CN-122017097-A - Device and method for detecting chlorosilane

Abstract

The invention relates to the technical field of chemical gas chromatography analysis and detection, in particular to a device and a method for detecting chlorosilane, comprising the following steps of inserting a needle head of a syringe into a chlorosilane sample bottle, pulling back a push rod at a V pull-back speed, and extracting a V1 sample; the needle head of the injector is inserted into the sample inlet of the heated gas chromatograph for detection, and the slow liquid pumping and bubble discharging steps effectively avoid the problem of inaccurate sample injection volume caused by bubbles generated by rapid volatilization of chlorosilane, thereby remarkably improving the accuracy of gas chromatography detection data and the repeatability of experiments, combining the high temperature of a specific sample inlet after the injection is finished, ensuring the instant complete gasification of the chlorosilane sample, preventing the needle head residue or the sample from volatilizing in advance in the needle, ensuring the detection integrity and avoiding the cross contamination to the sample inlet and the chromatographic column.

Inventors

• ZHANG KE
• ZHANG XUEQI
• BAI SHENGYU
• LIU FANG
• ZHOU JING

Assignees

• 安徽湛为气体有限公司

Dates

Publication Date

20260512

Application Date

20260127

Claims (10)

1. 1. A device for detecting chlorosilane is characterized by comprising, A syringe (101) for containing chlorosilanes, and a push rod (102) movable inside the syringe (101), the syringe (101) internal volume V c being expressed as: , When the chlorosilane sample is extracted and detected, the pull-back speed Q of the push rod (102) is 0.05-0.15 mL/s, and the stroke change speed v s of the push rod (102) meets the following relation: , Wherein A b is the cross-sectional area of the needle cylinder (101), S max is the maximum stroke of the push rod (102), pi is the circumference ratio, and D is the inner diameter of the needle cylinder (101).
2. 2. The device for chlorosilane detection as claimed in claim 1, characterized in that the needle cylinder (101) is made of polypropylene or polyethylene resistant to chlorosilane corrosion, the nominal value of the internal volume V c is nmL, and the cylinder body is provided with a volume mark of 0.1nmL based on the minimum scale of the stroke S; Wherein n is less than or equal to 3.
3. 3. The apparatus for detecting chlorosilanes as in claim 1 or 2 further comprising a needle (103) connected to the cylinder (101), wherein the length L of the needle (103) satisfies 25 mm≤L≤50 mm.
4. 4. The apparatus for detecting chlorosilanes as in claim 3, wherein said needle (103) has an inner diameter d of 0.1 mm≤d≤0.2 mm.
5. 5. A method for detecting chlorosilane, which comprises the device for detecting chlorosilane as in claim 1-4, and is characterized by comprising the following steps: Inserting a needle (103) of the injector into a chlorosilane sample bottle, and pulling back a push rod (102) at a V-pulling back speed to extract a V1 sample; The needle (103) of the injector is upwards, so that the bubbles float to the top, and the bubbles are pushed to be discharged, so that the syringe (101) is filled with the sample; The needle (103) is inserted into the sample inlet of the heated gas chromatograph for detection.
6. 6. The method for detecting chlorosilane according to claim 5, wherein the volume V1 of the extracted chlorosilane sample is 0.45-0.55 mL, and the time T for completing the injection is as follows: , Wherein F is pushing force of the push rod (102), and mu is dynamic viscosity of the chlorosilane sample.
7. 7. The method for detecting chlorosilane as in claim 6, wherein said inserting a needle (103) into an already heated gas chromatography sample inlet is performed while the time T for completing the injection is less than or equal to 1s.
8. 8. The method for chlorosilane detection as claimed in any one of claims 5 to 7, wherein the bubble removal completion is marked by visual observation of a complete sample droplet deposited at the end of the needle (103).
9. 9. The method for chlorosilane detection as in claim 8 wherein said chlorosilane sample comprises but is not limited to dichlorosilane, trichlorosilane, silicon tetrachloride or mixtures thereof.
10. 10. The method for chlorosilane detection as claimed in claim 5, 6,7 and 9, wherein the sample inlet temperature of said heated gas chromatograph is 120-180 ℃ during detection.

Description

Device and method for detecting chlorosilane Technical Field The invention relates to the technical field of chemical gas chromatography analysis and detection, in particular to a device and a method for detecting chlorosilane. Background Chlorosilane is a core raw material in the semiconductor and photovoltaic industries (such as trichlorosilane is a key intermediate for preparing polysilicon and silane gas), but has extremely active chemical properties, strong corrosiveness (easy reaction with metal and glass), easy hydrolysis, easy volatilization (low boiling point of partial varieties) and the like. In industrial production, rapid and accurate Gas Chromatography (GC) analysis of chlorosilane composition and impurity content is a key element in quality control. However, chlorosilanes have extremely strong chemical activity (easy hydrolysis, easy reaction with metal/glass) and high volatility, which presents serious challenges to conventional GC injection operations, leading to the following systematic drawbacks of existing detection methods: When the traditional injector rapidly extracts chlorosilane, instantaneous negative pressure is generated in a needle cylinder, so that chlorosilane components with lower boiling points are subjected to flash evaporation, a large number of microbubbles are generated, the microbubbles are difficult to completely remove in subsequent bubble removal operation, the volume of a detection sample actually entering a chromatographic column is smaller than a set value, the peak area is low, the quantification is inaccurate, and the detection deviation is often 5% -10%. The prior methods lack standardized operating parameters (such as extraction speed, bubble removal standard, sample injection speed). Operators are controlled by experience, the difference between different personnel and different operations is obvious, the Relative Standard Deviation (RSD) of the detection result is often more than 3%, and the requirements of modern industry on the precision of data can not be met. Aiming at the technical problems in the prior art, a device and a method for detecting chlorosilane are provided. Disclosure of Invention Some simplifications or omissions may be made in this section as well as in the description of the application and in the title of the application, which may not be used to limit the scope of the application. In order to solve the defects in the prior art, one aim of the invention is to provide a device for detecting chlorosilane. In order to achieve the above object, the present invention adopts the following technical scheme that an apparatus for detecting chlorosilane comprises a syringe for containing chlorosilane, and a push rod movable inside the syringe, wherein the syringe internal volume V c is expressed as: , When the chlorosilane sample is extracted and detected, the push rod pull-back speed Q is 0.05-0.15 mL/s, and the stroke change speed v s of the push rod meets the following relation: , Wherein A b is the cross-sectional area of the syringe, S max is the maximum stroke of the push rod, pi is the circumference ratio, and D is the inside diameter of the syringe. As a preferred scheme of the device for detecting chlorosilane, the syringe is made of polypropylene or polyethylene resistant to chlorosilane corrosion, the nominal value of the internal volume V c is nmL, and the cylinder body is provided with a volume mark with the minimum scale of 0.1nmL based on the stroke S, wherein n is less than or equal to 3. As a preferable scheme of the device for detecting chlorosilane, the device also comprises a needle connected with the syringe, wherein the length L of the needle is 25-mm-50 mm. As a preferable scheme of the device for detecting chlorosilane, the inner diameter d of the needle is 0.1 mm-0.2 mm. The device for detecting the chlorosilane has the beneficial effects that the core problems of flash evaporation and bubble generation of the chlorosilane caused by negative pressure generated by rapid liquid extraction are directly solved, the generation of bubbles is stopped from the source, a solid foundation is laid for the follow-up accurate sample injection, and a complete device scheme with a parameter which can be calculated and can be controlled is formed by combining a cylindrical structure and a volume formula of a needle cylinder. In order to solve the defects in the prior art, another object of the invention is to provide a method for detecting chlorosilane. In order to achieve the above-mentioned aim, the invention adopts the following technical scheme that the method for detecting chlorosilane comprises a device for detecting chlorosilane, and comprises the following steps of inserting a needle of a syringe into a chlorosilane sample bottle, pulling a push rod back at a pull speed of V to extract a sample of V1, upwards floating the needle of the syringe to the top, pushing bubbles to the top, discharging the bubbles, filling the syringe wi