Electronic-grade silane analysis system and method

Abstract

The invention provides an electronic-grade silane analysis system and method, belongs to the technical field of silane analysis, and aims to solve the problem of few impurity types in existing silane analysis and detection. The electronic-grade silane analysis system comprises a first valve, a second valve, a third valve, a fourth valve, a fifth valve and a sixth valve; the first valve is connected with the second valve through the first pre-analysis column, and the second valve is connected with the fourth valve through the first analysis column; the first valve is connected with a third valve through a second pre-analysis column, and the third valve is connected with a fourth valve through a second analysis column; the first valve is connected with a fifth valve through a gas pipeline, and the fifth valve is communicated with a sixth valve through a third analysis column and a fourth analysis column which are arranged in parallel; wherein the fourth valve is connected with the first DID detector, and the sixth valve is connected with the second DID detector; the first valve and the fifth valve are ten-way valves, and the other valves are four-way valves. The system can detect various impurities.

Description

Technical Field

[0001] This invention relates to the field of silane analysis technology, and specifically to an electronic-grade silane analysis system and method. Background Technology

[0002] With the development of semiconductors, the purity requirements for electronic specialty gases silane (SiH4) 6N-7N are becoming increasingly stringent. However, existing silane gas detection systems and methods can only detect a limited number of impurities, which is insufficient to meet the high purity requirements.

[0003] Therefore, there is an urgent need for a silane gas analysis system and method that can detect more impurities to safeguard gas purity. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a silane gas analysis system and method that can detect more impurities.

[0005] To solve the above-mentioned technical problems, the technical solution of the present invention is as follows: This invention provides an electronic-grade silane analysis system, comprising: a first valve, a second valve, a third valve, a fourth valve, a fifth valve, and a sixth valve; The first valve is connected to the second valve via a first pre-analysis column, and the second valve is connected to the fourth valve via a first analysis column; The first valve is connected to the third valve via the second pre-analysis column, and the third valve is connected to the fourth valve via the second analysis column; The first valve is connected to the fifth valve via a gas pipeline, and the fifth valve is connected to the sixth valve via a third and a fourth analytical column arranged in parallel. The fourth valve is connected to the first DID detector, and the sixth valve is connected to the second DID detector; the second valve is provided with a first vent pipe, the third valve is provided with a second vent pipe, the fourth valve is provided with a third vent pipe, and the sixth valve is provided with a fourth vent pipe. The first valve and the fifth valve are ten-way valves, and the second valve, the third valve, the fourth valve and the sixth valve are four-way valves.

[0006] Optionally, the first valve and the fifth valve are provided with ten ports in a clockwise direction, and the second valve, the third valve, the fourth valve and the sixth valve are provided with four ports in a clockwise direction. The inlet of the first pre-analysis column is connected to the second interface of the first valve, and the outlet of the first pre-analysis column is connected to the fourth interface of the second valve; the inlet of the first analysis column is connected to the first interface of the second valve, and the outlet of the first analysis column is connected to the second interface of the fourth valve. The inlet of the second pre-analysis column is connected to the sixth interface of the first valve, and the outlet of the second pre-analysis column is connected to the fourth interface of the third valve; the inlet of the second analysis column is connected to the first interface of the third valve, and the outlet of the second analysis column is connected to the fourth interface of the fourth valve. The inlet of the gas pipeline is connected to the fourth port of the first valve, and the outlet of the gas pipeline is connected to the ninth port of the fifth valve; the inlet of the third analytical column is connected to the second port of the fifth valve, and the outlet of the third analytical column is connected to the fourth port of the sixth valve; the inlet of the fourth analytical column is connected to the sixth port of the fifth valve, and the outlet of the fourth analytical column is connected to the second port of the sixth valve. The first DID detector is connected to the third interface of the fourth valve, and the second DID detector is connected to the first interface of the sixth valve; The first vent pipe is connected to the third port of the second valve; the second vent pipe is connected to the third port of the third valve; the third vent pipe is connected to the first port of the fourth valve; and the fourth vent pipe is connected to the third port of the sixth valve.

[0007] Optionally, the first valve may also include: The sample inlet line is connected to the 9th port of the first valve; The first carrier gas pipeline is connected to the first interface of the first valve; The second gas pipeline is connected to the 7th port of the first valve; The first quantitative pipeline is connected at both ends to the 10th and 3rd ports of the first valve, respectively; The second quantitative pipeline is connected at both ends to the 8th and 5th ports of the first valve, respectively.

[0008] Optionally, the second valve may also include: The third gas pipeline is connected to the second interface of the second valve.

[0009] Optionally, the third valve may also include: The fourth carrier gas line is connected to the second interface of the third valve.

[0010] Optionally, the fifth valve may also include: The fifth gas carrier line is connected to the first interface of the fifth valve; The sixth gas pipeline connects to the seventh port of the fifth valve; The third quantitative pipeline is connected at both ends to the 10th and 3rd ports of the fifth valve, respectively; The fourth quantitative pipeline is connected at both ends to the 8th and 5th ports of the fifth valve, respectively; The sample discharge pipeline is connected to the fourth port of the fifth valve.

[0011] Optionally, the first pre-analytical column (7) has a length of 8 feet, an outer diameter of 1 / 8 foot, and is packed with Hayesep Q, silanized; The first analytical column (8) has a length of 8 feet, an outer diameter of 1 / 8 foot, and is packed with 13X MS. The second pre-analytical column (9) is 12 feet long and has an outer diameter of 1 / 16 feet. The packing material is Hayesep Q. The second analytical column (10) is 10 feet long and has an outer diameter of 1 / 16 feet. The packing material is Hayesep Q. The third analytical column (12) is a 50m capillary column with an inner diameter of 0.53mm, a film thickness of 10um, and PoraBOND Q packing material. The fourth analytical column (13) is a 60m capillary column with an inner diameter of 0.53mm, a film thickness of 1.5um, and RTX-1 packing material.

[0012] Optionally, the first valve, second valve, third valve, fourth valve, fifth valve, and sixth valve are VICI. ® Brand name.

[0013] This invention also provides an electronic-grade silane analysis method, employing the aforementioned electronic-grade silane analysis system, comprising: The first valve injects the sample into the first pre-analysis column, where it undergoes pre-separation. The initial state of the second valve connects the first pre-analysis column to the first analysis column. By switching the state of the second valve, silane and CO2, which are at the end of the column, are vented through the first vent line, while H2, O2 / Ar, N2, CH4, and CO, which are at the beginning of the column, enter the first analysis column for further separation before entering the first DID detector to detect the content of H2, O2 / Ar, N2, CH4, and CO. The first valve injects the sample into the second pre-analysis column, where it undergoes pre-separation. The initial state of the third valve connects the second pre-analysis column to the second analysis column. By switching the state of the third valve, the silane in the middle is vented through the second vent line, while the CO2 in front and the C2H6 in the back enter the second analysis column for further separation before entering the first DID detector to detect the content of CO2 and C2H6. The first valve introduces the sample to the fifth valve via a gas pipeline. Switching the fifth valve allows the sample to enter the third analytical column. Switching the sixth valve vents the silane at the front of the column through the fourth vent line, while the silane at the back (Si₂H₆, C₃H₈, C₄H₆) is vented. 10 Si2H6, C3H8, and C4H are detected by the second DID detector via the sixth valve. 10 The content; The first valve introduces the sample into the fifth valve through the gas pipeline. Switching the state of the fifth valve allows the sample to enter the fourth analytical column. By switching the state of the sixth valve, the silane in front is vented through the fourth vent line, and the SiH2Cl2, SiHCl3, and SiCl4 in the back enter the second DID detector through the sixth valve to detect the content of SiH2Cl2, SiHCl3, and SiCl4.

[0014] Optionally, the injection volume of the first quantitative tube (21) and the second quantitative tube (22) is 0.5 ml, and the injection volume of the third quantitative tube (27) and the fourth quantitative tube (28) is 0.1 ml.

[0015] The above-described solution of the present invention has at least the following beneficial effects: In the above-described scheme of the present invention, each valve cooperates with each chromatographic column to achieve separation techniques such as back-cut (by switching the second valve to vent the silanes (SiH4) and CO2 that are listed later), center-cut (by switching the third valve to vent the silanes listed in the middle), and front-cut (by switching the sixth valve to vent the silanes listed earlier) by timely switching of valve states. Simultaneously, a DID detector is used to detect multiple impurities. Specifically, H2, O2 / Ar, N2, CH4, and CO are detected through the first pre-analysis column, the second valve, the first analytical column, and the fourth valve; CO2 and C2H6 are detected through the second pre-analysis column, the third valve, the second analytical column, and the fourth valve; and Si2H6, C3H8, and C4H6 are detected through the fifth valve, the third analytical column, and the sixth valve. 10 The detection of SiH2Cl2, SiHCl3, and SiCl4 is achieved through the fifth valve, the fourth analytical column, and the sixth valve, enabling the analysis of multiple trace impurities in electronic-grade silane gas and providing data support for the gases required by semiconductors. Attached Figure Description

[0016] Figure 1 This is a schematic diagram of the electronic-grade silane analysis system of the present invention; Figure 2 These are the spectra of SiH2Cl2, SiHCl3, and SiCl4 detected in embodiments of the present invention; Figure 3These are the spectra of H2, O2 / Ar, N2, CH4, CO, and CO2 detected in embodiments of the present invention; Figure 4 The C3H8, C2H6, and C4H detected in this embodiment of the invention. 10 Spectrum; Figure 5 This is the spectrum of Si2H6 detected in an embodiment of the present invention.

[0017] Figure label: 1-First valve; 2-Second valve; 3-Third valve; 4-Fourth valve; 5-Fifth valve; 6-Sixth valve; 7-First pre-analysis column; 8-First analytical column; 9-Second pre-analysis column; 10-Second analytical column; 11-Gas line; 12-Third analytical column; 13-Fourth analytical column; 14-First vent line; 15-Second vent line; 16-Third vent line; 17-Fourth vent line; 18-Sample injection line; 19-First carrier gas line; 20-Second carrier gas line; 21-First quantitative line; 22-Second quantitative line; 23-Third carrier gas line; 24-Fourth carrier gas line; 25-Fifth carrier gas line; 26-Sixth carrier gas line; 27-Third quantitative line; 28-Fourth quantitative line; 29-Sample discharge line. Detailed Implementation

[0018] Exemplary embodiments of the invention will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

[0019] like Figure 1 As shown, an embodiment of the present invention proposes an electronic-grade silane analysis system, comprising: a first valve 1, a second valve 2, a third valve 3, a fourth valve 4, a fifth valve 5, and a sixth valve 6; The first valve 1 is connected to the second valve 2 via the first pre-analysis column 7, and the second valve 2 is connected to the fourth valve 4 via the first analysis column 8; The first valve 1 is connected to the third valve 3 via the second pre-analysis column 9, and the third valve 3 is connected to the fourth valve 4 via the second analysis column 10; The first valve 1 is connected to the fifth valve 5 through a gas pipeline 11, and the fifth valve 5 is connected to the sixth valve 6 through the third analytical column 12 and the fourth analytical column 13 arranged in parallel. The fourth valve 4 is connected to the first DID detector, and the sixth valve 6 is connected to the second DID detector; the second valve 2 is provided with a first vent pipe 14, the third valve 3 is provided with a second vent pipe 15, the fourth valve 4 is provided with a third vent pipe 16, and the sixth valve 6 is provided with a fourth vent pipe 17. The first valve (1) and the fifth valve (5) are ten-way valves, and the second valve (2), the third valve (3), the fourth valve (4), and the sixth valve (6) are four-way valves.

[0020] For example, the first valve 1 and the fifth valve 5 are provided with ten interfaces in a clockwise direction, and the second valve 2, the third valve 3, the fourth valve 4 and the sixth valve 6 are provided with four interfaces in a clockwise direction. The inlet of the first pre-analysis column 7 is connected to the second interface of the first valve 1, and the outlet of the first pre-analysis column 7 is connected to the fourth interface of the second valve 2; the inlet of the first analysis column 8 is connected to the first interface of the second valve 2, and the outlet of the first analysis column 8 is connected to the second interface of the fourth valve 4. The inlet of the second pre-analysis column 9 is connected to the sixth interface of the first valve 1, and the outlet of the second pre-analysis column 9 is connected to the fourth interface of the third valve 3; the inlet of the second analysis column 10 is connected to the first interface of the third valve 3, and the outlet of the second analysis column 10 is connected to the fourth interface of the fourth valve 4. The inlet of the gas pipeline 11 is connected to the fourth interface of the first valve 1, and the outlet of the gas pipeline 11 is connected to the ninth interface of the fifth valve 5; the inlet of the third analysis column 12 is connected to the second interface of the fifth valve 5, and the outlet of the third analysis column 12 is connected to the fourth interface of the sixth valve 6; the inlet of the fourth analysis column 13 is connected to the sixth interface of the fifth valve 5, and the outlet of the fourth analysis column 13 is connected to the second interface of the sixth valve 6. The first DID detector is connected to the third interface of the fourth valve 4, and the second DID detector is connected to the first interface of the sixth valve 6; The first vent pipe 14 is connected to the third interface of the second valve 2; the second vent pipe 15 is connected to the third interface of the third valve 3; the third vent pipe 16 is connected to the first interface of the fourth valve 4; and the fourth vent pipe 17 is connected to the third interface of the sixth valve 6.

[0021] By switching valve states, specific adjacent interfaces on the valve can be connected, thereby achieving separation technology for front cutting, center cutting, and rear cutting.

[0022] For example, the first valve 1 further includes: The sample inlet line 18 is connected to the 9th port of the first valve 1 and is used to inject samples into the system. The first carrier gas line 19 is connected to the first interface of the first valve 1 and is used to provide carrier gas to the first pre-analysis column 7 and subsequent lines. The second carrier gas line 20 is connected to the 7th interface of the first valve 1 and is used to provide carrier gas to the second pre-analysis column 9 and subsequent lines. The first quantitative pipeline 21 is connected at both ends to the 10th and 3rd ports of the first valve 1, respectively, for introducing quantitative samples into the first pre-analysis column 7; The second quantitative pipeline 22 is connected at both ends to the 8th and 5th ports of the first valve 1, respectively, and is used to introduce quantitative samples into the second pre-analysis column 9.

[0023] For example, the second valve 2 also includes: The third carrier gas line 23 is connected to the second interface of the second valve 2 and is used to provide carrier gas for the second valve 2 to vent silane and CO2.

[0024] For example, the third valve 3 also includes: The fourth carrier gas line 24 is connected to the second interface of the third valve 3 and is used to provide carrier gas for the silane to be discharged from the third valve 3.

[0025] For example, the fifth valve 5 further includes: The fifth carrier gas line 25 is connected to the first interface of the fifth valve 5 and is used to supply carrier gas to the third analytical column 12 and subsequent lines. The sixth carrier gas line 26 is connected to the seventh interface of the fifth valve 5 and is used to supply carrier gas to the fourth analytical column 13 and subsequent lines. The third quantitative pipeline 27 is connected at both ends to the 10th and 3rd ports of the fifth valve 5, respectively, and is used to introduce quantitative samples into the third analytical column 12; The fourth quantitative tubing 28 is connected at both ends to the 8th and 5th ports of the fifth valve 5, respectively, for introducing quantitative samples into the fourth analytical column 13; The sample discharge line 29 is connected to the fourth interface of the fifth valve 5 and is used to discharge the sample when the fifth valve 5 is in the standby state.

[0026] For example, the first pre-analysis column 7 has a length of 8 feet, an outer diameter of 1 / 8 foot, and is packed with Hayesep Q silanized material. The first pre-analysis column 7 is used to separate H2, O2, Ar, N2, CH4, CO, silane, and CO2. Along the gas flow direction, H2, O2, Ar, N2, CH4, and CO are arranged in front of each other in the first pre-analysis column 7, while silane and CO2 are arranged behind them. Thus, silane and CO2 can be vented by switching the second valve 2, i.e., post-cut.

[0027] The first analytical column 8 has a length of 8 feet, an outer diameter of 1 / 8 foot, and is packed with 13X MS material; the first analytical column 8 is used for further separation of H2, O2, Ar, N2, CH4, and CO.

[0028] The second pre-analysis column 9 is 12 feet long and has an outer diameter of 1 / 16 feet. It is packed with Hayesep Q. The second pre-analysis column 9 is used to separate CO2, silane and C2H6. In the gas flow direction, CO2 is placed in front, silane is placed in the middle and C2H6 is placed at the back in the second pre-analysis column 9. The silane can be vented by switching the third valve 3, i.e., center cut.

[0029] The second analytical column 10 is 10 feet long and has an outer diameter of 1 / 16 feet. It is packed with Hayesep Q. The second analytical column 10 is used for further separation of CO2 and C2H6.

[0030] The third analytical column 12 is a 50m long capillary column with an inner diameter of 0.53mm and a film thickness of 10µm, packed with PoraBOND Q. The third analytical column 12 is used to separate silanes, Si2H6, C3H8, and C4H4. 10 Along the gas flow direction, in the third analytical column 12, silanes are listed first, followed by Si2H6, C3H8, and C4H6. 10 Following this, silane can be vented by switching the sixth valve 6, followed by Si2H6, C3H8, and C4H. 10 Enter the detector, i.e., cut ahead.

[0031] The fourth analytical column 13 is a 60m long capillary column with an inner diameter of 0.53mm and a film thickness of 1.5um, and is packed with RTX-1. The fourth analytical column 13 is used to separate silane, SiH2Cl2, SiHCl3, and SiCl4. Along the gas flow direction, silane is placed first in the fourth analytical column 13, followed by SiH2Cl2, SiHCl3, and SiCl4. Thus, by switching the sixth valve 6, the silane can be vented, and the following SiH2Cl2, SiHCl3, and SiCl4 can enter the detector, i.e., pre-cutting.

[0032] For example, the first valve 1, the second valve 2, the third valve 3, the fourth valve 4, the fifth valve 5, and the sixth valve 6 are VICI. ® The grade has a low leakage rate.

[0033] The silane analysis system of the present invention, when used in conjunction with a gas chromatograph, can detect trace impurities in electronic-grade silanes.

[0034] All pipelines in this invention are made of VICI SS 316L material.

[0035] Embodiments of the present invention also propose an electronic-grade silane analysis method, employing the aforementioned electronic-grade silane analysis system, comprising: The first valve 1 injects the sample into the first pre-analysis column 7, where it undergoes pre-separation. The initial state of the second valve 2 is to connect the first pre-analysis column 7 to the first analysis column 8. By switching the state of the second valve 2, the silane and CO2 that are downstream are vented through the first vent line 14, while the H2, O2, Ar, N2, CH4, and CO that are upstream enter the first analysis column 8 for further separation before entering the first DID detector to detect the content of H2, O2 / Ar, N2, CH4, and CO. The first valve 1 injects the sample into the second pre-analysis column 9, where it undergoes pre-separation. The initial state of the third valve 3 connects the second pre-analysis column 9 to the second analysis column 10. By switching the state of the third valve 3, the silane in the middle is vented through the second vent line 15, while the CO2 in front and the C2H6 in the back enter the second analysis column 10 for further separation before entering the first DID detector to detect the content of CO2 and C2H6. The first valve 1 introduces the sample into the fifth valve 5 through the gas pipeline 11. Switching the state of the fifth valve 5 allows the sample to enter the third analytical column 12. Switching the state of the sixth valve 6 vents the silane at the front through the fourth vent line 17, while the following silanes (Si2H6, C3H8, C4H6) are vented. 10 Si2H6, C3H8, and C4H are detected by the second DID detector via the sixth valve 6. 10 The content; The first valve 1 introduces the sample into the fifth valve 5 through the gas pipeline 11. Switching the state of the fifth valve 5 allows the sample to enter the fourth analytical column 13. By switching the state of the sixth valve 6, the silane in front is vented through the fourth vent pipeline 17, and the SiH2Cl2, SiHCl3, and SiCl4 in the back enter the second DID detector through the sixth valve 6 to detect the content of SiH2Cl2, SiHCl3, and SiCl4.

[0036] For example, the injection volume of the first quantitative tube 21 and the second quantitative tube 22 is 0.5 ml, and the injection volume of the third quantitative tube 27 and the fourth quantitative tube 28 is 0.1 ml. For example, the sample flow rate in the first quantitative line 21 and the second quantitative line 22 is 50-80 ml / min and the pressure is 15 psi.

[0037] Specifically, the electronic-grade silane analysis method of the present invention includes: When it is necessary to detect at least one impurity among H2, O2, Ar, N2, CH4, and CO, the state of the first valve 1 is adjusted so that the 9th and 10th ports of the first valve 1 are connected, and the 3rd and 2nd ports are connected. The sample is then injected into the first quantitative line 21 through the injection line 18. After quantification by the first quantitative line 21, the sample enters the first pre-analysis column 7, where it undergoes pre-separation. Along the gas flow direction, H2, O2, Ar, N2, CH4, and CO are listed first, followed by silane and CO2. The initial state of the second valve 2... Initially, the fourth port is connected to the first port. After H2, O2, Ar, N2, CH4, and CO enter the first analytical column 8 through the second valve 2, the state of the second valve 2 is switched to connect the fourth port to the third port, allowing the silane and CO2 that follow to be vented through the first vent line 14. The initial state of the fourth valve 4 is that the second port is connected to the third port. After H2, O2, Ar, N2, CH4, and CO are further separated in the first analytical column 8, they enter the first DID detector to detect the content of H2, O2, Ar, N2, CH4, and CO.

[0038] When it is necessary to detect at least one impurity among CO2 and C2H6, adjust the state of the first valve 1 so that the 9th port of the first valve 1 is connected to the 8th port, the 7th port to the 8th port, and the 5th port to the 6th port. The sample is then injected into the second quantitative line 22 through the injection line 18. After quantification by the second quantitative line 22, the sample enters the second pre-analysis column 9, where it undergoes pre-separation. Along the gas flow direction, CO2 is placed first, silane in the middle, and C2H6 last. The initial state of the third valve 3 is the 4th port. Connected to the first interface, after CO2 enters the second analytical column 10 through the third valve 3, the state of the third valve 3 is switched to connect the fourth interface with the third interface, allowing the silane in the middle to be vented through the second vent line 15. Then, the state of the third valve 3 is switched to connect the fourth interface with the first interface, allowing the C2H6 in the later stage to enter the second analytical column 10. The initial state of the fourth valve 4 is that the fourth interface is connected to the third interface. After CO2 and C2H6 are further separated in the second analytical column 10, they enter the first DID detector to detect the content of CO2 and C2H6.

[0039] It should be noted that when H2, O2, Ar, N2, CH4, and CO are detected in the first analytical column 8, the fourth port of the fourth valve 4 is connected to the first port, that is, the gas in the second analytical column 10 is vented; when CO2 and C2H6 are detected in the second analytical column 10, the second port of the fourth valve 4 is connected to the first port, that is, the gas in the first analytical column 8 is vented.

[0040] When it is necessary to detect Si2H6, C3H8, and C4H 10 When at least one impurity is present, the state of the first valve 1 is adjusted so that the 9th and 10th ports of the first valve 1 are connected, and the 3rd and 4th ports are connected. The sample is then injected into the first quantitative line 21 through the injection line 18. After quantification by the first quantitative line 21, the sample enters the gas line 11. The sample then enters the fifth valve 5 through the gas line 11. The initial state of the fifth valve 5 is such that the 9th and 10th ports are connected, and the 3rd and 2nd ports are connected. After quantification by the third quantitative line 27, the sample enters the third analytical column 12. In the third analytical column 12, along the gas flow direction, silanes are arranged first, followed by Si2H6, C3H8, and C4H6. 10 Following this, the initial state of the sixth valve 6 is that the fourth port is connected to the third port, venting silane through the fourth vent pipe 17. Then, the state of the sixth valve 6 is switched to connect the fourth port to the first port, allowing Si2H6, C3H8, and C4H to be released. 10 The content is then detected by the second DID detector.

[0041] When it is necessary to detect at least one impurity among SiH2Cl2, SiHCl3, and SiCl4, the state of the first valve 1 is adjusted so that the 9th and 10th ports of the first valve 1 are connected, and the 3rd and 4th ports are connected. The sample is injected into the first quantitative line 21 through the injection line 18. After quantification by the first quantitative line 21, the sample enters the gas line 11. The sample then enters the fifth valve 5 through the gas line 11. The initial state of the fifth valve 5 is such that the 9th and 8th ports are connected, the 8th and 7th ports are connected, and the 5th and 6th ports are connected. After quantification by the fourth quantitative line 28, the sample enters the fourth analytical column 13. In the fourth analytical column 13, along the gas flow direction, silane is placed first, followed by SiH2Cl2, SiHCl3, and SiCl4. The initial state of the sixth valve 6 is such that the 2nd and 3rd ports are connected, venting the silane through the fourth vent line 17. Then, the state of the sixth valve 6 is switched so that the 2nd port is connected to the 1st port, allowing Si2H6, C3H8, and C4H6 to be released. 10 The content is then detected by the second DID detector.

[0042] It should be noted that when detecting Si2H6, C3H8, and C4H in the third analytical column 12... 10When the gas in the fourth analytical column 13 is vented, the second and third ports of the sixth valve 6 are connected. When SiH2Cl2, SiHCl3, and SiCl4 in the fourth analytical column 13 are detected, the fourth and third ports of the sixth valve 6 are connected, that is, the gas in the fourth analytical column 13 is vented.

[0043] To further illustrate this invention, four bottles of standard gas were tested using the method described above. Since silane gas is very dangerous and it is inconvenient to use silane as a background gas for preparing the standard gas, helium was used instead of silane as the base gas to prepare four bottles of standard gas containing helium and specific impurities. The helium was vented during the pre-cutting, center-cutting, and post-cutting processes.

[0044] The first bottle of standard gas contained helium, SiH₂Cl₂, SiHCl₃, and SiCl₄. The test results are shown in Table 1 and... Figure 2 As shown.

[0045] The second bottle of standard gas contained helium, H2, O2 / Ar, N2, CH4, CO, and CO2. The test results are shown in Table 2 and... Figure 3 As shown.

[0046] The third bottle of standard gas contains helium, C3H8, and C4H. 10 C2H6, the test results are shown in Table 3 and Figure 4 As shown.

[0047] The fourth bottle of standard gas contained helium and Si2H6. The test results are shown in Table 4. Figure 5 As shown.

[0048] Table 1

[0049] Table 2

[0050] Table 3

[0051] Table 4

[0052] Through Tables 1 to 4, Figures 2 to 5 As can be seen, the system and method of the present invention can detect a variety of impurities.

[0053] The above description represents the preferred embodiments of the present invention. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. An electronic-grade silane analysis system, characterized in that, include: First valve (1), second valve (2), third valve (3), fourth valve (4), fifth valve (5), sixth valve (6); The first valve (1) is connected to the second valve (2) through the first pre-analysis column (7), and the second valve (2) is connected to the fourth valve (4) through the first analysis column (8); The first valve (1) is connected to the third valve (3) through the second pre-analysis column (9), and the third valve (3) is connected to the fourth valve (4) through the second analysis column (10); The first valve (1) is connected to the fifth valve (5) through a gas pipeline (11), and the fifth valve (5) is connected to the sixth valve (6) through the third analysis column (12) and the fourth analysis column (13) arranged in parallel. The fourth valve (4) is connected to the first DID detector, and the sixth valve (6) is connected to the second DID detector; the second valve (2) is provided with a first vent pipe (14), the third valve (3) is provided with a second vent pipe (15), the fourth valve (4) is provided with a third vent pipe (16), and the sixth valve (6) is provided with a fourth vent pipe (17). The first valve (1) and the fifth valve (5) are ten-way valves, and the second valve (2), the third valve (3), the fourth valve (4), and the sixth valve (6) are four-way valves.

2. The electronic-grade silane analysis system according to claim 1, characterized in that, The first valve (1) and the fifth valve (5) are provided with ten ports in a clockwise direction, and the second valve (2), the third valve (3), the fourth valve (4), and the sixth valve (6) are provided with four ports in a clockwise direction. The inlet of the first pre-analysis column (7) is connected to the second interface of the first valve (1), and the outlet of the first pre-analysis column (7) is connected to the fourth interface of the second valve (2); the inlet of the first analysis column (8) is connected to the first interface of the second valve (2), and the outlet of the first analysis column (8) is connected to the second interface of the fourth valve (4); The inlet of the second pre-analysis column (9) is connected to the sixth interface of the first valve (1), and the outlet of the second pre-analysis column (9) is connected to the fourth interface of the third valve (3); the inlet of the second analysis column (10) is connected to the first interface of the third valve (3), and the outlet of the second analysis column (10) is connected to the fourth interface of the fourth valve (4); The inlet of the gas pipeline (11) is connected to the fourth interface of the first valve (1), and the outlet of the gas pipeline (11) is connected to the ninth interface of the fifth valve (5); the inlet of the third analytical column (12) is connected to the second interface of the fifth valve (5), and the outlet of the third analytical column (12) is connected to the fourth interface of the sixth valve (6); the inlet of the fourth analytical column (13) is connected to the sixth interface of the fifth valve (5), and the outlet of the fourth analytical column (13) is connected to the second interface of the sixth valve (6); The first DID detector is connected to the third interface of the fourth valve (4), and the second DID detector is connected to the first interface of the sixth valve (6); The first vent pipe (14) is connected to the third interface of the second valve (2); the second vent pipe (15) is connected to the third interface of the third valve (3); the third vent pipe (16) is connected to the first interface of the fourth valve (4); and the fourth vent pipe (17) is connected to the third interface of the sixth valve (6).

3. The electronic-grade silane analysis system according to claim 2, characterized in that, The first valve (1) also includes: The sample inlet line (18) is connected to the 9th port of the first valve (1); The first gas pipeline (19) is connected to the first interface of the first valve (1); The second gas pipeline (20) is connected to the 7th interface of the first valve (1); The first quantitative pipeline (21) is connected at both ends to the 10th and 3rd ports of the first valve (1), respectively; The second quantitative pipeline (22) is connected at both ends to the 8th and 5th ports of the first valve (1), respectively.

4. The electronic-grade silane analysis system according to claim 2, characterized in that, The second valve (2) also includes: The third gas pipeline (23) is connected to the second interface of the second valve (2).

5. The electronic-grade silane analysis system according to claim 2, characterized in that, The third valve (3) also includes: The fourth carrier gas line (24) is connected to the second interface of the third valve (3).

6. The electronic-grade silane analysis system according to claim 2, characterized in that, The fifth valve (5) also includes: The fifth gas carrier line (25) is connected to the first interface of the fifth valve (5); The sixth gas pipeline (26) is connected to the seventh interface of the fifth valve (5); The third quantitative pipeline (27) is connected at both ends to the 10th and 3rd ports of the fifth valve (5), respectively; The fourth quantitative pipeline (28) is connected at both ends to the 8th and 5th ports of the fifth valve (5); The sample discharge line (29) is connected to the fourth port of the fifth valve (5).

7. The electronic-grade silane analysis system according to claim 1, characterized in that, The first pre-analytical column (7) is 8 feet long and 1 / 8 foot in outer diameter. It is packed with Hayesep Q and silanized. The first analytical column (8) has a length of 8 feet, an outer diameter of 1 / 8 foot, and is packed with 13X MS. The second pre-analytical column (9) is 12 feet long and has an outer diameter of 1 / 16 feet. The packing material is Hayesep Q. The second analytical column (10) is 10 feet long and has an outer diameter of 1 / 16 feet. The packing material is Hayesep Q. The third analytical column (12) is a 50m capillary column with an inner diameter of 0.53mm, a film thickness of 10um, and PoraBOND Q packing material. The fourth analytical column (13) is a 60m capillary column with an inner diameter of 0.53mm, a film thickness of 1.5um, and RTX-1 packing material.

8. The electronic-grade silane analysis system according to claim 1, characterized in that, The first valve (1), the second valve (2), the third valve (3), the fourth valve (4), the fifth valve (5), and the sixth valve (6) are VICI. ® Brand name.

9. A method for analyzing electronic-grade silanes, characterized in that, The electronic-grade silane analysis system according to any one of claims 1 to 8 comprises: The first valve (1) injects the sample into the first pre-analysis column (7), where the sample is pre-separated. The initial state of the second valve (2) is to connect the first pre-analysis column (7) with the first analysis column (8). By switching the state of the second valve (2), the silane and CO2 that are at the back are vented through the first vent line (14), while the H2, O2 / Ar, N2, CH4, and CO that are at the front enter the first analysis column (8) for further separation before entering the first DID detector to detect the content of H2, O2 / Ar, N2, CH4, and CO. The first valve (1) injects the sample into the second pre-analysis column (9). The sample is pre-separated in the second pre-analysis column (9). The initial state of the third valve (3) is to connect the second pre-analysis column (9) with the second analysis column (10). By switching the state of the third valve (3), the silane in the middle is vented through the second vent line (15). The CO2 in front and the C2H6 in the back enter the second analysis column (10) for further separation and then enter the first DID detector to detect the content of CO2 and C2H6. The first valve (1) injects the sample into the fifth valve (5) through the gas pipeline (11). Switching the state of the fifth valve (5) allows the sample to enter the third analytical column (12). By switching the state of the sixth valve (6), the silane at the front is vented through the fourth vent pipeline (17), and the following Si2H6, C3H8, and C4H6 are vented. 10 Si2H6, C3H8, and C4H are detected by the second DID detector via the sixth valve (6). 10 The content; The first valve (1) injects the sample into the fifth valve (5) through the gas pipeline (11). The state of the fifth valve (5) is switched to allow the sample to enter the fourth analytical column (13). The state of the sixth valve (6) is switched to allow the silane in front to be vented through the fourth vent pipeline (17). The SiH2Cl2, SiHCl3, and SiCl4 in the back enter the second DID detector through the sixth valve (6) to detect the content of SiH2Cl2, SiHCl3, and SiCl4.

10. The electronic-grade silane analysis method according to claim 9, characterized in that, The injection volume of the first quantitative tube (21) and the second quantitative tube (22) is 0.5 ml, and the injection volume of the third quantitative tube (27) and the fourth quantitative tube (28) is 0.1 ml.

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