An online chlorosilane vaporization detection system for polysilicon production lines

By designing the chlorosilane online vaporization detection system on the polycrystalline silicon production line, the problems of complex, time-consuming and low accuracy in the existing technology are solved, and efficient and accurate online detection and automated processing are achieved to ensure production stability.

CN116500166BActive Publication Date: 2025-08-12XINJIANG DAQO NEW ENERGY CO LTD
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Patent Information

Application Number
CN202310519645.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-10
Publication Date
2025-08-12
Estimated Expiration
2043-05-10

AI Technical Summary

Technical Problem

In the prior art, the chlorosilane detection method is an offline solution, which leads to the complex and time-consuming inspection process, and the inability to obtain data in time. Human operation is prone to sample contamination, affecting the detection accuracy and production stability.

Method used

Design a chlorosilane online vaporization detection system for polycrystalline silicon production lines, including feed vaporization system, sample preparation box, gas chromatograph and control device, and control chlorosilane flow rate is controlled through a vaporizer and a current limiting throttling orifice plate to realize online detection and automated sample processing.

Benefits of technology

It improves the detection efficiency and accuracy of the test results, reduces the impact on the production process, realizes automated control and sample freshness, and reduces the pollution risk caused by human operations.

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Abstract

The present invention relates to the technical field of polysilicon production equipment, and in particular to an online chlorosilane vaporization detection system for a polysilicon production line, wherein the fluid inlet of a vaporizer is connected to a chlorosilane delivery pipeline; a flow-limiting orifice plate 1 is arranged on the chlorosilane delivery pipeline; a flow-limiting orifice plate 2 is arranged at the fluid inlet of the vaporizer; a pressure relief pipeline 1 is arranged on the fluid outlet of the vaporizer; a sampling pipeline is arranged on the fluid outlet of the vaporizer; multiple fluid inlets on a sample preparation box are respectively connected to sampling pipelines of multiple feed vaporization systems; the sample preparation box has a detection outlet and a circulation outlet; a flow direction control valve is arranged between the fluid inlet and the detection outlet and the circulation outlet; a control device is respectively connected to a pressure transmitter, a temperature sensor, a pressure relief regulating valve, a sampling control valve and a flow direction control valve. The present invention is used to improve detection efficiency and the accuracy of detection results, and reduce the impact on the production process.
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Description

Technical Field

[0001] The present invention relates to the technical field of polysilicon production equipment, and in particular to an online chlorosilane vaporization detection system for a polysilicon production line. Background Art

[0002] Chlorosilane is the most important raw material in the production of polysilicon. Chlorosilane is mixed with a small amount of dichlorosilane. During the production process, the content of dichlorosilane in chlorosilane needs to be controlled within a predetermined range to ensure the quality grade of the finished polysilicon.

[0003] Currently, the detection of dichlorosilane content in chlorosilane materials relies on an offline approach. This requires manual sampling, processing, and then sending the sample to a testing laboratory for sample preparation. Results are then obtained only after testing with specialized analytical equipment. This existing testing method results in a complex and time-consuming process, lacks timely data, and has limited data availability. Furthermore, manual operation can easily contaminate the sample being tested, affecting the accuracy of the test results. Furthermore, frequent on-site operations lead to excessive uncertainties, impacting stable production operations, and increasing the risk of operational errors. Summary of the Invention

[0004] In view of this, the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, the main purpose of which is to improve the detection efficiency and the accuracy of the detection results and reduce the impact on the production process.

[0005] To achieve the above objectives, the present invention mainly provides the following technical solutions:

[0006] An embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, comprising: a feed vaporization system, a chlorosilane storage container, a sample preparation box, a gas chromatograph, and a control device;

[0007] The feed vaporization system includes: a chlorosilane delivery pipeline, a vaporizer, a first flow limiting throttling orifice plate and a second flow limiting throttling orifice plate;

[0008] The chlorosilane delivery pipeline is provided with a control valve 1;

[0009] A second control valve is provided on the chlorosilane delivery pipeline;

[0010] The chlorosilane delivery pipeline is provided with an on-site pressure gauge;

[0011] The fluid inlet of the vaporizer is connected to the chlorosilane delivery pipeline; the vaporizer is provided with a heat exchange medium inlet and a heat exchange medium outlet;

[0012] The flow limiting orifice plate 1 is arranged on the chlorosilane delivery pipeline, between the control valve 1 and the control valve 2;

[0013] The second flow limiting orifice plate is arranged at the fluid inlet of the vaporizer;

[0014] A pressure relief pipeline 1 is provided on the fluid outlet of the vaporizer; a pressure relief regulating valve is provided on the pressure relief pipeline 1; and a check valve 1 is provided on the pressure relief pipeline 1;

[0015] The vaporizer is provided with a temperature sensor and a pressure transmitter;

[0016] A sampling pipe is provided on the fluid outlet of the vaporizer;

[0017] There are multiple feed vaporization systems;

[0018] The sample preparation box is provided with a plurality of fluid inlets; the plurality of fluid inlets are respectively connected to the sampling pipes of the plurality of feed vaporization systems;

[0019] The sampling pipeline is provided with a sampling control valve;

[0020] The sample preparation box is provided with a detection outlet;

[0021] The feed port of the gas chromatograph is connected to the detection outlet; a post-detection loop is provided on the discharge port of the gas chromatograph; the post-detection loop is connected to the pressure relief pipe;

[0022] The sample preparation box is provided with a circulation outlet; the circulation outlet is communicated with the fluid inlet; a circulation pipeline is provided on the circulation outlet; the circulation pipeline is communicated with the pressure relief pipeline;

[0023] A flow direction control valve is provided between the fluid inlet, the detection outlet and the circulation outlet, for controlling the fluid inlet to be connected to the detection outlet or to be connected to the circulation outlet;

[0024] The sampling pipe is provided with an electric heating device;

[0025] The chlorosilane storage container is connected to the chlorosilane delivery pipeline through a liquid return line; the liquid return line is provided with a manual regulating valve and a second check valve;

[0026] The control device is connected to the pressure transmitter, the temperature sensor, the pressure relief regulating valve, the sampling control valve and the flow control valve respectively, and is used to collect temperature and pressure signals and control the pressure relief regulating valve, the sampling control valve and the flow control valve.

[0027] Furthermore, the aperture of the second flow limiting and throttling orifice plate is smaller than the aperture of the first flow limiting and throttling orifice plate.

[0028] Furthermore, the aperture of the flow limiting orifice plate 1 is 0.4-0.6 mm;

[0029] The aperture of the second flow limiting and throttling orifice plate is 0.1-0.3 mm.

[0030] Furthermore, the medium temperature used in the vaporizer is 80-150°C.

[0031] Furthermore, the heat exchange medium of the evaporator is steam or water.

[0032] Furthermore, the pressure in the vaporizer is maintained at 0.1-0.3 MPa.

[0033] Furthermore, it also includes: a pressure relief system;

[0034] The pressure relief system is in communication with the pressure relief pipeline.

[0035] Furthermore, a pressure relief line 2 is provided on the pressure relief line 1; the input end of the pressure relief line 2 is connected to the pressure relief line 1 and is located upstream of the pressure relief regulating valve; the output end of the pressure relief line 2 is connected to the pressure relief line 1 and is located between the pressure relief regulating valve and the check valve 1.

[0036] By means of the above technical solution, the chlorosilane online vaporization detection system for a polysilicon production line of the present invention has at least the following advantages:

[0037] It can improve detection efficiency and the accuracy of test results, and reduce the impact on the production process.

[0038] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 A schematic diagram of an online chlorosilane vaporization detection system for a polysilicon production line provided in an embodiment of the present invention.

[0040] As shown in the figure:

[0041] 1 is the chlorosilane delivery pipeline, 2 is the flow limiting throttling orifice plate 1, 3 is the flow limiting throttling orifice plate 2, 4 is the vaporizer, 5 is the sample preparation box, 6 is the chlorosilane storage container, 7 is the control valve 1, 8 is the control valve 2, 9 is the on-site pressure gauge, 10 is the heat exchange medium inlet, 11 is the heat exchange medium outlet, 12 is the pressure relief pipeline 1, 13 is the pressure relief pipeline 2, 14 is the sampling pipeline, 15 is the gas chromatograph, 16 is the post-detection loop, 17 is the circulation pipeline, 18 is the return liquid pipeline, and 19 is the pressure relief system. DETAILED DESCRIPTION

[0042] To further illustrate the technical means and effects employed by the present invention to achieve its intended objectives, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention is provided in conjunction with the accompanying drawings and preferred embodiments. In the following description, different references to "one embodiment" or "embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.

[0043] like Figure 1 As shown, one embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, comprising: a feed vaporization system, a chlorosilane storage container 6, a sample preparation box 5, a gas chromatograph 15, and a control device. The feed vaporization system includes: a chlorosilane delivery pipeline 1, a vaporizer 4, a flow-limiting orifice plate 2, and a flow-limiting orifice plate 3. The input end of the chlorosilane delivery pipeline 1 is connected to the chlorosilane delivery channel in the polysilicon production system to guide the material to be tested. The chlorosilane delivery pipeline 1 is provided with a control valve 1 7 for controlling the flow rate of the chlorosilane delivery pipeline 1; the chlorosilane delivery pipeline 1 is provided with a control valve 2 8 for controlling the flow rate of the chlorosilane delivery pipeline 1. The chlorosilane delivery pipeline 1 is provided with a field pressure gauge 9 for detecting the pressure within the chlorosilane delivery pipeline 1.

[0044] The fluid inlet of vaporizer 4 is connected to chlorosilane delivery pipeline 1. Vaporizer 4 is provided with a heat exchange medium inlet 10 and a heat exchange medium outlet 11 for circulating the heat exchange medium to heat and vaporize the chlorosilane. In this embodiment, the medium temperature used in vaporizer 4 is preferably between 80°C and 150°C to ensure heated vaporization of the chlorosilane. Furthermore, vaporizer 4 preferably uses steam or water as the heat exchange medium, which provides stable heating and low cost.

[0045] The flow-limiting orifice plate 1-2 is arranged on the chlorosilane delivery pipeline 1, between the control valve 1-7 and the control valve 2-8, and is used to limit the flow of chlorosilane. The arrangement of the control valve 1-7 and the control valve 2-8 facilitates the cleaning and replacement of the flow-limiting orifice plate 1-2. The flow-limiting orifice plate 2-3 is arranged at the fluid inlet of the vaporizer 4, and is used to further limit the flow of chlorosilane. In this embodiment, the aperture of the flow-limiting orifice plate 2-3 is preferably smaller than the aperture of the flow-limiting orifice plate 1-2, so as to further limit the flow of chlorosilane and maintain a small flow rate entering the vaporizer 4. It is further preferred that the aperture of the flow-limiting orifice plate 1-2 is 0.4-0.6 mm; the aperture of the flow-limiting orifice plate 2-3 is 0.1-0.3 mm, so as to meet the flow requirements of the current gas chromatograph 15. Of course, apertures of other sizes are not excluded.

[0046] A pressure relief line 12 is provided at the fluid outlet of vaporizer 4 to relieve the gas pressure within vaporizer 4. A pressure relief regulating valve is installed on pressure relief line 12 to adjust the pressure relief flow rate and maintain the gas pressure within vaporizer 4. In this embodiment, the pressure within vaporizer 4 is preferably maintained between 0.1 and 0.3 MPa to meet typical testing requirements. A check valve is installed on pressure relief line 12 to ensure unidirectional gas flow.

[0047] The vaporizer 4 is provided with a temperature sensor and a pressure transmitter for detecting the temperature and pressure data in the vaporizer 4. A sampling pipe 14 is provided at the fluid outlet of the vaporizer 4; there are multiple feed vaporization systems; and the multiple feed vaporization systems are connected in parallel.

[0048] The sample preparation box 5 has multiple fluid inlets, which are respectively connected to the sampling pipes 14 of the multiple feed vaporization systems. The sampling pipes 14 are provided with sampling control valves for controlling the on-off of the sampling pipes 14 . The sample preparation box 5 is provided with a detection outlet; the feed port of the gas chromatograph 15 is connected to the detection outlet; the discharge port of the gas chromatograph 15 is provided with a post-detection loop 16; the post-detection loop 16 is connected to the pressure relief line 12; the sample preparation box 5 is provided with a circulation outlet; the circulation outlet is connected to the fluid inlet; a circulation line 17 is provided on the circulation outlet; the circulation line 17 is connected to the pressure relief line 12; a flow control valve is provided between the fluid inlet and the detection outlet and the circulation outlet, which is used to control the fluid inlet to be connected to the detection outlet or to the circulation outlet; when it is necessary to select one of the multiple feed vaporization systems for detection, the gas in the feed vaporization system is diverted to the detection outlet through the flow control valve and detected by the gas chromatograph 15; the gas in other feed vaporization systems is diverted to the circulation outlet for unloading, and the material in the vaporizer 4 is always in a flowing state, and is all fresh flowing material, which can ensure the freshness of the gas detected by the gas chromatograph 15, and the detection result corresponds to the real-time nature of the material in use.

[0049] The sampling pipe 14 is provided with an electric heating device to ensure the temperature in the sampling pipe 14 and keep the material in the sampling pipe 14 in a gaseous state.

[0050] The chlorosilane storage container 6 is connected to the chlorosilane delivery pipeline 1 through a liquid return line 18; a manual regulating valve and a second check valve are provided on the liquid return line 18 to prevent cross-contamination.

[0051] The control device is connected to the pressure transmitter, temperature sensor, pressure relief regulating valve, sampling control valve and flow control valve respectively, and is used to collect temperature and pressure signals and control the pressure relief regulating valve, sampling control valve and flow control valve.

[0052] An embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, which can improve detection efficiency and the accuracy of detection results and reduce the impact on the production process.

[0053] As a preference of the above embodiments, an embodiment of the present invention proposes an online chlorosilane vaporization detection system for a polysilicon production line, which also includes: a pressure relief system 19; the pressure relief system 19 is connected to the pressure relief pipeline 12 to receive the material output by the pressure relief pipeline 12 for further processing.

[0054] As a preferred embodiment of the above embodiment, a pressure relief line 2 13 is provided on the pressure relief line 1 12; the input end of the pressure relief line 2 13 is connected to the pressure relief line 1 12 and is located upstream of the pressure relief regulating valve; the output end of the pressure relief line 2 13 is connected to the pressure relief line 1 12 and is located between the pressure relief regulating valve and the check valve 1, and a pressure relief control valve is provided on the pressure relief line 2 13 for controlling the on and off of the pressure relief line 2 13, so that when sampling and testing are not required, the vaporizer 4 can be used normally and the pressure can be directly relieved through the pressure relief line 2 13.

[0055] An embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, which achieves precise control of the complete vaporization of chlorosilane, avoids raw material waste, is conducive to improving and stabilizing the quality of polysilicon products, and is conducive to realizing automated control.

[0056] An embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, which realizes automated control of sampling and sample preparation by a gas chromatograph 15, reduces contamination of the sample to be detected during manual operation, and improves the accuracy of the detection and processing results.

[0057] An embodiment of the present invention provides an online chlorosilane vaporization detection system for a polysilicon production line, which can enable an online gas chromatograph 15 to automatically detect component data of multiple raw material lines.

[0058] Further explanation, although the terms first, second, etc. can be used to describe various elements in this article, these terms should not limit these elements. These terms are only used to distinguish one element from another element. For example, the first element can be called the second element, and, similarly, the second element can be called the first element, and these terms are only used to distinguish one element from another element. This does not depart from the scope of exemplary embodiments. Similarly, element one and element two do not represent the order of elements, and these terms are only used to distinguish one element from another element. As used herein, the term "and / or" includes any combination and all combinations of one or more associated listed items.

[0059] In the description of the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "connected," and "fixed" should be understood in a broad sense. For example, they may refer to fixed connection, detachable connection, or integration; mechanical connection or electrical connection; direct connection or indirect connection through an intermediate medium; and internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention in specific circumstances.

[0060] The standard parts used in the present invention can all be purchased from the market, and special-shaped parts can be customized according to the description in the specification and the drawings. The specific connection methods of each part adopt conventional means such as mature bolts, rivets, welding, etc. in the existing technology. The machinery, parts and equipment all adopt conventional models in the existing technology, and the circuit connection adopts the conventional connection method in the existing technology, which will not be described in detail here.

[0061] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Any simple modifications, equivalent changes and modifications made to the above embodiment based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A chlorosilane online vaporization detection system for a polysilicon production line, characterized in that: Includes: feed vaporization system, chlorosilane storage container, sample preparation box, gas chromatograph and control device; The feed vaporization system includes: a chlorosilane delivery pipeline, a vaporizer, a first flow limiting throttling orifice plate and a second flow limiting throttling orifice plate; The chlorosilane delivery pipeline is provided with a control valve 1; A second control valve is provided on the chlorosilane delivery pipeline; The chlorosilane delivery pipeline is provided with an on-site pressure gauge; The fluid inlet of the vaporizer is connected to the chlorosilane delivery pipeline; the vaporizer is provided with a heat exchange medium inlet and a heat exchange medium outlet; The flow limiting orifice plate 1 is arranged on the chlorosilane delivery pipeline, between the control valve 1 and the control valve 2; The second flow limiting orifice plate is arranged at the fluid inlet of the vaporizer; A pressure relief pipeline 1 is provided on the fluid outlet of the vaporizer; a pressure relief regulating valve is provided on the pressure relief pipeline 1; and a check valve 1 is provided on the pressure relief pipeline 1; The vaporizer is provided with a temperature sensor and a pressure transmitter; A sampling pipe is provided on the fluid outlet of the vaporizer; There are multiple feed vaporization systems; The sample preparation box is provided with a plurality of fluid inlets; the plurality of fluid inlets are respectively connected to the sampling pipes of the plurality of feed vaporization systems; The sampling pipeline is provided with a sampling control valve; The sample preparation box is provided with a detection outlet; The feed port of the gas chromatograph is connected to the detection outlet; a post-detection loop is provided on the discharge port of the gas chromatograph; the post-detection loop is connected to the pressure relief pipe; The sample preparation box is provided with a circulation outlet; the circulation outlet is communicated with the fluid inlet; a circulation pipeline is provided on the circulation outlet; the circulation pipeline is communicated with the pressure relief pipeline; A flow direction control valve is provided between the fluid inlet, the detection outlet and the circulation outlet, for controlling the fluid inlet to be connected to the detection outlet or to be connected to the circulation outlet; The sampling pipe is provided with an electric heating device; The chlorosilane storage container is connected to the chlorosilane delivery pipeline through a liquid return line; the liquid return line is provided with a manual regulating valve and a second check valve; The control device is connected to the pressure transmitter, the temperature sensor, the pressure relief regulating valve, the sampling control valve and the flow control valve respectively, and is used to collect temperature and pressure signals and control the pressure relief regulating valve, the sampling control valve and the flow control valve.

2. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 1, characterized in that: The aperture of the second flow limiting and throttling orifice plate is smaller than the aperture of the first flow limiting and throttling orifice plate.

3. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 2, characterized in that: The aperture of the current limiting orifice plate 1 is 0.4-0.6 mm; The aperture of the second flow limiting and throttling orifice plate is 0.1-0.3 mm.

4. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 1, characterized in that: The medium temperature used in the vaporizer is 80-150°C.

5. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 4, characterized in that: The heat exchange medium of the evaporator is steam or water.

6. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 1, characterized in that: The pressure in the vaporizer is maintained at 0.1-0.3 MPa.

7. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 1, characterized in that: Also includes: Pressure relief system; The pressure relief system is in communication with the pressure relief pipeline.

8. The chlorosilane online vaporization detection system for a polysilicon production line according to claim 1, characterized in that: A pressure relief line 2 is provided on the pressure relief line 1; the input end of the pressure relief line 2 is connected to the pressure relief line 1 and is located upstream of the pressure relief regulating valve; the output end of the pressure relief line 2 is connected to the pressure relief line 1 and is located between the pressure relief regulating valve and the check valve 1.

Citation Information

Patent Citations

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