Trace phosphorane detection device for disilane synthesis and purification process

Abstract

The utility model relates to the technical field of trace phosphine analysis, in particular to a trace phosphine detection device for a disilane synthesis and purification process, which comprises a six-way valve, a first interface, a second interface, a third interface, a fourth interface, a fifth interface and a sixth interface are annularly and sequentially arranged on the six-way valve at equal intervals, the second interface is a carrier gas inlet, and the third interface is a carrier gas outlet. The fifth interface is a sample inlet, and the sixth interface is an emptying hole; the two ends of the first air pipe are communicated with the first connector and the fourth connector respectively, and a quantitative pipe is arranged on the first air pipe; one end of the second gas pipe is communicated with the third interface, the second organ is provided with a chromatographic column and a DID helium ionization detector, and the chromatographic column is arranged between the third interface and the DID helium ionization detector. When trace phosphorane is analyzed, impurity concentration changes can be rapidly detected, a balanced (stable state) analysis value can be rapidly measured, and the method has the advantages of being accurate in quantification, low in detection limit and short in analysis period.

Description

Technical Field

[0001] This utility model relates to the field of trace phosphine analysis technology, specifically to a trace phosphine detection device 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. At its own vapor pressure, diethylsilane is a colorless, transparent liquid. It possesses chemical properties similar to silane, but its reactivity is stronger, and it can spontaneously combust in air. It is mainly used in solar cells, photosensitive rollers, amorphous silicon films, epitaxial growth, oxide films, nitride films, and chemical vapor deposition. Phosphine is produced during the preparation of diethylsilane.

[0003] Phosphine is a highly toxic gas that strongly irritates the respiratory system, causing symptoms such as coughing and difficulty breathing upon inhalation. It also damages the cardiovascular system, affecting heart function and leading to arrhythmias. Furthermore, phosphine is flammable and can form explosive mixtures with air, easily igniting and exploding, causing fires and other serious accidents, resulting in casualties and property damage. Current methods for detecting trace amounts of phosphine suffer from slow detection speed and low accuracy. Utility Model Content

[0004] The purpose of this invention is to provide a device for detecting trace amounts of phosphine in the synthesis and purification process of silane, so as to overcome the above-mentioned shortcomings in the prior art.

[0005] To achieve the above objectives, this utility model provides the following technical solution:

[0006] A trace phosphine detection device for the synthesis and purification process of silane includes a six-way valve with a first, second, third, fourth, fifth, and sixth interface arranged circumferentially and at equal intervals. The second interface is a carrier gas inlet, the fifth interface is a sample inlet, and the sixth interface is a vent. A first gas tube is connected at both ends to the first and fourth interfaces, respectively, and a quantitative tube is installed on the first gas tube. A second gas tube is connected at one end to the third interface, and a chromatographic column and a DID helium ionization detector are installed on the second gas tube, with the chromatographic column positioned between the third interface and the DID helium ionization detector.

[0007] Furthermore, both the first and second tracheas are made of 316L stainless steel.

[0008] Furthermore, each valve in the six-way valve is a passivated purge type valve.

[0009] Furthermore, the valve plane of the six-way valve remains in high-purity helium gas.

[0010] Furthermore, the volume of the metering tube is 0.1 ml.

[0011] Furthermore, the chromatographic column is 50 meters long and has an inner diameter of 1 / 16 inch.

[0012] Furthermore, the chromatographic column is a PLOT-Q column.

[0013] Furthermore, the chromatographic column is equipped with a capillary column with an inner diameter of 0.25 mm and a stationary phase thickness of 0.25 μm.

[0014] The beneficial effects of the trace phosphine detection device in the silane synthesis and purification process provided by this utility model, as described above, are as follows:

[0015] The detection device of this application can quickly detect changes in impurity concentration when analyzing trace amounts of phosphine, and can rapidly measure the equilibrium (steady-state) analytical value. It also has the advantages of accurate quantification, low detection limit and short analysis cycle.

[0016] It should be understood that the foregoing general description and the following detailed description are exemplary and illustrative only, and are not intended to limit this disclosure.

[0017] This application provides an overview of various implementations or examples of the technology described in this disclosure, and is not a full disclosure of the entire scope or all features of the disclosed technology. Attached Figure Description

[0018] 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.

[0019] Figure 1 This is a schematic diagram of the S1 structure provided in an embodiment of the present utility model;

[0020] Figure 2 This is a schematic diagram of the S2 structure provided for an embodiment of the present utility model.

[0021] Explanation of reference numerals in the attached figures:

[0022] 100. Six-way valve; 101. First port; 102. Second port; 103. Third port; 104. Fourth port; 105. Fifth port; 106. Sixth port;

[0023] 201. Quantitative tube;

[0024] 301. Chromatographic column;

[0025] 401. DID helium ionization detector;

[0026] 501. First trachea;

[0027] 502. Second trachea. Detailed Implementation

[0028] To make the objectives, technical solutions, and advantages of the embodiments of this disclosure clearer, the technical solutions of the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this disclosure. All other embodiments obtained by those skilled in the art based on the described embodiments of this disclosure without creative effort are within the scope of protection of this disclosure.

[0029] Please see Figure 1-2 A trace phosphine detection device for the synthesis and purification process of silane includes a six-way valve 100. The six-way valve 100 has a first port 101, a second port 102, a third port 103, a fourth port 104, a fifth port 105, and a sixth port 106 arranged circumferentially and at equal intervals. The second port 102 is a carrier gas inlet, the fifth port 105 is a sample inlet, and the sixth port 106 is a vent. A first gas pipe 501 is connected at both ends to the first port 101 and the fourth port 104, respectively, and a quantitative tube 201 is installed on the first gas pipe 501. A second gas pipe 502 is connected at one end to the third port 103, and a chromatographic column 301 and a DID helium ionization detector 401 are installed on the second gas pipe, with the chromatographic column 301 positioned between the third port 103 and the DID helium ionization detector 401. The sixth port 106 is connected to an external gas storage device to collect waste gas during the detection process.

[0030] Furthermore, both the first air pipe 501 and the second air pipe 502 are made of 316L stainless steel to improve weldability and resistance to intergranular corrosion. The 316L stainless steel is also treated with an electrolytic polishing process to enhance the smoothness of the surfaces of the first air pipe 501 and the second air pipe 502.

[0031] Furthermore, each valve in the six-way valve 100 is a passivated purge type valve.

[0032] Furthermore, the valve plane of the six-way valve 100 is kept in high-purity helium gas. The valve plane is a key structural component of the six-way valve 100; it is the planar area where the various channels (typically corresponding to the six ports) converge. A continuous flow of high-purity helium gas surrounds the valve plane in the operating environment of the six-way valve 100 to prevent oxygen, moisture, and other impurities from the outside air from contacting the valve plane, thereby improving valve performance and the accuracy of analytical results.

[0033] Furthermore, the volume of the metering tube 201 is 0.1 ml.

[0034] Furthermore, the chromatographic column 301 is 50 meters long and has an inner diameter of 1 / 16 inch.

[0035] Furthermore, the chromatographic column 301 is a PLOT-Q column. The PLOT-Q column is a bonded polystyrene-divinylbenzene chromatographic column 301, which can effectively separate C1 to C3 isomers and alkanes up to C12, and can also separate ethane, ethylene, and acetylene.

[0036] Furthermore, the chromatographic column 301 is equipped with a capillary column with an inner diameter of 0.25 mm and a stationary phase thickness of 0.25 μm.

[0037] Operating steps:

[0038] S1: Switch the valve to connect the second port 102 and the third port 103, the fourth port 104 and the fifth port 105, and the sixth port 106 and the first port 101 (as shown in the attached diagram). Figure 1 As shown), high-purity silane is introduced through the fifth port 105. The high-purity silane replaces the metering tube 201 through the first gas tube 501 at a flow rate of 0.1 MPa and 300 mL / min and is maintained for 1 min.

[0039] S2: Switch the valves to connect the first port 101 and the second port 102; connect the third port 103 and the fourth port 104; connect the fifth port 105 and the sixth port 106 (as shown in the attached diagram). Figure 2 (As shown); Carrier gas is introduced through the second port 102. The carrier gas, through the first gas tube 501, sends the high-purity silane in the quantitative tube 201 into the chromatographic column 301 on the second gas tube 502 via the third port 103 on the six-way valve 100 for separation, so that impurities such as phosphine can enter the DID helium ionization detector 401 of the chromatograph for quantitative analysis. The relevant parameters are set as follows: carrier gas pressure 0.6 MPa, driving gas pressure 0.5 MPa, carrier gas flow rate 30 mL / min; column temperature of chromatographic column 301 80℃, and temperature of DID helium ionization detector 401 120℃.

[0040] 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 device for detecting trace phosphine in an ethylsilane synthesis and purification process, comprising a six-way valve (100), wherein a first port (101), a second port (102), a third port (103), a fourth port (104), a fifth port (105) and a sixth port (106) are arranged equidistantly in a ring on the six-way valve (100), characterized in that: The second interface (102) is a carrier gas inlet, the fifth interface (105) is a sample inlet, and the sixth interface (106) is a vent hole; A first gas pipe (501) is in communication with the first interface (101) and the fourth interface (104) at two ends, and a quantitative tube (201) is arranged on the first gas pipe (501); A second gas pipe (502) is in communication with the third interface (103) at one end, and a chromatographic column (301) and a DID helium ionization detector (401) are arranged on the second gas pipe, and the chromatographic column (301) is arranged between the third interface (103) and the DID helium ionization detector (401).

2. The apparatus according to claim 1, wherein the apparatus is used for detecting trace phosphine in a process for synthesizing and purifying di-silane, characterized in that, The first gas pipe (501) and the second gas pipe (502) are made of 316L stainless steel.

3. The apparatus of claim 1, wherein the apparatus is used for detecting trace phosphine in a process for synthesizing and purifying di-silane, and the apparatus is characterized in that, Each valve of the six-way valve (100) is a passivation purging type valve.

4. The apparatus of claim 3, wherein the apparatus is used in a process for the synthesis and purification of disilane. The valve plane of the six-way valve (100) is kept in high-purity helium.

5. The apparatus of claim 1, wherein the apparatus is used in a process for the synthesis and purification of disilane. The volume of the quantitative tube (201) is 0.1 milliliter.

6. The apparatus of claim 1, wherein the apparatus is used in a process for the synthesis and purification of disilane. The length of the chromatographic column (301) is 50 meters, and the inner diameter is 1 / 16 inch.

7. A trace phosphine detection device for an ethylsilane synthesis purification process according to claim 6, wherein, The chromatographic column (301) is a PLOT-Q column.

8. The apparatus of claim 6, wherein the apparatus is used in a process for the synthesis and purification of di-silane. A capillary column is arranged in the chromatographic column (301), the inner diameter of the capillary column is 0.25 millimeter, and the thickness of the stationary phase of the capillary column is 0.25 micrometer.

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