A pretreatment device for chlorosilane sample detection

Abstract

The utility model provides a kind of pretreatment device for chlorosilane sample detection, it is related to chlorosilane sample content detection technical field, it includes: box, buckling piece, gas storage tank, pump body, vacuum pump and pressure gauge, box is hinged with switch door, and side wall surface is respectively provided with air inlet and air outlet;Buckling piece is used to switch door buckling in the opening of box;Gas storage tank is filled with inert gas inside;Air outlet is communicated with air inlet between gas storage tank side wall surface and air inlet and is provided with air inlet pipe;Pump body is between box and gas storage tank, for pumping the gas in gas storage tank into the inside of box;Vacuum pump is equipped with the air outlet pipe of communication between air outlet;Pressure gauge is located at the top of box, for real-time display the pressure value in the inside of box.The pretreatment device can avoid the problems of sample content loss, heating operation risk, and the influence of open system on the sample to be measured during the drying process.

Description

Technical Field

[0001] This utility model relates to the field of chlorosilane sample content detection technology, specifically to a pretreatment device for chlorosilane sample detection. Background Technology

[0002] Currently, in the process of volatilizing chlorosilane samples, apart from some cases where natural evaporation is used under inert gas at room temperature, others typically employ direct heating of the sample to accelerate the volatilization rate and facilitate subsequent content detection. However, direct heating has the following disadvantages:

[0003] 1. For chlorosilane samples containing high-boiling-point substances, flash combustion can easily occur during heating due to the presence of these substances, leading to a loss of sample mass and hindering accurate quantitative analysis.

[0004] Second, boron and phosphorus exist in chlorosilanes in various forms of compounds. For example, BCl3 (boron trichloride) has a boiling point of 12.5℃ and PFCl2 has a boiling point of 13.9℃. These substances have boiling points below room temperature. Under heating conditions, even if the sample does not flash, the sample volatilizes and carries away a large amount of boron and phosphorus, resulting in a loss of boron and phosphorus mass and making it impossible to accurately detect the content of boron and phosphorus.

[0005] Third, flash fires that occur during sample heating pose operational and analytical risks.

[0006] IV. Sample heating is carried out in an open system, and the sample is subject to interference from environmental impurities. Utility Model Content

[0007] This invention addresses the problems of sample content loss, operational risks, and environmental impact during the direct heating and volatilization of chlorosilane samples. It provides a pretreatment device for chlorosilane sample detection, which places the chlorosilane in a low-pressure, closed device for volatilization, thus avoiding sample content loss, operational risks, and the introduction of impurities into the sample during the volatilization process.

[0008] The technical solution adopted in this utility model is:

[0009] A pretreatment apparatus for detecting chlorosilane samples is provided, comprising:

[0010] The enclosure comprises a hinged door at one open end for rotating and sealing the enclosure; an air inlet and an air outlet communicating with the interior of the enclosure are respectively opened on the side walls of the enclosure; a fastener is located on the outer wall of the door and the outer wall of the enclosure for fastening the door to the opening of the enclosure; a gas storage tank is located on one side of the enclosure and is filled with inert gas; an exhaust port is opened on the side wall of the gas storage tank, and an air inlet pipe connects the exhaust port of the gas storage tank to the air inlet of the enclosure; a pump body is located between the enclosure and the gas storage tank and is connected to the air inlet pipe for pumping the gas in the gas storage tank into the interior of the enclosure; a vacuum pump is located on one side of the enclosure, and an exhaust pipe connects the vacuum pump to the air outlet of the enclosure; and a pressure gauge is located on the top of the enclosure, with the sensing end of the pressure gauge located inside the enclosure for real-time display of the internal pressure value of the enclosure.

[0011] Optionally, an observation opening is provided on the side wall of the door, and an observation window is provided on the side wall of the door at the observation opening.

[0012] Optionally, an oxygen concentration detector is also installed on the top of the chamber. The detection end of the oxygen concentration detector is located inside the chamber and is used to detect whether the interior of the chamber is a completely inert gas environment.

[0013] Optionally, the fastening element includes a buckle and a locking block. The buckle is located on the outer wall of the enclosure, and the locking block is located on the outer wall of the door. When the door is rotated to the opening of the enclosure, the interior of the enclosure is sealed by the engagement of the locking block and the buckle.

[0014] Optionally, it also includes a PLC control cabinet, which is located on one side of the enclosure and is electrically connected to the pump body and the vacuum pump respectively; a pressure sensor is also provided on the top of the enclosure, with the detection end of the pressure sensor located inside the enclosure. The pressure sensor is electrically connected to the PLC control cabinet and is used to receive the signal transmitted by the pressure sensor and adjust the working status of the pump body and the vacuum pump.

[0015] Optionally, an alarm is installed on the top of the PLC control cabinet. When the pressure inside the cabinet exceeds a threshold, the alarm is triggered by the PLC control cabinet.

[0016] Optionally, an explosion-proof pressure relief valve that communicates with the interior of the enclosure is also provided on the side wall of the enclosure. The explosion-proof pressure relief valve is electrically connected to the PLC control cabinet. When the pressure value inside the enclosure exceeds the threshold, the explosion-proof pressure relief valve is opened through the PLC control cabinet to release pressure.

[0017] Optionally, a sealing gasket is provided on the closing surface of the door and the housing.

[0018] Optionally, the vacuum pump is an acid-resistant vacuum pump, the housing is made of polychlorotrifluoroethylene (PTFE) sheet, and both the inlet and outlet pipes are made of PTFE tubing.

[0019] Optionally, the inner wall surface of the enclosure is coated with PTFE.

[0020] The beneficial effects of this utility model are:

[0021] 1. By opening the hinged door at the box outlet, the container containing chlorosilane is placed inside the box. The door is then rotated until the box outlet is sealed. The door is then fastened to the box outlet using the fasteners to create a closed space, preventing the chlorosilane from being affected by contact with air.

[0022] 2. Gas circulation inside the chamber is achieved by installing a gas storage tank, an inlet pipe, and a pump body on the outside of the chamber, as well as a vacuum pump and an outlet pipe. The gas storage tank is connected to the inside of the chamber via the inlet pipe, and the pump body is located on the wall of the inlet pipe. The gas storage tank is filled with inert gas, and the vacuum pump is connected to the inside of the chamber via the outlet pipe. Before the chlorosilane is placed inside the chamber, the switch door is closed to seal the inside of the chamber. Then, the pump body is used to pump the inert gas from the gas storage tank into the inside of the chamber through the inlet pipe. After the inert gas has been introduced for a period of time, the vacuum pump is turned on to expel the mixture of inert gas and air inside the chamber until the inside of the chamber is an inert gas environment. Then, the switch door is opened, the chlorosilane is placed inside the chamber, and the switch door is closed again. The inert gas is then introduced again to keep the chlorosilane in an inert gas environment, preventing it from being affected by air. The vacuum pump maintains a low pressure inside the chamber, which lowers the boiling point of the chlorosilane, thereby accelerating its volatilization.

[0023] 3. By installing a pressure gauge on the top of the housing, with the sensing end of the pressure gauge located inside the housing, the pressure value inside the housing can be displayed in real time. This allows for adjustment of the operating status of the pump and vacuum pump based on the pressure value, preventing the volatilization process of chlorosilane from being affected. Attached Figure Description

[0024] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 This is a top view of the pretreatment device for chlorosilane sample detection disclosed in Example 1;

[0026] Figure 2 This is a schematic diagram of the main structure of the preprocessing device;

[0027] Figure 3 A top view of the pretreatment unit with the addition of a PLC control cabinet;

[0028] Figure 4 A schematic diagram of the main structure of the pretreatment device with the addition of a PLC control cabinet;

[0029] Figure 5 for Figure 1 A magnified view of a portion of point A in the middle;

[0030] Figure 6 for Figure 1 A magnified view of a portion of point B in the middle.

[0031] Figure label:

[0032] 1-Box body, 10-Door switch, 100-Observation window, 11-Pressure gauge, 12-Oxygen concentration detector, 13-Pressure sensor, 14-Explosion-proof pressure relief valve, 15-Sealing gasket;

[0033] 2-Air storage tank, 20-Air inlet pipe;

[0034] 3-Pump body;

[0035] 4 - Vacuum pump, 40 - Outlet pipe;

[0036] 5-Snap fastener;

[0037] 6-Card Block;

[0038] 7-PLC control cabinet, 70-alarm device. Detailed Implementation

[0039] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0040] The following disclosure provides many different embodiments or examples for implementing various structures of this invention. To simplify the disclosure, specific examples of components and arrangements are described below. Of course, these are merely examples and are not intended to limit the scope of this invention.

[0041] The embodiments of the utility model will now be described in detail with reference to the accompanying drawings.

[0042] Example 1

[0043] Please see Figure 1 , Figure 2 , Figure 5 and Figure 6 As shown, this embodiment discloses a pretreatment device for chlorosilane sample detection, including a housing 1. One end face of the housing 1 has an opening, and an air inlet and an air outlet communicating with the interior of the housing 1 are respectively formed on the side wall of the housing 1. A hinged door 10 is connected to the opening of the housing 1, and the door 10 can seal the housing 1 by rotation. Fastening components are provided on the outer wall of the housing 1 and the outer wall of the door 10. These fastening components can lock the door 10 at the opening of the housing 1 after it has rotated to cover and seal the opening. In this embodiment, the fastening components are a locking block 6 and a latch 5. The locking block 6 is located on the outer wall of the door 10. When the door 10 rotates on the outer wall of the housing 1 to seal the opening, the locking block 6 and the latch 5 cooperate to fix the door 10, preventing it from rotating on its own and avoiding any impact on the chlorosilane sample inside the housing 1 during processing. An observation opening is provided on the side wall of the door 10, and an observation window 100 is provided at the observation opening to allow staff to observe the state of chlorosilane inside the chamber 1. An oxygen concentration detector 12 is also provided on the top of the chamber 1. The detection end of the oxygen concentration detector 12 is located inside the chamber 1 and can detect whether there is still air inside the chamber 1.

[0044] A gas storage tank 2 is provided on one side of the aforementioned housing 1. The interior of the gas storage tank 2 is filled with an inert gas. Specifically, in this embodiment, the inert gas is a gas with a density greater than air, such as argon. This allows the inert gas to deposit at the bottom of the housing 1, completely encapsulating the chlorosilanes and reducing the possibility of flash combustion of chlorosilanes containing high-boiling-point compounds, thus improving the safety of sample analysis operations. An exhaust port is provided on the side wall of the gas storage tank 2, and an inlet pipe 20 is connected between the exhaust port and the inlet port. A pump body 3 is provided between the gas storage tank 2 and the housing 1, and the pump body 3 is connected to the inlet pipe 20. That is, by operating the pump body 3, the inert gas inside the gas storage tank 2 can be pumped into the interior of the housing 1 through the inlet pipe 20.

[0045] A vacuum pump 4 is also provided on one side of the aforementioned chamber 1. An outlet pipe 40 connects the vacuum pump 4 to the outlet. When the vacuum pump 4 operates, it evacuates the interior of the chamber 1, reducing the internal pressure and creating a low-pressure environment. Under low pressure, the boiling point of chlorosilanes decreases, thus accelerating the evaporation rate of the chlorosilane sample and improving the detection efficiency. It is worth noting that since the inert gas used in this embodiment is argon, a gas with a density greater than air, air is located at the top of the chamber 1, while the inert gas is located at the bottom. Therefore, to facilitate the removal of air from the chamber 1, the outlet is located near the top of the chamber 1. A pressure gauge 11 is installed at the top of the chamber 1, with its detection end located inside the chamber 1. This gauge is used to monitor and display the internal pressure of the chamber 1 in real time for easy observation by personnel.

[0046] The working principle of this embodiment:

[0047] First, open the hinged door 10 on the outer wall of the chamber 1, place the container containing the chlorosilane sample into the chamber 1, and then close the door 10. The door 10 seals the opening of the chamber 1 through the engagement of the latch 6 and the buckle 5. Next, run the vacuum pump 4 to extract some air from the chamber 1, then stop the vacuum pump 4 and turn on the pump body 3. The pump body 3 pumps the inert gas from the gas storage tank 2 into the chamber 1 through the inlet pipe 20. Since the inert gas used in this embodiment is denser than air, it will be located at the bottom of the chamber 1. As the inert gas gradually accumulates, it will push the remaining air inside the chamber 1 to the top. At this point, turn on the vacuum pump 4, which will extract the remaining air from the chamber 1, ensuring that the chlorosilane inside the chamber 1 is completely enveloped by the inert gas.

[0048] After vacuum pump 4 has been running for a period of time, the presence of air inside chamber 1 can be determined by observing the oxygen concentration detector 12. If air is present, vacuum pump 4 continues to extract it. If no air is present, vacuum pump 4 is turned off, but pump body 3 remains on. Pump body 3 introduces inert gas into chamber 1 until the pressure displayed on pressure gauge 11 reaches the preset value. Then, pump body 3 is stopped. The chlorosilane is now enclosed in an inert gas environment, preventing flash combustion. Next, vacuum pump 4 is turned on to evacuate the interior of chamber 1. During the evacuation process, the pressure inside chamber 1 gradually decreases. This decrease in pressure causes the boiling point of the chlorosilane to gradually decrease, thereby accelerating the evaporation rate of the sample. After vacuum pump 4 continues to run until the pressure inside chamber 1 reaches the preset low-pressure range, pump 3 begins to operate. Pump 3 pumps the inert gas from storage tank 2 into the interior of chamber 1 through inlet pipe 20. During this process, the pressure inside chamber 1 will not gradually decrease. At this time, pump 3 is used to maintain the interior of chamber 1 at a low pressure. During this period, the operator controls the operation of pump 3 by observing the changes in pressure gauge 11. If too much inert gas is introduced into pump 3, causing an excessive increase in pressure inside chamber 1, it will affect the volatilization of chlorosilane. When the pressure inside the chamber 1 is close to the preset low pressure range, stop running pump 3 until the pressure gauge 11 shows that the internal pressure of the chamber 1 is close to the preset low pressure range. Then start pump 3 again to introduce inert gas into the chamber 1. Repeat the above operation until the operator observes through the observation window 100 that the state of the chlorosilane inside the chamber 1 is suitable. Then stop running vacuum pump 4 and continue running pump 3 until the pressure inside the chamber 1 is close to atmospheric pressure. Then stop running pump 3, change the engagement state of the latch 6 and the buckle 5 so that the door 10 can be opened. Finally, the chlorosilane sample can be taken out.

[0049] Example 2

[0050] This embodiment is a further optimization based on Embodiment 1, specifically, as follows: Figure 3 and Figure 4As shown, a PLC control cabinet 7 is also provided on one side of the housing 1. The PLC control cabinet 7 is electrically connected to both the pump body 3 and the vacuum pump 4, meaning that the PLC control cabinet 7 can control the operating status of the pump body 3 and the vacuum pump 4 respectively. A pressure sensor 13 is also provided on the top of the housing 1. The pressure sensor 13 is electrically connected to the PLC control cabinet 7. The detection end of the pressure sensor 13 is located inside the housing 1, meaning that the pressure sensor 13 can feed back the pressure changes inside the housing 1 to the PLC control cabinet 7 in real time, thereby enabling the PLC control cabinet 7 to control the working status of the pump body 3 and the vacuum pump 4 respectively. Here, the pressure sensor 13 replaces the function of the pressure gauge 11 in Embodiment 1. An alarm 70 is electrically connected to the top of the PLC control cabinet 7. When the pressure value inside the housing 1 exceeds a preset pressure threshold, the alarm 70 will sound, prompting on-site personnel to take action. Furthermore, if the internal pressure of chamber 1 rises too quickly and exceeds the preset pressure threshold, pressure relief is required. Therefore, an explosion-proof pressure relief valve 14 is installed on the side wall of chamber 1. The explosion-proof pressure relief valve 14 is electrically connected to the PLC control cabinet 7, allowing it to open and relieve pressure when the internal pressure of chamber 1 becomes too high. Additionally, when the vacuum pump 4 malfunctions, the explosion-proof pressure relief valve 14 can also be used to relieve pressure, thus protecting the sample and equipment from damage. This embodiment replaces the manual operation of embodiment one with automated control; the specific working process is not significantly different from embodiment one. It is worth noting that when detecting whether there is remaining air inside chamber 1, the oxygen concentration detector 12 can be electrically connected to the PLC control cabinet 7, allowing the PLC control cabinet 7 to make corresponding operations based on the detection results of the oxygen concentration detector 12.

[0051] A sealing gasket 15 is provided on the closing surface of the aforementioned switch door 10 and housing 1. When the switch door 10 rotates to seal the housing 1, the sealing gasket 15 fills the gap between the switch door 10 and housing 1, preventing gas leakage inside housing 1 from affecting the evaporation of chlorosilane inside housing 1. Furthermore, since chlorosilane produces acidic gas during evaporation, which can affect housing 1, inlet pipe 20, outlet pipe 40, pump body 3, and vacuum pump 4, housing 1, inlet pipe 20, and outlet pipe 40 are all made of polychlorotrifluoroethylene. A PTFE coating can also be applied to the inner wall of housing 1 for enhanced protection. Pump body 3 and vacuum pump 4 are both acid-resistant pumps to prevent the acidic gas generated by chlorosilane evaporation from affecting the various components.

[0052] Example 3

[0053] This embodiment describes the processing method for chlorosilane samples that do not contain high-boiling-point substances. The chlorosilane samples also include low-boiling-point chlorosilanes (31.8°C) evaporated under argon atmosphere at room temperature, as well as chlorosilanes with boiling points of around 60°C and above evaporated. The principle for evaporating chlorosilanes with boiling points of around 60°C and above is the same as that for chlorosilanes containing high-boiling-point substances: the boiling point is lowered by reducing the pressure, thereby accelerating the evaporation. For the evaporation of low-boiling-point chlorosilane (31.8℃) in a room-temperature argon environment, first place the container containing the chlorosilane inside the chamber 1, then close the switch door 10, run pump 3 but not vacuum pump 4, so that the inert gas fills the chamber 1, then run vacuum pump 4 to extract the air from the inside of the chamber 1. When the oxygen concentration detector 12 detects that the air content is close to zero, adjust vacuum pump 4 so that the rate at which vacuum pump 4 extracts the gas is consistent with the rate at which the inert gas fills the inside of the chamber 1, so that the inside of the chamber 1 is always in an environment surrounded by inert gas.

[0054] Finally, it should be noted that the above are merely preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention can have various modifications and variations. Without conflict, the embodiments and features described in the embodiments of this application can be arbitrarily combined with each other. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A pretreatment device for detecting chlorosilane samples, characterized in that, include: The enclosure comprises a box with an open end hinged to a door for rotating and sealing the enclosure; an air inlet and an air outlet communicating with the interior of the enclosure are respectively opened on the side wall of the enclosure; a fastener is located on the outer wall of the door and the outer wall of the enclosure for fastening the door to the opening of the enclosure; a gas storage tank is located on one side of the enclosure and is filled with inert gas; an exhaust port is opened on the side wall of the gas storage tank, and an air inlet pipe is connected between the exhaust port of the gas storage tank and the air inlet of the enclosure; a pump body is located between the enclosure and the gas storage tank and is connected to the air inlet pipe for pumping the gas in the gas storage tank into the interior of the enclosure; a vacuum pump is located on one side of the enclosure, and an exhaust pipe is connected between the vacuum pump and the air outlet of the enclosure; and a pressure gauge is located on the top of the enclosure, with the sensing end of the pressure gauge located inside the enclosure for real-time display of the pressure value inside the enclosure.

2. The pretreatment apparatus for detecting chlorosilane samples according to claim 1, characterized in that, An observation opening is provided on the side wall of the switch door, and an observation window is provided on the side wall of the switch door at the observation opening.

3. The pretreatment apparatus for detecting chlorosilane samples according to claim 2, characterized in that, The top of the chamber is also equipped with an oxygen concentration detector. The detection end of the oxygen concentration detector is located inside the chamber and is used to detect whether the interior of the chamber is a completely inert gas environment.

4. The pretreatment apparatus for detecting chlorosilane samples according to claim 3, characterized in that, The fastening component includes a buckle and a locking block. The buckle is located on the outer wall of the housing, and the locking block is located on the outer wall of the switch door. When the switch door is rotated to the opening of the housing, the interior of the housing is sealed by the engagement of the locking block and the buckle.

5. The pretreatment apparatus for detecting chlorosilane samples according to claim 4, characterized in that, It also includes a PLC control cabinet, which is located on one side of the housing and is electrically connected to the pump body and the vacuum pump respectively; a pressure sensor is also provided on the top of the housing, with the detection end of the pressure sensor located inside the housing. The pressure sensor is electrically connected to the PLC control cabinet and is used to receive the signal transmitted by the pressure sensor and adjust the working status of the pump body and the vacuum pump.

6. The pretreatment apparatus for detecting chlorosilane samples according to claim 5, characterized in that, An alarm is installed on the top of the PLC control cabinet. When the pressure inside the cabinet exceeds a threshold, the alarm is triggered by the PLC control cabinet.

7. The pretreatment apparatus for detecting chlorosilane samples according to claim 6, characterized in that, The side wall of the enclosure is also equipped with an explosion-proof pressure relief valve that communicates with the interior of the enclosure. The explosion-proof pressure relief valve is electrically connected to the PLC control cabinet. When the pressure value inside the enclosure is greater than the threshold, the explosion-proof pressure relief valve is opened by the PLC control cabinet to release the pressure.

8. The pretreatment apparatus for detecting chlorosilane samples according to claim 1, characterized in that, A sealing gasket is provided on the closed surface of the switch door and the box body.

9. The pretreatment apparatus for detecting chlorosilane samples according to claim 1, characterized in that, The vacuum pump is an acid-resistant vacuum pump, the housing is made of polychlorotrifluoroethylene (PTFE) sheet, and both the inlet pipe and the outlet pipe are PTFE pipes.

10. The pretreatment apparatus for detecting chlorosilane samples according to claim 1, characterized in that, The inner wall of the enclosure is coated with PTFE.

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