System for analyzing impurity components in electronic gas disilane

Abstract

The invention relates to the technical field of a system for analyzing components in electronic gas disilane, in particular to a system for analyzing impurity components in electronic gas disilane. Comprising a first switching valve, a second switching valve communicated with the first switching valve, a third switching valve communicated with the first switching valve and the second switching valve, a first quantitative loop communicated with the first switching valve, a second quantitative loop communicated with the second switching valve and a first carrier gas arranged on the first switching valve, a second carrier gas and sample inlet; and the first switching valve, the second switching valve and the third switching valve are respectively communicated with a first needle valve, a second needle valve and a third needle valve. Therefore, the system for analyzing the impurity components in the electronic gas disilane can solve the technical problems of insufficient separation degree and low qualitative and quantitative accuracy in the prior art.

Description

Technical Field

[0001] This application relates to the technical field of component analysis systems for electronic gas disilane, and more specifically, to an impurity component analysis system for electronic gas disilane. Background Art

[0002] In the fields of semiconductor manufacturing and high-tech electronic materials, disilane (Si2H6), as a key inorganic compound, plays a crucial role. Disilane is a colorless and transparent gas at normal temperature and pressure, with a pungent odor. It is widely used in epitaxial and diffusion processes and is an indispensable material for the preparation of semiconductor devices. At the same time, it is also a core component of solar cells and photosensitive drums for electronic lighting. The purity of disilane is directly related to the yield and performance accuracy of electronic components. Therefore, precise control and analysis of its purity are particularly important.

[0003] However, in the prior art, the analysis of impurity components in disilane still faces many challenges. Although there may be various analysis methods, these methods often have deficiencies in terms of resolution, qualitative and quantitative accuracy, or detection limit. Especially in high-tech fields such as semiconductors and solar cells, the requirements for the purity of disilane are extremely high, and any tiny impurity may have a serious impact on product quality. Therefore, the existing analysis methods are difficult to meet the high-precision analysis requirements for trace impurities in disilane. Summary of the Invention

[0004] Based on the above problems, this application proposes an impurity component analysis system for electronic gas disilane to solve the technical problems of insufficient resolution and low qualitative and quantitative accuracy existing in the prior art.

[0005] To solve the above technical problems, the technical solution adopted by the present invention is:

[0006] An impurity component analysis system for electronic gas disilane includes a first switching valve, a second switching valve connected to the first switching valve, a third switching valve connected to the first switching valve and the second switching valve, a first quantitative loop connected to the first switching valve, a second quantitative loop connected to the second switching valve, and a first carrier gas, a second carrier gas, and a sample inlet provided on the first switching valve; first needle valves, second needle valves, and third needle valves are respectively connected to the first switching valve, the second switching valve, and the third switching valve, first chromatographic columns, third chromatographic columns, and fourth chromatographic columns are respectively connected to the first switching valve, the second switching valve, and the third switching valve, and a second chromatographic column is provided between the first switching valve and the third switching valve; a pulsed discharge helium ionization detector and a fourth needle valve are connected to the third switching valve; a third carrier gas and a fourth carrier gas are connected to the second switching valve.

[0007] In a specific feasible embodiment, ten interfaces are provided on both the first switching valve and the second switching valve, and six interfaces are provided on the third switching valve, and the adjacent interfaces are connected to each other.

[0008] In a specific feasible embodiment, a sample outlet is provided on the second switching valve.

[0009] In a specific feasible embodiment, the inlet and outlet of the first chromatographic column are respectively connected to two of the interfaces on the first switching valve, and the inlet and outlet of the third chromatographic column are respectively connected to two of the interfaces on the second switching valve.

[0010] In a specific feasible embodiment, one end of the fourth chromatographic column is connected to the interface on the third switching valve, and the other end of the fourth chromatographic column is connected to the interface on the second switching valve.

[0011] Positive effects of the present invention:

[0012] This application can detect components of H2, O2, Ar, N2, CH4, CO, CO2, SiH4, C2H6, C3H8, and C4H10 in disilane. The resolution R between each component is ≥1.5, the qualitative and quantitative analysis is accurate, and the detection limit can reach the ppb level.

[0013] By the sequential switching of the first switching valve, the second switching valve, and the third switching valve, a multi-dimensional separation channel is constructed. The first chromatographic column and the second chromatographic column form a complementary separation system, and in combination with the cascade of the third chromatographic column and the fourth chromatographic column, gradient separation of impurity components is achieved. For example, for common homolog impurities in disilane, the system can achieve effective separation of complex mixtures through the combination of chromatographic columns with different polarities.

[0014] Dynamic compensation of the quantitative loop. Through the design of quantitative loops with different capacities, automatic adjustment can be achieved for impurities in different concentration ranges, avoiding the masking effect of high-concentration components on trace impurities, and significantly improving the separation effect of low-content impurities. The detection limit of key impurities reaches an extremely low level, meeting the strict requirements for the purity of disilane in high-tech fields. Description of the drawings

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only the embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained according to the provided drawings without creative efforts.

[0016] Figure 1 It is the sampling state diagram of the present invention;

[0017] Figure 2 is the state diagram for analyzing the states of H2, O2, Ar, N2, CH4, and CO in the present invention;

[0018] Figure 3 is the state diagram for analyzing CO2, SiH4, C2H6, C3H8, C4H 10 in the present invention;

[0019] Description of the reference numerals in the drawings

[0020] 1. First switching valve; 2. Second switching valve; 3. Third switching valve; 4. Sample inlet; 5. First sampling loop; 6. Second sampling loop; 7. Sample outlet; 8. First carrier gas; 9. Second carrier gas; 10. Third carrier gas; 11. Fourth carrier gas; 12. First chromatographic column; 13. Second chromatographic column; 14. Third chromatographic column; 15. Fourth chromatographic column; 16. Pulse discharge helium ionization detector; 17. First needle valve; 18. Second needle valve; 19. Third needle valve; 20. Fourth needle valve. Detailed implementation manners

[0021] Next, the technical solutions in the embodiments of the present application will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present application without creative efforts shall fall within the protection scope of the present application.

[0022] Embodiment

[0023] As Figures 1-3 shown, an impurity component analysis system for disilane in electronic gases includes a first switching valve 1, a second switching valve 2 connected to the first switching valve 1, and a sample outlet 7 provided on the second switching valve 2.

[0024] The first switching valve 1 and the second switching valve 2 are connected to a third switching valve 3. The first switching valve 1 is connected to a first sampling loop 5. The second switching valve 2 is connected to a second sampling loop 6, and a first carrier gas 8, a second carrier gas 9, and a sample inlet 4 are provided on the first switching valve 1. First needle valves 17, second needle valves 18, and third needle valves 19 are respectively connected to the first switching valve 1, the second switching valve 2, and the third switching valve 3. First chromatographic columns 12, third chromatographic columns 14, and fourth chromatographic columns 15 are respectively connected to the first switching valve 1, the second switching valve 2, and the third switching valve 3. A second chromatographic column 13 is provided between the first switching valve 1 and the third switching valve 3. A pulse discharge helium ionization detector 16 and a fourth needle valve 20 are connected to the third switching valve 3.

[0025] As the core detection unit, the helium ionization detector has extremely high sensitivity and significant response values to silane compounds. Combining with the carrier gas modulation function of the needle valve, it can optimize the impurity peak shape and improve the quantitative repeatability. Through the flow control of multiple needle valves, the system can synchronously collect multi-dimensional data such as chromatographic retention time, peak area, and peak height, and realize the accurate qualitative analysis of impurity components by comparing with the standard database.

[0026] Both the first switching valve 1 and the second switching valve 2 are provided with ten interfaces, and the third switching valve 3 is provided with six interfaces, and the adjacent interfaces are connected to each other. The ten-way switching valve is selected as the first switching valve 1 and the second switching valve 2 to achieve complex gas flow control.

[0027] This application realizes the clear definition of the number and connection method of the switching valve interfaces, effectively solving the problems of unclear gas flow path and improper interface matching. Specifically, the design of ten interfaces enables the first switching valve 1 and the second switching valve 2 to simultaneously accommodate multiple gas channels, quantitative loops, chromatographic columns, and carrier gas input and output, ensuring the complete connection and non-interference between each functional module. The six interfaces of the third switching valve 3 match its simplified functional requirements in the system, avoiding redundant structures. Thus, the overall structure of the gas analysis system is more compact, the gas flow path is clearer, and the potential gas leakage risk is reduced.

[0028] Furthermore, the connection design between adjacent interfaces eliminates the possible disconnection or misconnection risks between interfaces, ensuring the continuous path and stable pressure of the gas flowing inside the switching valve, thereby improving the reliability of impurity separation and detection. The six-way switching valve is selected as the third switching valve 3 for further gas flow distribution and sample analysis. The six-way switching valve has a compact structure and simple operation, and is suitable for high-precision analysis.

[0029] The inlet and outlet of the first chromatographic column 12 are respectively connected to two of the interfaces on the first switching valve 1, and the inlet and outlet of the third chromatographic column 14 are respectively connected to two of the interfaces on the second switching valve 2.

[0030] One end of the fourth chromatographic column 15 is connected to the interface on the third switching valve 3, and the other end of the fourth chromatographic column 15 is connected to the interface on the second switching valve 2.

[0031] By means of the sequential switching of the first switching valve 1, the second switching valve 2, and the third switching valve 3, a multi-dimensional separation channel is constructed. The first chromatographic column 12 and the second chromatographic column 13 form a complementary separation system, which, in combination with the cascade of the third chromatographic column 14 and the fourth chromatographic column 15, realizes the gradient separation of impurity components. For the homologous impurities commonly found in disilane, the system can achieve the effective separation of complex mixtures through the combination of chromatographic columns with different polarities.

[0032] Through the design of sampling loops with different volumes, automatic adjustment can be achieved for impurities in different concentration ranges, avoiding the masking effect of high-concentration components on trace impurities and significantly improving the separation effect of low-content impurities.

[0033] Sampling process: As Figure 1 In the [specific state], the sample enters from the sample inlet 4, sequentially passes through the second interface, the third interface, the first sampling loop 5, and the tenth interface of the first switching valve 1, and then enters the first interface, the tenth interface, the second sampling loop 6, the third interface, and the second interface of the second switching valve 2 from the first interface of the first switching valve 1, and finally is discharged from the sample outlet 7.

[0034] Analysis process: Switch the first switching valve 1 to Figure 2 In the [specific state], the first carrier gas 8 carries the sample in the first sampling loop 5 through the first chromatographic column 12, and then enters the pulsed discharge helium ionization detector 16 through the second chromatographic column 13 to detect impurities such as hydrogen, oxygen, argon, nitrogen, methane, and carbon monoxide. When the first switching valve 1 is reset, the heavy components in disilane are carried by the first carrier gas 8 and the heavy components retained in the first chromatographic column 12 are discharged through the eighth interface of the first switching valve 1 by the first needle valve 17.

[0035] Switch the second switching valve 2 and the third switching valve 3 to Figure 3 In the [specific state], the third carrier gas 10 carries the sample in the second sampling loop 6 through the third chromatographic column 14, and then enters the pulsed discharge helium ionization detector 16 through the fourth chromatographic column 15 to detect impurities such as carbon dioxide, silane, ethane, propane, and n-butane. When the second switching valve 2 is reset, the remaining disilane is carried by the fourth carrier gas 11 and the disilane retained in the third chromatographic column 14 is discharged through the eighth interface of the second switching valve 2 by the second needle valve 18.

[0036] The resolution of common impurities in disilane is significantly improved, meeting the analysis requirements of high-purity disilane. The detection limit of key impurities reaches an extremely low level, meeting the strict requirements for the purity of disilane in high-tech fields.

[0037] Finally, it should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the presence of other identical elements in the process, method, article or device including the elements.

[0038] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. An impurity component analysis system for disilane in electronic gases, characterized in that, It includes a first switching valve (1), a second switching valve (2) connected to the first switching valve (1), a third switching valve (3) connected to the first switching valve (1) and the second switching valve (2), a first quantitative loop (5) connected to the first switching valve (1), a second quantitative loop (6) connected to the second switching valve (2), and a first carrier gas (8), a second carrier gas (9) and a sample inlet (4) provided on the first switching valve (1); a first needle valve (17), a second needle valve (18) and a third needle valve (19) are respectively connected to the first switching valve (1), the second switching valve (2) and the third switching valve (3), a first chromatographic column (12), a third chromatographic column (14) and a fourth chromatographic column (15) are respectively connected to the first switching valve (1), the second switching valve (2) and the third switching valve (3), and a second chromatographic column (13) is provided between the first switching valve (1) and the third switching valve (3); a pulsed discharge helium ionization detector (16) and a fourth needle valve (20) are connected to the third switching valve (3); a third carrier gas (10) and a fourth carrier gas (11) are connected to the second switching valve (2).

2. The impurity component analysis system for disilane in electronic gas according to claim 1, wherein Ten interfaces are provided on both the first switching valve (1) and the second switching valve (2), six interfaces are provided on the third switching valve (3), and adjacent interfaces are connected to each other.

3. An impurity component analysis system for disilane in electronic gas according to claim 1, characterized in that, A sample outlet (7) is provided on the second switching valve (2).

4. The impurity component analysis system for disilane in electronic gas according to claim 1, wherein, The inlet and outlet of the first chromatographic column (12) are respectively connected to two of the interfaces on the first switching valve (1), and the inlet and outlet of the third chromatographic column (14) are respectively connected to two of the interfaces on the second switching valve (2).

5. The impurity component analysis system for disilane in electronic gas according to claim 1, wherein One end of the fourth chromatographic column (15) is connected to the interface on the third switching valve (3), and the other end of the fourth chromatographic column (15) is connected to the interface on the second switching valve (2).

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