A trace ammonia analysis system for ethylsilane synthesis and purification process

Abstract

This utility model discloses a trace ammonia analysis system for the synthesis and purification process of silane, relating to the field of trace ammonia analysis technology. The system includes: a valve with a first, second, third, fourth, fifth, and sixth interface; the second interface is a carrier gas inlet, the fifth interface is a sample gas inlet, and the sixth interface is a vent hole; a quantitative tube, one end of which is fixedly connected to the first interface and the other end to the fourth interface; and a chromatographic column, one end of which is fixedly connected to the third interface and the other end of which is fixedly connected to an MS quadrupole mass detector. The trace ammonia analysis system for the synthesis and purification process of silane provided by this utility model, using MS for the analysis of trace impurities, has the advantages of high sensitivity, a universal detector for all components, and the ability to vent analytical errors caused by the additional equipment of silane through backflushing technology in the gas path design, resulting in accurate quantification and effectively reducing analysis time.

Description

Technical Field

[0001] This utility model relates to the field of trace ammonia analysis technology, specifically a trace ammonia analysis system for the synthesis and purification process of silane. Background Technology

[0002] Diethylsilane is an inorganic compound with the chemical formula Si₂H₆. At room temperature and pressure, it is a colorless, transparent, toxic gas with an unpleasant, pungent odor. It possesses similar chemical properties to silane, but its reactivity is stronger. It is mainly used in the manufacture of amorphous silicon films, epitaxial growth, oxide films, nitride films, and chemical vapor deposition. Diethylsilane is a flammable liquid at room temperature and pressure. It has similar chemical properties to silane, but its reactivity is stronger; it can spontaneously combust in air. The main applications of diethylsilane are in the manufacture of semiconductor silicon films and amorphous silicon.

[0003] For example, publication number CN221960024U, publication date November 5, 2024, titled "Ammonia Concentration Detection System," describes a system comprising a sampling module, a detection cell, a temperature control component, a heating component, a temperature monitoring component, a detection module, and a control module. The sampling module is installed on the device under test. The gas input end of the detection cell is connected to the output end of the sampling module via a pipe. The temperature control component is located on the pipe connecting the sampling module and the detection cell. The heating component is located on the outer wall of the detection cell to change the temperature inside the cell. The temperature monitoring component is also located on the outer wall of the detection cell to monitor the temperature inside the cell and upload the temperature data to the control module. The detection module is connected to the detection cell to detect the ammonia concentration within it. The control module is connected to the sampling module, heating component, temperature monitoring component, and detection module. This system can improve the accuracy of ammonia concentration detection.

[0004] In existing technologies, such as those containing the aforementioned patents, it is currently impossible to accurately and quickly detect and analyze ammonia in trace amounts in silane. When ammonia is detected, the analysis results may still have certain errors, and accurate quantification is not possible. Furthermore, the detection and analysis also require a certain amount of time. Utility Model Content

[0005] The purpose of this invention is to provide a trace ammonia analysis system for the synthesis and purification process of silane, so as to overcome the shortcomings of the prior art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a trace ammonia analysis system for the synthesis and purification process of silane, comprising:

[0007] The valve has a first interface, a second interface, a third interface, a fourth interface, a fifth interface, and a sixth interface.

[0008] The second interface is the carrier gas inlet, the fifth interface is the sample gas inlet, and the sixth interface is the vent hole;

[0009] A quantitative tube, one end of which is fixedly connected to the first interface and the other end of which is fixedly connected to the fourth interface;

[0010] The chromatographic column is fixedly connected to the third interface at one end and to an MS quadrupole mass detector at the other end.

[0011] Furthermore, the chromatographic column is a PLOT-Q column.

[0012] Furthermore, the volume of the metering tube is 0.1 mL.

[0013] Furthermore, the chromatographic column is 100m long and has an inner diameter of one-sixteenth of an inch.

[0014] Furthermore, a 0.25 mm × 0.53 μm capillary column is installed inside the chromatographic column.

[0015] Furthermore, the average detection limit of the MS quadrupole mass detector is 0.1 x 10^-6 (ppm).

[0016] Compared with existing technologies, the trace ammonia analysis system for the synthesis and purification process of silane provided by this utility model has the advantages of high sensitivity, universal detectors for all components, and the ability to vent silane through backflushing technology in the gas path design to reduce analytical errors, thus accurately quantifying the trace impurities and effectively reducing the analysis time. Attached Figure Description

[0017] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings.

[0018] Figure 1 This is a schematic diagram of the air intake state provided for an embodiment of the present utility model;

[0019] Figure 2 This is a schematic diagram of the detection state provided for an embodiment of the present utility model.

[0020] Explanation of reference numerals in the attached diagram: 1. Valve; 11. First port; 12. Second port; 13. Third port; 14. Fourth port; 15. Fifth port; 16. Sixth port; 2. Quantitative tube; 3. Chromatographic column; 4. MS quadrupole mass detector. Detailed Implementation

[0021] To enable those skilled in the art to better understand the technical solution of this utility model, the present utility model will be further described in detail below with reference to the accompanying drawings.

[0022] Please see Figure 1-2 The present invention provides a trace ammonia analysis system for the synthesis and purification process of silane, comprising: a valve 1 having a first interface 11, a second interface 12, a third interface 13, a fourth interface 14, a fifth interface 15 and a sixth interface 16.

[0023] Specifically, the second interface 12 is a carrier gas inlet, the fifth interface 15 is a sample gas inlet, and the sixth interface 16 is a vent hole;

[0024] Understandable: Valve 1 has both an intake state and a detection state.

[0025] In the intake state: the first port 11 is connected to the sixth port 16; the second port 12 is connected to the third port 13; and the fourth port 14 is connected to the fifth port 15.

[0026] In the detection state: the first interface 11 is connected to the second interface 12; the third interface 13 is connected to the fourth interface 14; and the fifth interface 15 is connected to the sixth interface 16.

[0027] The quantitative tube 2 has one end fixedly connected to the first interface 11 and the other end fixedly connected to the fourth interface 14; wherein, the volume of the quantitative tube 2 is 0.1 mL.

[0028] The chromatographic column 3 is fixedly connected at one end to the third interface 13, and at the other end is fixedly connected to the MS quadrupole mass detector 4.

[0029] Specifically, column 3 is a PLOT-Q column; column 3 is 100m long and has an inner diameter of one-sixteenth of an inch; a 0.25mm*0.53μm capillary column is installed inside column 3.

[0030] Specifically, the average detection limit of the MS quadrupole mass detector 4 is 0.1 x 10^-6 (ppm).

[0031] Preferably, all pipelines in contact with the sample gas are made of 316L EP stainless steel.

[0032] Preferably, all valves in contact with the sample gas are passivated purge type valves.

[0033] Preferably, the valve face is constantly protected by high-purity helium gas.

[0034] In the intake state: the sample gas is introduced through the fifth port 15. Since the fifth port 15 is connected to the fourth port 14 at this time, the sample gas will pass through the fourth port 14, the metering tube 2, the first port 11 in sequence, and come out from the sixth port 16. At this time, the metering tube 2 stores a certain amount of sample gas.

[0035] In this process, high-purity silane was used to replace quantitative tube 2 at a flow rate of 0.1 MPa and 300 mL / min for 1 min.

[0036] Subsequently, the state of valve 1 is changed, that is, its connection state is changed to the detection state. At this time, carrier gas is introduced into the second port 12. The carrier gas passes through the first port 11, the quantitative tube 2, the fourth port 14, the third port 13, the chromatographic column 3, and the MS quadrupole mass detector 4 in sequence for detection.

[0037] During the detection process, the carrier gas pressure was 0.55 MPa, the driving gas pressure was 0.5 MPa, the carrier gas flow rate was 20 mL / min, the column temperature was 120 ℃, and the detector temperature was 150 ℃.

[0038] The foregoing description only illustrates certain exemplary embodiments of the present invention. Undoubtedly, those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A trace ammonia analysis system for the synthesis and purification process of silane, characterized in that, include: The valve (1) has a first interface (11), a second interface (12), a third interface (13), a fourth interface (14), a fifth interface (15) and a sixth interface (16). The second interface (12) is the carrier gas inlet, the fifth interface (15) is the sample gas inlet, and the sixth interface (16) is the vent hole; A quantitative tube (2) has one end fixedly connected to the first interface (11) and the other end fixedly connected to the fourth interface (14); The chromatographic column (3) is fixedly connected at one end to the third interface (13) and at the other end to the MS quadrupole mass detector (4).

2. The trace ammonia analysis system for the synthesis and purification process of silane according to claim 1, characterized in that, The chromatographic column (3) is a PLOT-Q column.

3. The trace ammonia analysis system for the synthesis and purification process of silane according to claim 1, characterized in that, The volume of the metering tube (2) is 0.1 mL.

4. The trace ammonia analysis system for the synthesis and purification process of silane according to claim 1, characterized in that, The chromatographic column (3) is 100m long and has an inner diameter of one-sixteenth of an inch.

5. The trace ammonia analysis system for the synthesis and purification process of silane according to claim 1, characterized in that, The chromatographic column (3) is fitted with a 0.25mm×0.53μm capillary column.

6. The trace ammonia analysis system for the synthesis and purification process of silane according to claim 1, characterized in that, The average detection limit of the MS quadrupole mass detector (4) is 0.1 × 10 to the power of negative six (ppm).

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