falls into the water, thereby shortening the time for synthesizing gas.

[0034] Specifically, a through hole 9 is formed on the rotating shaft 5 , and a connecting rod 10 is slidably installed in the through hole 9 . The connecting rod 10 is fixedly connected to the guide platform 6 , and the connecting rod 10 is driven to rise and fall by an electric cylinder 11 .

[0035] In a specific embodiment, through the connection between the connecting rod 10 and the guide platform 6, when the rotating shaft 5 rotates, the guide platform 6 can keep rotating synchronously with the rotating shaft 5 through the limiting effect of the connecting rod 10, and the control box monitors the water level through the water level sensor, and drives the connecting rod 10 to move up and down in the through hole 9 through the electric cylinder 11, thereby driving the guide platform 6 to rise and fall on the rotating shaft 5, ensuring that the guide platform 6 is higher than the water level in the reactor 1.

[0036] More specifically, the guide platform 6 is provided with a plurality of arc-shaped discharge holes 7 , and the discharge holes 7 are located in the middle of the umbrella surface of the guide platform 6 .

[0037] In a specific embodiment, the aperture of the discharge hole 7 can be controlled to limit the actual use situation so that only part of the phosphide can pass through. When the granular phosphide falls onto the guide platform 6, it will slide to its edge. In this process, due to the rotation of the guide platform 6 and its own gravity, large particles of phosphide will not be able to fall from the discharge hole 7 due to their inertia, and will fall into the water from the edge of the guide platform 6, while small particles of phosphide will fall from the discharge hole 7 and directly enter the water, dividing the area where the phosphide falls into the water, making the distribution of the phosphide in the water more dispersed and avoiding excessive local concentration.

[0038] More specifically, one end of the rotating shaft 5 close to the material conveying pipe 2 is configured as a dome 12 .

[0039] In a specific embodiment, the dome 12 faces the discharge end of the feed pipe 2. When the phosphide falls, it will impact the dome 12, causing it to disperse and fall onto the surface of the guide table 6, while also preventing the phosphide from remaining on one end of the rotating shaft 5.

[0040] Meanwhile, it should be noted that two stirring rods 8 are fixedly connected to the surface of the rotating shaft 5 , and the two stirring rods 8 are symmetrically arranged.

[0041] In a specific embodiment, two stirring rods 8 are provided so that when the rotating shaft 5 rotates, the water in the reaction kettle 1 can be stirred, so that the reactants in the water are mixed more evenly, thereby accelerating the reaction speed.

[0042] More specifically, an auger blade 13 is rotatably installed in the feed pipe 2 and is coaxially arranged with the rotating shaft 5 . The auger blade 13 is driven to rotate by a second driving source, and the edge of the auger blade 13 is slidably matched with the inner wall of the feed pipe 2 .

[0043] In a specific embodiment, the second driving source can be set as a second motor, which continuously delivers the particulate phosphide to the reactor 1 through the auger blades 13 and the feed pipe 2. Due to the continuity of its delivery and the stability of the delivery amount, combined with the guiding and diversion effects of the guide platform 6, it can ensure that the phosphide is always stably delivered to the water to react with water to generate phosphine gas, thereby ensuring the stability of the production gas in the reactor 1 and avoiding the discontinuity of the production gas and large changes in the production gas volume.

[0044] Meanwhile, it should be noted that the feed pipe 2 is connected to the feed pipe 14 , the discharge end of the feed pipe 14 faces the auger blade 13 , and the height of the discharge end of the feed pipe 14 is not lower than the height of the auger blade 13 .

[0045] In a specific implementation, the phosphide is introduced into the delivery pipe 2 through the feed pipe 14, and the height of the discharge end of the feed pipe 14 is not lower than the height of the auger blade 13, which can ensure that the phosphide can be transported immediately after entering the delivery pipe 2, avoiding the phenomenon of inconsistent material transportation amount.

[0046] The above shows and describes the basic principle, main features and advantages of the utility model. Those skilled in the art should understand that the utility model is not limited by the above embodiments, and the above embodiments and descriptions are only for explaining the principle of the utility model. Without departing from the spirit and scope of the utility model, the utility model may have various changes and improvements, and these changes and improvements fall within the scope of the utility model to be protected.

Claims

1. An electronic grade phosphine synthesis and purification device, characterized in that: The invention comprises a reactor (1), wherein a feed pipe (2) and a connecting pipe (3) are arranged on the top of the reactor (1), the reactor (1) is connected to a water inlet pipe (4), a discharge pipe (15) is arranged on the bottom of the reactor (1), a rotating shaft (5) is rotatably mounted on the bottom plate of the reactor (1), and the rotating shaft (5) is coaxially arranged with the feed pipe (2), an umbrella-shaped flow guide platform (6) is arranged on the rotating shaft (5), the discharge end of the feed pipe (2) faces the flow guide platform (6), and the rotating shaft (5) is connected to the water inlet pipe (4) by the first A driving source drives the flow guide platform (6) to rotate, and the flow guide platform (6) is driven to rotate by the rotating shaft (5). An electric cylinder (11) is arranged in the rotating shaft (5) for driving the flow guide platform (6) to rise and fall. A water level monitoring component is arranged in the reactor (1). The water level monitoring component and the electric cylinder (11) are both connected to the control box. When the water level in the reactor (1) changes, the electric cylinder (11) drives the flow guide platform (6) to rise and fall, so that the height at the edge of the flow guide platform (6) is higher than the water level in the reactor (1).

2. The electronic grade phosphine synthesis and purification device according to claim 1, characterized in that: The rotating shaft (5) is provided with a through hole (9), a connecting rod (10) is slidably mounted in the through hole (9), the connecting rod (10) is fixedly connected to the guide platform (6), and the connecting rod (10) is driven to rise and fall by an electric cylinder (11).

3. The electronic grade phosphine synthesis and purification device according to claim 1, characterized in that: The guide platform (6) is provided with a plurality of discharge holes (7) in an arc shape, and the discharge holes (7) are located in the middle of the umbrella surface of the guide platform (6).

4. The electronic grade phosphine synthesis and purification device according to claim 2, characterized in that: One end of the rotating shaft (5) close to the material conveying pipe (2) is configured as a dome (12).

5. The electronic grade phosphine synthesis and purification device according to claim 2, characterized in that: Two stirring rods (8) are fixedly connected to the surface of the rotating shaft (5), and the two stirring rods (8) are symmetrically arranged.

6. The electronic grade phosphine synthesis and purification device according to claim 1, characterized in that: An auger blade (13) is rotatably mounted in the feed pipe (2) and is coaxially arranged with the rotating shaft (5). The auger blade (13) is driven to rotate by a second driving source, and the edge of the auger blade (13) is slidably engaged with the inner wall of the feed pipe (2).

7. The electronic grade phosphine synthesis and purification device according to claim 5, characterized in that: The feed pipe (2) is connected to the feed pipe (14), the discharge end of the feed pipe (14) faces the auger blade (13), and the height of the discharge end of the feed pipe (14) is not lower than the height of the auger blade (13).

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