Polycrystalline silicon sample processing system for laboratory

Abstract

The utility model discloses a polycrystalline silicon sample processing system for laboratories, which belongs to the technical field of polycrystalline silicon sample processing devices for laboratories and comprises a sample container used for containing samples, a protective cover used for preventing gas from escaping is arranged outside the sample container, a heating mechanism is arranged in the protective cover, the protective cover is connected with an inert gas filling pipeline, and the inert gas filling pipeline is communicated with the sample container. A tail gas exhaust port is also formed in the protective cover and is connected with the water treatment tank through a pipeline I; a valve I and a valve II are arranged on the pipeline I and the pipeline II respectively, the water treatment tank and the alkali liquor tank are connected with an air inlet of a vacuum pump through a pipeline III and a pipeline IV respectively, and an air outlet of the vacuum pump is connected with a fuming cupboard. The problems that in the prior art, in a laboratory without a complete tail gas treatment facility, tail gas containing nitric oxide or chlorosilane, hydrogen chloride and the like escapes into the laboratory when a polycrystalline silicon sample is treated, the health of workers is unfavorable, and an exhaust system is easily corroded are solved.

Description

Technical Field

[0001] The utility model relates to the technical field of laboratory polysilicon sample processing devices, in particular to a laboratory polysilicon sample processing system. Background Art

[0002] For old factories in the polysilicon industry that have been in production for more than 10 years, the supporting facilities of the analysis and testing center are incomplete, and the available space is very limited due to factors such as the equipment and instruments installed in the current area. Especially in the pre-treatment process of samples such as liquid chlorosilane evaporation and silicon powder digestion, tail gas containing nitrogen oxides or chlorosilane, hydrogen chloride and other gases will be generated, and when the gas sample sampling bag is processed, chlorosilane and hydrogen chloride gases will be emitted / discharged into the working environment. These tail gases cannot directly enter the dedicated elution device / system, which is easy to cause the following problems:

[0003] 1. The amount of chlorosilane, hydrogen chloride and other gases emitted / discharged into the air is small and difficult to be centrally treated. In addition, the exhaust gas is emitted into the air, resulting in a poor working environment in the testing center, which is not conducive to the health of the staff;

[0004] 2. The exhaust gas continues to spread into the environment, causing impact on the environment;

[0005] 3. Because there are nitrogen oxides, hydrogen chloride and chlorosilane in the exhaust gas, there is a certain degree of corrosion to the fume hoods and exhaust facilities. In addition, after silica scales in the dead corners of the fume hoods, exhaust devices and other structures, it affects the service life of the exhaust facilities.

[0006] Therefore, for the tail gases containing nitrogen oxides or chlorosilane, hydrogen chloride, etc. generated when polysilicon samples are processed in the laboratory, especially for old plants with incomplete tail gas treatment facilities, it is necessary to optimize the existing equipment to improve the above problems. Utility Model Content

[0007] The utility model aims to solve the problem in the prior art that in laboratories without complete exhaust gas treatment facilities, especially in old factories producing polysilicon, exhaust gases containing nitrogen oxides, chlorosilanes, hydrogen chloride, etc. escape into the laboratory when polysilicon samples are processed, which is harmful to the health of the workers and easily corrodes structures such as fume hoods in the exhaust system.

[0008] In order to achieve the above-mentioned invention object, the technical solution of the utility model is as follows:

[0009] A laboratory polysilicon sample processing system comprises a sample container for containing samples, a protective cover for preventing gas from escaping is arranged outside the sample container, a heating mechanism is arranged inside the protective cover, an inert gas filling pipeline is connected to the protective cover, an exhaust gas outlet is also arranged on the protective cover, the exhaust gas outlet is connected to a water treatment tank through pipeline I; the exhaust gas outlet is connected to an alkali liquid tank through pipeline II, valves I and valve II are arranged on pipeline I and pipeline II respectively, the water treatment tank and the alkali liquid tank are connected to the air inlet of a vacuum pump through pipeline III and pipeline IV respectively, and the air outlet of the vacuum pump is connected to a fume hood.

[0010] Furthermore, a dryer I is provided on pipeline III, and a dryer II is provided on pipeline IV.

[0011] Furthermore, the heating mechanism is a graphite heating plate.

[0012] Furthermore, the graphite heating plate is installed below the sample container and is contact-connected with the sample container.

[0013] Furthermore, a gas inlet pipe nipple is provided in the water treatment tank and the alkali liquid tank, one end of the gas inlet pipe nipple is connected to pipeline I or pipeline II; the other end is provided with an opening, and a plurality of exhaust holes are provided on the pipe wall of the gas inlet pipe nipple close to the opening side, and a corrosion-resistant coating is provided on the gas inlet pipe nipple.

[0014] Furthermore, the water treatment tank and the alkali liquid tank are both provided with a gas inlet pipe nipple, one end of which is connected to pipeline I or pipeline II; a plurality of exhaust holes are provided on the end side and the pipe wall of the other end, and a corrosion-resistant coating is provided on the gas inlet pipe nipple.

[0015] Furthermore, a gas detector is provided in the protective cover, valve I and valve II are both solenoid valves, and the gas detector is respectively controlled and connected with valve I and valve II.

[0016] Furthermore, the pipeline II is also connected to a pipeline V for connecting to a gas sample bag, and a valve III is provided on the pipeline V.

[0017] Beneficial effects of the utility model:

[0018] 1. In the utility model, a protective cover is designed in the laboratory polysilicon sample processing system. The protective cover can isolate the sample in the sample container in a relatively closed space to prevent the sample in the sample container from emitting nitrogen oxides or chlorosilane, hydrogen chloride and other gases. The gas in the protective cover uses a vacuum pump to generate negative pressure, so that the entire system generates a pressure difference before and after, so that the tail gas collected in the protective cover enters the water treatment tank / alkali liquid tank through pipeline Ⅰ / pipeline Ⅱ, and the tail gas is processed, and then sent to the fume hood through pipeline Ⅲ / pipeline Ⅳ and vacuum pump, and then concentrated into the exhaust system or discharged to the outside. The sample processing system can process nitrogen oxides or chlorosilane, hydrogen chloride and other gases as much as possible, reduce pollution to the environment, and provide a better working environment for the staff. At the same time, it also reduces the corrosion of the tail gas generated by the laboratory polysilicon sample processing on the structure of the fume hood.

[0019] 2. In the utility model, a dryer I is provided on pipeline III, and a dryer II is provided on pipeline IV. The gas treated by the water treatment tank and the alkali liquid tank contains some water and carries some chlorosilane. The gas treated by dryer I / dryer II is purer and is not prone to residual fluids that have a corrosive effect on structures such as fume hoods.

[0020] 3. In the utility model, the heating mechanism uses a graphite heating plate, and the use of the graphite heating plate to heat the sample can accelerate the evaporation of chlorosilane and other logistics and shorten the entire treatment process. Preferably, the graphite heating plate is installed below the sample container and is contact-connected to the sample container.

[0021] Fourth, in the utility model, a special gas inlet pipe nipple is provided in the water treatment tank and the alkali liquid tank. Firstly, because the logistics in the tank body is highly corrosive, it is necessary to use a pipe made of corrosion-resistant materials or a structural component with a corrosion-resistant material coating sprayed on it to introduce the exhaust gas; secondly, in the exhaust gas treatment of polysilicon samples, silica suspended matter and scaling are easily generated, and the introduction of a special gas inlet pipe nipple can facilitate the handling of the staff. Preferably, the gas inlet pipe nipple and the water treatment tank / alkali liquid tank are designed to form a detachable structure. In this scheme, two better gas inlet pipe nipple structures are also proposed, which have a simple structure, are easy to process, and are also convenient for disassembly and maintenance. The gas inlet pipe nipple can be reused.

[0022] 5. In the utility model, a gas detector is provided in the protective cover. Valve I and valve II are both solenoid valves. The gas detector is respectively controlled and connected with valve I and valve II. According to the gas composition in the protective cover detected by the gas detector, valve I or valve II can be automatically opened to allow the tail gas to enter a suitable treatment tank (water treatment tank or alkali liquid tank) without manually opening the valve.

[0023] 6. In the utility model, the pipeline II is also connected to a pipeline V for connecting to a gas sample bag, and a valve III is provided on the pipeline V. When treating the gas sample bag, the tail gas can directly enter the pipeline II through the pipeline V, and then enter the alkali liquid tank for tail gas absorption treatment.

[0024] 7. In the utility model, the laboratory polysilicon sample processing system is suitable for various detection scenarios such as liquid chlorosilane impurity analysis, silicon powder detection, polysilicon gas samples, etc. in polysilicon sample processing. The system has a wide range of applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a structural schematic diagram of Example 1.

[0026] Figure 2 It is a structural schematic diagram of Example 2.

[0027] Figure 3 It is a structural schematic diagram of another implementation mode of the utility model.

[0028] Figure 4 It is a structural schematic diagram of another implementation mode of the utility model.

[0029] Figure 5 It is a structural schematic diagram of another preferred implementation mode of the utility model.

[0030] Figure 6 It is a structural schematic diagram of another preferred implementation mode of the utility model.

[0031] Figure 7 It is a structural schematic diagram of the gas inlet pipe short section.

[0032] Figure 8 It is a structural schematic diagram of another implementation of a gas inlet pipe short section.

[0033] Fig. 9 It is a structural schematic diagram of another implementation method of a gas inlet pipe short section.

[0034] Among them, 1. sample container; 2. protective cover; 3. heating mechanism; 4. inert gas filling pipeline; 5. tail gas outlet; 6. pipeline I; 7. water treatment tank; 8. pipeline II; 9. alkali liquid tank; 10. valve I; 11. valve II; 12. pipeline III; 13. pipeline IV; 14. vacuum pump; 15. fume hood; 16. dryer I; 17. dryer II; 18. gas inlet pipe nipple I; 19. gas inlet pipe nipple II; 20. opening; 21. exhaust hole; 22. corrosion-resistant coating; 23. gas detector; 24. gas sample bag; 25. pipeline V; 26. valve III; 14.1. air inlet; 14.2. air outlet. DETAILED DESCRIPTION

[0035] The present invention is further described in detail below in conjunction with the embodiments, but the implementation manner of the present invention is not limited thereto.

[0036] Example 1

[0037] This embodiment is the most basic implementation method, a laboratory polysilicon sample processing system, which relates to the technical field of laboratory polysilicon sample processing devices, and refers to Figure 1 , including a sample container 1 for holding a sample, a protective cover 2 for preventing gas from escaping is arranged outside the sample container 1, a heating mechanism 3 is arranged inside the protective cover 2, an inert gas filling pipeline 4 is connected to the protective cover 2, and an exhaust gas outlet 5 is also arranged on the protective cover 2, and the exhaust gas outlet 5 is connected to a water treatment tank 7 through a pipeline I6; the exhaust gas outlet 5 is connected to an alkali liquid tank 9 through a pipeline II8, and valves I10 and II11 are respectively arranged on the pipeline I6 and the pipeline II8, the water treatment tank 7 and the alkali liquid tank 9 are respectively connected to an air inlet 14.1 of a vacuum pump 14 through a pipeline III12 and a pipeline IV13, and an air outlet 14.2 of the vacuum pump 14 is connected to a fume hood 15.

[0038] In this embodiment, the protective cover 2 isolates the sample in the sample container 1 in a relatively closed space to prevent the sample in the sample container 1 from emitting gases such as nitrogen oxides or chlorosilane, hydrogen chloride, etc. The gas in the protective cover 2 generates negative pressure by using the vacuum pump 14, so that a pressure difference is generated before and after the entire system, so that the tail gas collected in the protective cover 2 enters the water treatment tank 7 / alkali liquid tank 9 through pipeline I6 / pipeline II8, and the water treatment tank 7 containing water or the alkali liquid tank 9 containing alkali liquid processes the tail gas, and then sends it to the fume hood 15 through pipeline III12 / pipeline IV13 and vacuum pump 14, and then enters the exhaust system or is discharged to the outside.

[0039] In this embodiment, the sample processing system can process nitrogen oxides or chlorosilane, hydrogen chloride and other gases as much as possible, reduce pollution to the environment, and provide a better working environment for the staff. At the same time, it also reduces the corrosion effect of the exhaust gas generated by the laboratory polysilicon sample processing on the structure of the fume hood 15.

[0040] Example 2

[0041] This embodiment is a further optimization of the embodiment 1. The difference is that the pipeline III 12 is provided with a dryer I 16, and the pipeline IV 13 is provided with a dryer II 17. Figure 2 The dryer Ⅰ16 dries the material flowing through the pipeline Ⅲ12, and the dryer Ⅱ17 dries the material flowing through the pipeline Ⅳ13, so as to prevent the chlorosilane from being carried in the material and then entering the rear-end fume hood 15.

[0042] Example 3

[0043] The difference between this embodiment and embodiment 1-2 is that the heating mechanism 3 is a graphite heating plate.

[0044] Preferably, the graphite heating plate is installed below the sample container 1 and is in contact connection with the sample container 1 .

[0045] Example 4

[0046] The present embodiment is different from the embodiments 1-3 in that the water treatment tank 7 is provided with a gas inlet pipe short section I18, and the alkali liquid tank 9 is provided with a gas inlet pipe short section II19. Figure 3 The gas inlet pipe short section Ⅰ18 is connected to the pipeline Ⅰ6, and the gas inlet pipe short section Ⅱ19 is connected to the pipeline Ⅱ8.

[0047] The gas inlet pipe nipple Ⅰ18 and the gas inlet pipe nipple Ⅱ19 in this embodiment have the same structure. An opening 20 is provided at the far end of the gas inlet pipe nipple. A plurality of exhaust holes 21 are provided on the pipe wall of the gas inlet pipe nipple near the opening 20. A corrosion-resistant coating 22 is provided on the gas inlet pipe nipple. The structure of the gas inlet pipe nipple is shown in FIG. Figure 7 .

[0048] Example 5

[0049] The present embodiment is different from the embodiments 1-3 in that the water treatment tank 7 is provided with a gas inlet pipe short section I18, and the alkali liquid tank 9 is provided with a gas inlet pipe short section II19. Figure 3 The gas inlet pipe short section Ⅰ18 is connected to the pipeline Ⅰ6, and the gas inlet pipe short section Ⅱ19 is connected to the pipeline Ⅱ8.

[0050] The gas inlet pipe nipple Ⅰ18 and the gas inlet pipe nipple Ⅱ19 in this embodiment have the same structure. A plurality of exhaust holes 21 are provided on the end side and the pipe wall of the gas inlet pipe nipple. A corrosion-resistant coating 22 is provided on the gas inlet pipe nipple. The structure of the gas inlet pipe nipple is shown in FIG. Figure 8 .

[0051] In specific implementation, the gas inlet pipe nipple can be designed into different shapes according to specific needs, and the exhaust hole 21 can also be designed into a circular, elliptical or long strip shape, such as Fig. 9 shown.

[0052] In addition, the gas inlet pipe short section I 18 and the gas inlet pipe short section II 19 can also be designed as short sections with different structures.

[0053] Example 6

[0054] The difference between this embodiment and embodiments 1-5 is that a gas detector 23 is provided in the protective cover 2. Figure 4Or 5, valve I10 and valve II11 are both solenoid valves, and the gas detector 23 is respectively controlled and connected with valve I10 and valve II11. According to the gas composition in the protective cover 2 detected by the gas detector 23, valve I10 or valve II11 can be automatically opened to allow the exhaust gas to enter the appropriate treatment tank (water treatment tank 7 or alkali liquid tank 9) without manual opening of the valve.

[0055] Example 7

[0056] Compared with Embodiments 1-6, the present embodiment is different in that the pipeline II8 is further connected to a pipeline V25 for connecting to a gas sample bag 24, and a valve III26 is provided on the pipeline V25. Figure 6 .

[0057] Example 9

[0058] This embodiment takes a relatively good laboratory polysilicon sample processing system as an example, and further illustrates this solution in combination with three practical application scenarios.

[0059] refer to Figure 6 , including a sample container 1 for holding a sample, a protective cover 2 for preventing gas from escaping is provided outside the sample container 1, a heating mechanism 3 is provided inside the protective cover 2, an inert gas filling pipeline 4 is connected to the protective cover 2, and an exhaust outlet 5 is also provided on the protective cover 2, and the exhaust outlet 5 is connected to the water treatment tank 7 through the pipeline Ⅰ6; the exhaust outlet 5 is connected to the alkali liquid tank 9 through the pipeline Ⅱ8, and the pipeline Ⅰ6 and the pipeline Ⅱ8 are respectively provided with valves Ⅰ10 and valve Ⅱ11, and the water treatment tank 7 and the alkali liquid tank 9 are respectively connected to the air inlet 14.1 of the vacuum pump 14 through the pipeline Ⅲ12 and the pipeline Ⅳ13, and the air outlet 14.2 of the vacuum pump 14 is connected to the fume hood 15. A dryer Ⅰ16 is provided on the pipeline Ⅲ12, and a dryer Ⅱ17 is provided on the pipeline Ⅳ13. The pipeline Ⅱ8 is also connected to a pipeline Ⅴ25 for connecting with a gas sample bag 24, and a valve Ⅲ26 is provided on the pipeline Ⅴ25.

[0060] In this embodiment, the heating mechanism 3 is a graphite heating plate, which is installed below the sample container 1 and is in contact connection with the sample container 1 .

[0061] In this embodiment, a gas inlet pipe nipple I18 is provided in the water treatment tank 7, a gas inlet pipe nipple II19 is provided in the alkali liquid tank 9, the gas inlet pipe nipple I18 is connected to the pipeline I6, and the gas inlet pipe nipple II19 is connected to the pipeline II8.

[0062] The gas inlet pipe nipple Ⅰ 18 and the gas inlet pipe nipple Ⅱ 19 in this embodiment have the same structure. Figure 7 An opening 20 is provided at the far end of the gas inlet pipe short section, a plurality of exhaust holes 21 are provided on the pipe wall of the gas inlet pipe short section near the opening 20, and a corrosion-resistant coating 22 is provided on the gas inlet pipe short section.

[0063] In this embodiment, a gas detector 23 is provided in the protective cover 2. Both valve I 10 and valve II 11 are solenoid valves. The gas detector 23 is control-connected to valve I 10 and valve II 11 respectively.

[0064] When using,

[0065] Ⅰ. When pre-treating the analysis of liquid chlorosilane impurities, open the valve on the inert gas filling pipeline 4 connected to the protective cover 2, connect argon or nitrogen to the front end of the protective cover 2, and the graphite heating plate in the protective cover 2 heats the chlorosilane to accelerate the evaporation of the sample liquid. The evaporated chlorosilane gas enters the water treatment tank 7 through the pipeline Ⅰ6. After being absorbed by the water treatment tank 7, the exhaust gas passes through the dryer Ⅰ16 and enters the fume hood 15, and then is sent to the next stage - the exhaust system for discharge.

[0066] Among them, the material mainly contains chlorosilane. Since chlorosilane is very easy to hydrolyze, the tail gas is sent to the water treatment tank 7 for treatment. Water is used as an absorption liquid to absorb chlorosilane. When a large amount of suspended silica appears in the water treatment tank 7 and no longer increases, it can be cleaned (clean off the suspended silica or scrape off the silica scale in time) and the water can be directly replaced.

[0067] Ⅱ. When acid digestion is added during silicon powder detection, argon gas may not be introduced. The valve on the inert gas filling pipeline 4 is closed, the valve Ⅰ10 on the pipeline Ⅰ6 is closed, and the valve Ⅱ11 on the pipeline Ⅱ8 is opened. The tail gas containing nitrogen oxides and acid mist generated is sent to the alkali liquid tank 9 for absorption treatment to ensure that the tail gas is effectively absorbed. Since the polysilicon production process involves the use of industrial alkali liquid, the industrial alkali liquid produced can be directly used instead of purchasing alkali flakes to configure alkali liquid, which can reduce the cost of use. The gas after absorption treatment is then sent to the dryer Ⅱ17 for drying. The dried gas enters the fume hood 15 and then sent to the next stage - the exhaust system for discharge.

[0068] Ⅲ. When the gas sample bag is processed, the tail gas involves acidic gases such as chlorosilane and hydrogen chloride. The gas sample bag 24 can be directly connected to the alkali liquid tank 9 through the pipeline V25, and the alkali liquid is used to absorb the acidic gases such as chlorosilane and hydrogen chloride. The remaining steps are the same as Ⅱ. The gas after the alkali liquid absorption treatment is sent to the dryer Ⅱ17 for drying. The dried gas enters the fume hood 15 and is then sent to the next stage - the exhaust system for discharge.

[0069] From the above, it can be seen that by using the laboratory polysilicon sample processing system of the utility model, it is possible to realize the effective absorption of corrosive and toxic tail gases such as nitrogen oxides or chlorosilanes, hydrogen chloride, etc. present during the processing of polysilicon samples in laboratories that are not equipped with complete tail gas treatment facilities, especially in the laboratories of old factories producing polysilicon, and then send them to the post-processing system for further processing or discharge to the outside, thereby achieving the "elution absorption" effect and avoiding the special construction of large-scale spray absorption equipment, saving construction costs.

Claims

1. A laboratory polysilicon sample processing system, characterized in that: The invention comprises a sample container (1) for containing a sample. The sample container (1) is provided with a protective cover (2) for preventing gas from escaping. The protective cover (2) is provided with a heating mechanism (3). The protective cover (2) is connected to an inert gas charging pipeline (4). The protective cover (2) is also provided with an exhaust gas outlet (5). The exhaust gas outlet (5) is connected to a water treatment tank (7) through a pipeline I (6). The exhaust gas outlet (5) is connected to an alkali liquid tank (9) through a pipeline II (8). The pipeline I (6) and the pipeline II (8) are provided with valves I (10) and II (11) respectively. The water treatment tank (7) and the alkali liquid tank (9) are connected to an air inlet (14.1) of a vacuum pump (14) through pipelines III (12) and IV (13) respectively. The air outlet (14.2) of the vacuum pump (14) is connected to a fume hood (15).

2. The laboratory polysilicon sample processing system according to claim 1, characterized in that: A dryer I (16) is provided on pipeline III (12), and a dryer II (17) is provided on pipeline IV (13).

3. The laboratory polysilicon sample processing system according to claim 1, characterized in that: The heating mechanism (3) is a graphite heating plate.

4. The laboratory polysilicon sample processing system according to claim 3, characterized in that: The graphite heating plate is installed below the sample container (1) and is contact-connected to the sample container (1).

5. The laboratory polysilicon sample processing system according to claim 1, characterized in that: The water treatment tank (7) and the alkali liquid tank (9) are both provided with a gas inlet pipe nipple, one end of the gas inlet pipe nipple is connected to the pipeline I (6) or the pipeline II (8); the other end is provided with an opening (20), a plurality of exhaust holes (21) are provided on the pipe wall of the gas inlet pipe nipple near the opening (20), and a corrosion-resistant coating (22) is provided on the gas inlet pipe nipple.

6. The laboratory polysilicon sample processing system according to claim 1, characterized in that: The water treatment tank (7) and the alkali liquid tank (9) are both provided with a gas inlet pipe nipple, one end of which is connected to pipeline I (6) or pipeline II (8); a plurality of exhaust holes (21) are provided on the end side and the pipe wall of the other end, and a corrosion-resistant coating (22) is provided on the gas inlet pipe nipple.

7. A laboratory polysilicon sample processing system according to any one of claims 1 to 6, characterized in that: A gas detector (23) is provided in the protective cover (2); valve I (10) and valve II (11) are both solenoid valves; and the gas detector (23) is controllably connected to valve I (10) and valve II (11), respectively.

8. The laboratory polysilicon sample processing system according to claim 1, characterized in that: The pipeline II (8) is also connected to a pipeline V (25) for connecting to a gas sample bag (24), and a valve III (26) is provided on the pipeline V (25).

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