Silicon powder detection device
By designing a silicon powder detection device including a heat-receiving bottle, a chlorosilane absorption hydrolysis bottle and a exhaust gas inspection bottle, the difficulty of detecting chlorosilane in silicon powder in the prior art is solved, and a fast, safe and efficient detection effect is achieved.
Patent Information
- Application Number
- CN202421761029.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-24
- Publication Date
- 2025-06-24
- Estimated Expiration
- 2034-07-24
AI Technical Summary
When the prior art detects chlorosilane in silicon powder produced by-production in polycrystalline silicon, there are problems such as long operating time, incomplete component extraction, and limited equipment. The uniformity and representativeness of the sample are difficult to guarantee, making it difficult to achieve detection.
A silicon powder detection device is designed, including a heat-receiving bottle, a chlorosilane absorption hydrolysis bottle and a exhaust gas inspection bottle. Through heating and hydrolysis reactions, chlorosilane in the silicon powder is absorbed and detected, and reabsorbed by a exhaust gas inspection bottle to improve detection safety.
The rapid detection of chlorosilane content of silicon powder is achieved, which is simple to operate and high efficiency, and improves the safety of the device and the accuracy of detection.
Smart Images
Figure CN223021687U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of silicon powder detection, and particularly relates to a silicon powder detection device. Background Art
[0002] Among the by-product silicon powder in the polysilicon production process, there is a certain amount of chlorosilane. The main hazards of chlorosilane are low boiling point, easy volatilization, and release of toxic gases (hydrogen chloride), and even spontaneous combustion. During transportation and smelting, if not properly disposed of, it will pose a safety hazard.
[0003] In the prior art, according to the production process, it can be judged that in the by-product silicon powder, the chlorosilane is mainly hexachloroethylsilane and a small amount of trichlorosilane and silicon tetrachloride. At present, the best way for gas phase analysis is purge and trap, but purge and trap has problems such as long operation time, incomplete component extraction, equipment limitation, and problems such as whether the sample is uniform and representative, and recondensation of low-boiling components due to temperature change, resulting in difficulty in implementing this method. Moreover, after hydrolysis analysis, detecting chloride ions and detecting the content of hydrogen chloride cannot fully reflect the quality of the by-product silicon powder. Summary of the Utility Model
[0004] The purpose of the utility model is to develop a silicon powder detection device with simple operation and high detection operation efficiency.
[0005] The utility model is realized through the following technical solutions:
[0006] A silicon powder detection device includes:
[0007] A housing;
[0008] A partition plate, arranged in the housing;
[0009] A heating bottle, located in the housing and arranged on the partition plate;
[0010] A heating plate, arranged at the bottom of the heating bottle;
[0011] A chlorosilane absorption and hydrolysis bottle and a first tail gas inspection bottle, arranged in the housing;
[0012] Wherein, the heating bottle, the chlorosilane absorption and hydrolysis bottle and the first tail gas inspection bottle are sequentially arranged in the housing and are all connected with an intake pipe and an exhaust pipe. The exhaust pipe of the heating bottle is connected to the intake pipe of the chlorosilane absorption and hydrolysis bottle, the exhaust pipe of the chlorosilane absorption and hydrolysis bottle is connected to the intake pipe of the first tail gas inspection bottle, the intake pipe of the heating bottle extends out of the housing, and a first valve is arranged on the intake pipe outside the housing.
[0013] Optionally, a second tail gas inspection bottle is further provided inside the housing. An intake pipe and an outlet pipe are connected to the second tail gas inspection bottle. The outlet pipe of the first tail gas inspection bottle is connected to the intake pipe of the second tail gas inspection bottle.
[0014] Optionally, the bottom ends of the intake pipes inside the heating bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle extend to the lower part inside the bottles.
[0015] Optionally, the heating bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle are sequentially arranged inside the housing.
[0016] Optionally, there is water inside the chlorosilane absorption and hydrolysis bottle with a liquid level higher than the bottom end of the intake pipe inside it.
[0017] Optionally, there is a neutral indicator inside the first tail gas inspection bottle and the second tail gas inspection bottle with a liquid level higher than the bottom end of the intake pipe inside them.
[0018] Optionally, the neutral indicator is bromothymol blue indicator.
[0019] Optionally, a heating seat is provided on the partition board. A seat groove is provided at the top of the heating seat. The heating bottle is arranged inside the seat groove, and the heating plate is arranged at the bottom of the seat groove.
[0020] Optionally, a top cover is provided at the top of the housing. Bottle stoppers are provided inside the top bottle mouths of the heating bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle. The intake pipe and the outlet pipe are arranged on the bottle stoppers.
[0021] Optionally, an inlet pipe and a drain pipe extending outside the housing are respectively connected to the top and bottom of the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle. A second valve is provided on the inlet pipe, and a third valve is provided on the drain pipe.
[0022] The beneficial effects of the present utility model are:
[0023] The structure of the present utility model is simple, with low cost and easy to carry. It can quickly detect the chlorosilane content in silicon powder, with simple operation and high efficiency. The provided first tail gas inspection bottle and second tail gas inspection bottle can reabsorb the uncompletely absorbed chlorosilane and hydrogen chloride, improving the safety of the device during use. Description of the Drawings
[0024] To more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0025] Figure 1 This is the structural diagram of the utility model.
[0026] Reference numerals: 1, housing; 2, partition; 3, heating base; 4, seat groove; 5, heating plate; 6, heat-receiving bottle; 7, bottle stopper; 8, intake pipe; 9, exhaust pipe; 10, first valve; 11, second valve; 12, third valve; 13, liquid inlet pipe; 14, drain pipe; 15, chlorosilane absorption and hydrolysis bottle; 16, first tail gas inspection bottle; 17, second tail gas inspection bottle. Detailed implementation manners
[0027] In the following, only some exemplary embodiments are simply described. As those skilled in the art can recognize, the described embodiments can be modified in various different ways without departing from the spirit or scope of the present invention. Therefore, the drawings and the description are considered to be exemplary in nature rather than restrictive.
[0028] In the description of the present invention, it should be understood that the orientation or positional relationships indicated by 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. are based on the orientation or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus cannot be understood as a limitation to the present invention.
[0029] The following will describe the embodiments of the present utility model in detail with reference to the drawings.
[0030] As Figure 1 shown, the present utility model discloses a silicon powder detection device, which includes a housing 1. A detachable top cover is provided at the top of the housing 1. Inside the housing 1, a heat-receiving bottle 6, a chlorosilane absorption and hydrolysis bottle 15, a first tail gas inspection bottle 16, and a second tail gas inspection bottle 17 are sequentially arranged.
[0031] Inside the housing 1 at the bottom of the heat-receiving bottle 6, there is a partition 2 which is made of heat-insulating material and has the function of heat insulation. On the partition 2, there is a heating seat 3. At the top of the heating seat 3, there is a seat groove 4. At the bottom of the seat groove 4, there is a heating plate 5. The heat-receiving bottle 6 is arranged in the seat groove 4.
[0032] Inside the top bottle mouths of the heat-receiving bottle 6, the chlorosilane absorption and hydrolysis bottle 15, the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17, there are bottle stoppers 7. Inside the bottle stoppers 7, there are air inlet pipes 8 and air outlet pipes 9. The bottom end of the air inlet pipe 8 extends vertically downward to the lower part inside the bottle body where the bottle stopper 7 is located. The bottom end of the air outlet pipe 9 is at the bottom of the bottle stopper 7.
[0033] The air inlet pipe 8 on the bottle stopper 7 of the heat-receiving bottle 6 passes through the side wall of the housing 1. A first valve 10 is arranged on the air inlet pipe 8 and is located outside the housing 1. The air outlet pipe 9 on the bottle stopper 7 of the heat-receiving bottle 6 is communicated with the air inlet pipe 8 on the bottle stopper 7 of the chlorosilane absorption and hydrolysis bottle 15 through a pipeline.
[0034] The air outlet pipe 9 on the bottle stopper 7 of the chlorosilane absorption and hydrolysis bottle 15 is communicated with the air inlet pipe 8 on the bottle stopper 7 of the first tail gas inspection bottle 16 through a pipeline. The air outlet pipe 9 on the bottle stopper 7 of the first tail gas inspection bottle 16 is communicated with the air inlet pipe 8 on the bottle stopper 7 of the second tail gas inspection bottle 17 through a pipeline. The air outlet pipe 9 on the bottle stopper 7 of the second tail gas inspection bottle 17 extends outside the housing 1.
[0035] On the chlorosilane absorption and hydrolysis bottle 15, the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17, there are liquid inlet pipes 13 and liquid discharge pipes 14. The liquid inlet pipes 13 are communicated with the top of the bottle body below the bottle stopper 7. The liquid discharge pipes 14 are communicated with the bottom of the bottle body. Both the liquid inlet pipes 13 and the liquid discharge pipes 14 extend outside the housing 1. A second valve 11 is arranged on the liquid inlet pipe 13 outside the housing 1. A third valve 12 is arranged on the liquid discharge pipe 14 outside the housing 1. Both the liquid inlet pipes 13 and the liquid discharge pipes 14 are inclined. The lower end of the liquid inlet pipe 13 is communicated with the bottle body. The higher end of the liquid discharge pipe 14 is communicated with the bottle body.
[0036] Inside the chlorosilane absorption and hydrolysis bottle 15, there is water with a liquid level higher than the bottom end of the air inlet pipe 8 inside it. Inside the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17, there is a neutral indicator with a liquid level higher than the bottom end of the air inlet pipe 8 inside it. The neutral indicator can be bromothymol blue indicator.
[0037] Before the silicon powder is detected, water is injected into the chlorosilane absorption and hydrolysis bottle 15 through the liquid inlet pipe 13 to submerge the bottom end of the gas inlet pipe 8. A neutral indicator is injected into the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17 through the liquid inlet pipe 13 to submerge the bottom end of the gas inlet pipe 8. The top cover and the bottle stopper 7 of the heating bottle 6 are opened, and the silicon powder is placed into the heating bottle 6. When the silicon powder is detected, the heating bottle 6 is heated by the heating plate 5, and the heating temperature is 130-140 degrees. The gas inlet pipe 8 of the heating bottle 6 is connected to the gas source of the inert gas and the first valve 10 is opened. The inert gas is introduced into the bottom of the heating bottle 6 to carry away the low-boiling-point chlorosilane evaporated from the silicon powder. The chlorosilane enters the chlorosilane absorption and hydrolysis bottle 15 with the inert gas for hydrolysis and produces hydrogen chloride. The inert gas then enters the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17 in sequence through the pipeline and is output.
[0038] Under normal circumstances, the chlorosilane absorption and hydrolysis bottle 15 can absorb the chlorosilane completely. The inert gas entering the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17 usually does not contain chlorosilane and hydrogen chloride. At this time, the third valve 12 on the drain pipe 14 of the chlorosilane absorption and hydrolysis bottle 15 is opened, and the solution in the chlorosilane absorption and hydrolysis bottle 15 is discharged and the hydrogen chloride content is detected, so as to indirectly detect the chlorosilane. The hydrogen chloride content detection can use the titration method, which is the prior art and will not be elaborated here.
[0039] In a few cases, if the first tail gas inspection bottle 16 changes color and the second tail gas inspection bottle 17 does not change color, it means that the chlorosilane absorption and hydrolysis bottle 15 has not absorbed the chlorosilane completely, and there is chlorosilane or hydrogen chloride entering the first tail gas inspection bottle 16, and the first tail gas inspection bottle 16 absorbs the chlorosilane and hydrogen chloride completely. The absorption liquid in the first tail gas inspection bottle 16 also needs to be included in the calculation. At this time, the solutions in the chlorosilane absorption and hydrolysis bottle 15 and the first tail gas inspection bottle 16 need to be combined for titration and calculation.
[0040] In extremely rare cases, both the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17 change color. In this case, a small amount of chlorosilane and hydrogen chloride may be output outside the housing 1 with the inert gas. Due to the three-time absorption of the chlorosilane absorption and hydrolysis bottle 15, the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17, the amount of chlorosilane and hydrogen chloride output outside the housing 1 is also very small and will not cause damage to the environment and human body. At this time, since it is impossible to judge whether the second tail gas inspection bottle 17 has completely absorbed the remaining chlorosilane and hydrogen chloride, the detection operation fails and the detection needs to be carried out again or the detection device needs to be checked for faults.
[0041] After the detection operation is completed, the heating bottle 6 can be taken out for cleaning. The chlorosilane absorption and hydrolysis bottle 15, the first tail gas inspection bottle 16 and the second tail gas inspection bottle 17 can be cleaned through the liquid inlet pipe 13 and the drain pipe 14, or they can be taken out for cleaning by opening the top cover.
[0042] Chlorosilanes in silicon powder may cause accidents such as fires during transportation and smelting. However, not all chlorosilanes cause accidents. For example, the boiling point of hexachloroethylsilane reaches 144 degrees, which is safe under normal operating conditions. Therefore, for the risk assessment of silicon powder in this utility model, it is only necessary to detect the low-boiling components in chlorosilanes. Thus, the heating temperature is 130 - 140 degrees, and then the chlorosilanes are detected by indirectly detecting the hydrogen chloride after hydrolysis, avoiding the use of a relatively expensive gas chromatograph, with relatively simple operation, simplified detection procedures, and being easier to operate.
[0043] This utility model has a simple structure, low cost, and is portable. It can quickly detect the chlorosilane content in silicon powder, with simple operation and high efficiency. The provided first tail gas inspection bottle 16 and second tail gas inspection bottle 17 can re-absorb the unabsorbed chlorosilanes and hydrogen chloride, improving the safety of the device during use.
[0044] The above embodiments are only the preferred embodiments of this utility model, and do not limit the technical solutions of this utility model. Any technical solutions that can be achieved on the basis of the above embodiments without creative labor shall be regarded as falling within the scope of the patent rights of this utility model.
Claims
1. A silicon powder detection device, characterized in that: include: case; A partition plate is disposed in the shell; A heated bottle is located in the shell and is arranged on the partition; A heating plate is arranged at the bottom of the heated bottle; The chlorosilane absorption and hydrolysis bottle and the first tail gas inspection bottle are arranged in the shell; Among them, the heated bottle, chlorosilane absorption and hydrolysis bottle and the first exhaust gas inspection bottle are arranged in sequence in the shell and are all connected with an air inlet pipe and an air outlet pipe. The air outlet pipe of the heated bottle is connected with the air inlet pipe of the chlorosilane absorption and hydrolysis bottle, and the air outlet pipe of the chlorosilane absorption and hydrolysis bottle is connected with the air inlet pipe of the first exhaust gas inspection bottle. The air inlet pipe of the heated bottle extends out of the shell and a first valve is provided on the air inlet pipe outside the shell.
2. The silicon powder detection device according to claim 1, characterized in that: A second exhaust gas inspection bottle is also provided in the shell, and an air inlet pipe and an air outlet pipe are connected to the second exhaust gas inspection bottle, and the air outlet pipe of the first exhaust gas inspection bottle is connected to the air inlet pipe of the second exhaust gas inspection bottle.
3. The silicon powder detection device according to claim 2, characterized in that: The bottom ends of the air inlet pipes in the heating bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle extend to the lower part of the bottle body.
4. The silicon powder detection device according to claim 2, characterized in that: The heating bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle are arranged in sequence in the shell.
5. The silicon powder detection device according to claim 2, characterized in that: The chlorosilane absorption and hydrolysis bottle is provided with water whose liquid level is higher than the bottom end of the internal air inlet pipe.
6. The silicon powder detection device according to claim 2, characterized in that: The first exhaust gas inspection bottle and the second exhaust gas inspection bottle are provided with a neutral indicator whose liquid level is higher than the bottom end of the internal air intake pipe.
7. The silicon powder detection device according to claim 6, characterized in that: The neutral indicator is bromothymol blue indicator.
8. The silicon powder detection device according to claim 2, characterized in that: A heating seat is arranged on the partition, a seat groove is arranged on the top of the heating seat, the heated bottle is arranged in the seat groove, and the heating plate is arranged at the bottom of the seat groove.
9. The silicon powder detection device according to claim 2, characterized in that: A top cover is provided on the top of the shell, and bottle plugs are provided in the top bottle openings of the heated bottle, the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle, and the air inlet pipe and the air outlet pipe are arranged on the bottle plugs.
10. The silicon powder detection device according to claim 2, characterized in that: The tops and bottoms of the chlorosilane absorption and hydrolysis bottle, the first tail gas inspection bottle and the second tail gas inspection bottle are respectively connected with a liquid inlet pipe and a liquid discharge pipe extending out of the shell, the liquid inlet pipe is provided with a second valve, and the liquid discharge pipe is provided with a third valve.