CN104849366B - Detecting system and detection method - Google Patents
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- CN104849366B CN104849366B CN201510236831.3A CN201510236831A CN104849366B CN 104849366 B CN104849366 B CN 104849366B CN 201510236831 A CN201510236831 A CN 201510236831A CN 104849366 B CN104849366 B CN 104849366B
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Abstract
The invention provides a kind of detecting system and detection method.The detecting system includes hydrogen feeding mechanism, inert gas feeding mechanism, vaporizer and mixing chamber, vaporizer has the injection port for being used for being passed through chlorosilane, the first entrance of mixing chamber is connected with the outlet of vaporizer, and the outlet of hydrogen feeding mechanism and the outlet of inert gas feeding mechanism are connected in parallel in the second entrance of mixing chamber；The detecting system also includes chlorosilane reduction apparatus, removing means, methane adsorption desorption device, gas chromatograph and the data output device for being sequentially connected in series setting, and the entrance of chlorosilane reduction apparatus and the outlet of mixing chamber, removing means are used to remove hydrogen chloride and unreacted chlorosilane.Carbon hydro-reduction in chlorine-containing silane is methane by chlorosilane reduction apparatus by the present invention, and then methane is sent into gas chromatograph and the carbon content in methane is measured, it is achieved thereby that the total carbon content in detection chlorine-containing silane.
Description
Technical field
The present invention relates to analysis detection field, in particular to a kind of detecting system and detection method.
Background technology
In current polysilicon preparation field, meeting association generation silicon tetrachloride, dichlorosilane when producing trichlorosilane.Also
It is to say, in polysilicon preparation field, three kinds of chlorosilanes can not individually produce, but three kinds of chlorosilanes have (the i.e. present invention simultaneously
In chlorine-containing silane).Wherein, trichlorosilane is the important raw and processed materials for preparing grade multi-crystalline silicon and solar-grade polysilicon,
And the important intermediate of manufacture silane coupler and other organosilicon products.With it is international and domestic to polysilicon demand increasingly
The stable supply of the trichlorosilane of increase, high-volume and high quality just seems and of crucial importance.
At present, generally use distillation technology purifies to trichlorosilane in chlorine-containing silane, and impurity content is more low better, its
In described impurity include carbon (total carbon) existing for various forms.In the quality index of polysilicon, carbon content is one
Important index.Carbon content number directly affect polycrystalline silicon material application and device efficiency, and the carbon in chlorine-containing silane is then
It is the important sources of carbon in polysilicon, therefore for the measurement of total carbon content in chlorine-containing silane, it appears it is particularly important.
The existence form of carbon is mainly that various methylchlorosilanes, ethyl chlorosilane, chloroform etc. are carbon containing in chlorine-containing silane
Compound.It is inflammable, explosive due to chlorosilane low boiling point, facile hydrolysis, and hydrogen chloride and hydrated SiO 2 are then produced after hydrolyzing,
Make system corrosion, block and be contaminated, so the on-line checking analysis to chlorosilane is very difficult.At present, in chlorosilane
Carbon content, analysis measurement is typically carried out using instruments such as gas chromatographicanalyzer, infrared spectrum analyser, gas-matter analyzers.More than
Although analytical equipment can be carried out to carbon content in chlorosilane, can only all analysis detection be carried out to single or fractions,
And the total carbon content in chlorosilane can not be measured.Therefore, using existing method of testing, it is impossible to these middle productions to trichlorosilane
Carbon content is monitored control in product, so as to cannot also monitor influence of the total carbon to polysilicon product quality in chlorosilane.
High-temperature hydrogen reduction gas chromatograph is used occasionally to survey the element such as phosphorus, arsenic in trichlorosilane, but it is total not always to be used to measurement
Carbon content, the total carbon content in chlorine-containing silane is also measured using this equipment without the method for correlation.
The content of the invention
It is a primary object of the present invention to provide a kind of detecting system and detection method, to detect the total carbon in chlorine-containing silane
Content.
To achieve these goals, according to an aspect of the invention, there is provided a kind of detecting system, chloride for detecting
Total carbon content in silane, the detecting system include hydrogen feeding mechanism, inert gas feeding mechanism, vaporizer and mixing chamber,
Vaporizer has the injection port for being used for being passed through chlorosilane, and the first entrance of mixing chamber is connected with the outlet of vaporizer, and hydrogen supplies
The outlet of device and the outlet of inert gas feeding mechanism is answered to be connected in parallel in the second entrance of mixing chamber；The detecting system is also wrapped
Include the chlorosilane reduction apparatus for being sequentially connected in series setting, removing means, methane adsorption desorption device, gas chromatograph and data output dress
Put, and the outlet of the entrance of chlorosilane reduction apparatus and mixing chamber, removing means is used to removing hydrogen chloride and unreacted
Chlorosilane.
Further, detecting system also includes exhausting pipeline, and the outlet of removing means, methane adsorption desorption device enter
Mouth, the outlet of inert gas feeding mechanism, the entrance of gas chromatograph, the outlet of methane adsorption desorption device and exhausting pipeline order
It is connected on six-way valve；When six-way valve is adjusted to Enrichment Mode, the outlet of removing means and the entrance of methane adsorption desorption device it
Between, between the entrance of the outlet of inert gas feeding mechanism and gas chromatograph and methane adsorption desorption device outlet and put
Turned between vacant duct；When six-way valve is adjusted to analytical model, between the outlet of removing means and exhausting pipeline, methane adsorption desorption
Between the outlet of the entrance and inert gas feeding mechanism of device, the entrance of the outlet of methane adsorption desorption device and gas chromatograph
Between turn on.
Further, set between the outlet of inert gas feeding mechanism, the outlet of hydrogen feeding mechanism and second entrance
There is triple valve.
Further, chlorosilane reduction apparatus includes quartz ampoule and heater.
Further, removing means includes the hydrogen chloride removing pipe being sequentially connected and condenser, and condenser includes filling liquid
The condensing container of nitrogen and the dehydrating tube being placed in liquid nitrogen.
Further, methane adsorption desorption device includes filling the adsorption desorption container of solvent and the enrichment being arranged in solvent
Post；When methane adsorption desorption device is used for adsorbed methane, solvent is liquid nitrogen, molten when methane adsorption desorption device is used to be desorbed methane
Agent is boiling water.
Further, hydrogen feeding mechanism includes hydrogen source and the hydrogen being connected with hydrogen source decompression pressure regulator；Inertia
Gas supply device includes inert gas source and the inert gas being connected with inert gas source decompression pressure regulator；Gas chromatograph
Including flame ionization ditector；Data output device is computer or data logger.
To achieve these goals, according to another aspect of the present invention, there is provided a kind of detection method, the detection method
The total carbon content in chlorine-containing silane is detected using the detecting system of the bright offer of this law, the detection method includes following step
Suddenly：Step S1, the inert gas feeding mechanism in detecting system is opened, carrying out gas to detecting system using inert gas puts
Change；Step S2, the chlorosilane reduction apparatus in detecting system is warming up to preset temperature；Step S3, open in detecting system
Hydrogen feeding mechanism, gas chromatograph and data output device, and hydrogen is passed through into detecting system；Step S4, it is to detection
Injection port in system is passed through chlorosilane, makes the chlorosilane reduction apparatus of chlorosilane and hydrogen in the detection system react to form first
Alkane；Step S5, methane is adsorbed and is desorbed using the methane adsorption desorption device in detecting system, and utilize gas chromatograph
Parsing test is carried out to the methane after desorption, while using the peak area of data output device record methane.
Further, inert gas feeding mechanism includes inert gas decompression pressure regulator, and inert gas feeding mechanism goes out
Mouthful, be provided with triple valve between the second entrance of mixing chamber in the outlet and detecting system of hydrogen feeding mechanism；In step S1,
Adjust inert gas and depressurize pressure regulator to 1~5MPa, and swivel tee valve is so that inert gas is put to the gas in detecting system
Change 3~10min.
Further, the removing means in detecting system includes the hydrogen chloride removing pipe being sequentially connected and condenser, detection
System also includes six-way valve, and methane adsorption desorption device includes enriching column；In step S2, dehydrating tube is inserted in liquid nitrogen, six are led to
Valve is adjusted to analytical model, chlorosilane reduction apparatus then is warming up into 800~1100 DEG C, the heating-up time is 40~60min.
Further, hydrogen feeding mechanism includes hydrogen source and the hydrogen being connected with hydrogen source decompression pressure regulator, gas phase
Chromatograph includes flame ionization ditector；In step S3, hydrogen source is opened, and swivel tee revolves and causes hydrogen to enter detection
System, gas chromatograph is then opened, into gas chromatograph, injector temperature is 80~120 DEG C, the temperature 180 of chromatographic column~
200 DEG C, the temperature of detector is 200~250 DEG C, and the nebulizer gas pressure of gas chromatograph is 0.395~0.405MPa, gas-chromatography
The flow of hydrogen is 30ml/min~50ml/min in instrument, and controls hydrogen decompression pressure regulator Hydrogen Vapor Pressure control is existed
2.0Mpa, finally light flame ionization ditector and log-on data output device.
Further, in step S4, six-way valve is rotated to Enrichment Mode, while enriching column is inserted in liquid nitrogen, then
The vaporizer entered using 20~100 microlitres of chlorosilane of microsyringe absorption in detecting system.
Further, in step S5, after the injection port into detecting system is passed through 10~20min of chlorosilane, rotation six is logical
Valve inserts enriching column in boiling water to analytical model and carries out parsing test, while the peak of methane is recorded by data output device
Area；After step s 5, detection method also includes：Enriching column is taken out from boiling water, swivel tee valve is to be passed through indifferent gas
Body cools to chlorosilane reduction apparatus；Hydrogen feeding mechanism and data output device are closed, and works as chlorosilane reduction apparatus
Inert gas feeding mechanism is closed when being cooled to less than 200 DEG C.
Further, chlorine-containing silane is reacted by the raw material including hydrogen and tetrachloro silicane and formed, main group of chlorine-containing silane
It is divided into dichlorosilane, trichlorosilane and silicon tetrachloride.
Apply the technical scheme of the present invention, the present invention is hydrogenated the carbon in chlorine-containing silane by chlorosilane reduction apparatus
Methane is reduced to, then methane is sent into gas chromatograph and the carbon content in methane is measured, it is achieved thereby that inspection
The total carbon content surveyed in chlorine-containing silane.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the schematic diagram of the detecting system provided according to the specific embodiment of the invention；And
Fig. 2 a show that the six-way valve in the detecting system provided according to the specific embodiment of the invention is adjusted to Enrichment Mode
When schematic diagram；And
Fig. 2 b show that the six-way valve in the detecting system provided according to the specific embodiment of the invention is adjusted to analytical model
When schematic diagram.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the application in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
For the ease of description, space relative terms can be used herein, as " ... on ", " ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be appreciated that space relative terms are intended to comprising the orientation except device described in figure
Outside different azimuth in use or operation.For example, if the device in accompanying drawing is squeezed, it is described as " in other devices
It will be positioned as " under other devices or construction after the device of part or construction top " or " on other devices or construction "
Side " or " under other devices or construction ".Thus, exemplary term " ... top " can include " ... top " and
" in ... lower section " two kinds of orientation.The device can also other different modes positioning (being rotated by 90 ° or in other orientation), and
And respective explanations are made to the relative description in space used herein above.
From background technology, prior art can not measure the total carbon content in chlorine-containing silane.The present inventor's pin
Above mentioned problem is studied, there is provided a kind of detecting system, for detecting the total carbon content in chlorine-containing silane.As shown in figure 1,
The detecting system includes：Hydrogen feeding mechanism 1, inert gas feeding mechanism 2, vaporizer 3 and mixing chamber 4, vaporizer 3, which has, to be used
In the injection port for being passed through chlorosilane, the first entrance of mixing chamber 4 is connected with the outlet of vaporizer 3, and hydrogen feeding mechanism 1 goes out
The outlet of mouth and inert gas feeding mechanism 2 is connected in parallel in the second entrance of mixing chamber 4；The detecting system also includes going here and there successively
Join chlorosilane reduction apparatus 6, removing means, methane adsorption desorption device, gas chromatograph 12 and the data output device 13 set,
And the outlet of the entrance of chlorosilane reduction apparatus 6 and mixing chamber 4, removing means are used to remove hydrogen chloride and unreacted chlorine
Silane.
Carbon hydro-reduction in chlorine-containing silane is methane by chlorosilane reduction apparatus 6 by above-mentioned detection device, so
Methane is sent into gas chromatograph 12 afterwards and the carbon content in methane is measured, it is achieved thereby that in detection chlorine-containing silane
Total carbon content.
In a preferred embodiment, detecting system also includes exhausting pipeline, and outlet, the methane suction of removing means
The entrance of desorption apparatus, the outlet of inert gas feeding mechanism 2, the entrance of gas chromatograph 12, methane adsorption desorption device go out
Mouth and exhausting pipeline are linked in sequence on six-way valve 9；When six-way valve 9 is adjusted to Enrichment Mode, the outlet of removing means and methane
Between the entrance of adsorption desorption device, between the entrance of the outlet of inert gas feeding mechanism 2 and gas chromatograph 12 and methane
Turned on (as shown in Figure 2 a) between the outlet of adsorption desorption device and exhausting pipeline；When six-way valve 9 is adjusted to analytical model, removing dress
Between the outlet put and exhausting pipeline, between the outlet of the entrance of methane adsorption desorption device and inert gas feeding mechanism 2, methane
Turned on (as shown in Figure 2 b) between the outlet of adsorption desorption device and the entrance of gas chromatograph 12.
Preferably, set between the outlet of inert gas feeding mechanism 2, the outlet of hydrogen feeding mechanism 1 and second entrance
There is triple valve 5.Chlorosilane reduction apparatus 6 includes quartz ampoule and heater.Removing means includes the hydrogen chloride removing being sequentially connected
Pipe 7 and condenser, condenser include filling the condensing container of liquid nitrogen and the dehydrating tube 8 being placed in liquid nitrogen.
Specifically, methane adsorption desorption device includes filling the adsorption desorption container of solvent and the enriching column being arranged in solvent
10；When methane adsorption desorption device is used for adsorbed methane, solvent is liquid nitrogen, molten when methane adsorption desorption device is used to be desorbed methane
Agent is boiling water.Hydrogen feeding mechanism 1 includes hydrogen source and the hydrogen being connected with hydrogen source decompression pressure regulator；Inert gas is supplied
Device 2 includes inert gas source and the inert gas being connected with inert gas source decompression pressure regulator；Gas chromatograph 12 includes
Flame ionization ditector；Data output device 13 is computer or data logger.Preferably, inert gas is nitrogen.
Wherein, flame ionization ditector (FID) is using more wide in the detection and analysis experiment of gas chromatograph 12
A kind of general detector, its operation principle are：Flame is produced as the energy using oxygen combustion in hydrogen and air, works as detected sample
During into flame, under the high energy effect of flame, it is excited and produces ion.Ion is in the presence of interpolar DC electric field, quilt
Excite and produce ion.Ion, with regard to displacement, forms a kind of weak current, Ran Houliu in the presence of interpolar DC electric field
Voltage signal is taken out through high resistance, the amplified secondary signal recording apparatus of feeding is recorded.
According to another aspect of the present invention, there is provided a kind of detection method, the detection method utilize the bright offer of this law
Detecting system detects to the total carbon content in chlorine-containing silane, and the detection method comprises the following steps：Step S1, detection is opened
Inert gas feeding mechanism 2 in system, gas displacement is carried out to detecting system using inert gas；Step S2, it is by detection
Chlorosilane reduction apparatus 6 in system is warming up to preset temperature；Step S3, the hydrogen feeding mechanism 1 in opening detecting system, gas phase
Chromatograph 12 and data output device 13, and hydrogen is passed through into detecting system；Step S4, the injection port into detecting system leads to
Enter chlorosilane, the reaction of chlorosilane reduction apparatus 6 of chlorosilane and hydrogen in the detection system is formed methane；Step S5, utilize
Methane adsorption desorption device in detecting system is adsorbed and is desorbed to methane, and using gas chromatograph 12 to the first after desorption
Alkane carries out parsing test, while the peak area of methane is recorded using data output device 13.Wherein, chlorine-containing silane is by including hydrogen
React to be formed with the raw material of tetrachloro silicane, the key component of chlorine-containing silane is dichlorosilane, trichlorosilane and silicon tetrachloride.
The illustrative embodiments according to detection method provided by the invention are described in more detail below.However, these
Illustrative embodiments can be implemented by many different forms, and should not be construed to be limited solely to set forth herein
Embodiment.It should be appreciated that these embodiments are provided so that disclosure herein is thoroughly and complete, and will
The design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
First, step S1 is performed, that is, the inert gas feeding mechanism 2 in detecting system is opened, using inert gas to inspection
Examining system carries out gas displacement.Preferably, inert gas feeding mechanism 2 includes inert gas decompression pressure regulator, and inert gas supplies
Answer the outlet of device 2, mixing chamber 4 in the outlet and detecting system of hydrogen feeding mechanism 1 second entrance between be provided with three
Port valve 5；In step S1, regulation inert gas depressurizes pressure regulator to 1~5MPa, and swivel tee valve 5 so that inert gas to inspection
3~10min of gas displacement in examining system.
Then, step S2 is performed, i.e., the chlorosilane reduction apparatus 6 in detecting system is warming up to preset temperature.Preferably,
The hydrogen chloride removing pipe 7 and condenser, detecting system that removing means in detecting system includes being sequentially connected also include six-way valve
9, methane adsorption desorption device includes enriching column 10；In step S2, dehydrating tube 8 is inserted in liquid nitrogen, six-way valve 9 is adjusted to analysis
Pattern, chlorosilane reduction apparatus 6 is then warming up to 800~1100 DEG C, the heating-up time is 40~60min.
Next, performing step S3, that is, open hydrogen feeding mechanism 1, gas chromatograph 12 and data in detecting system
Output device 13, and hydrogen is passed through into detecting system.It is connected when hydrogen feeding mechanism 1 including hydrogen source and with hydrogen source
Hydrogen depressurizes pressure regulator, and gas chromatograph 12 includes flame ionization ditector；In step S3, hydrogen source is opened, and rotate
Threeway, which is revolved, causes hydrogen to enter detecting system, then opens gas chromatograph 12, injector temperature is into gas chromatograph 12
80~120 DEG C, 180~200 DEG C of the temperature of chromatographic column, the temperature of detector is 200~250 DEG C, the carrier gas of gas chromatograph 12
Pressure is 0.395~0.405MPa, and the flow of hydrogen is 30ml/min~50ml/min in gas chromatograph 12, and controls hydrogen
Decompression pressure regulator makes Hydrogen Vapor Pressure control in 2.0Mpa, finally lights flame ionization ditector and log-on data output device
13。
Next, performing step S4, i.e., the injection port into detecting system is passed through chlorosilane, is examining chlorosilane and hydrogen
The reaction of chlorosilane reduction apparatus 6 in examining system forms methane.Specifically, in step S4, six-way valve 9 is rotated to enrichment mode
Formula, while enriching column 10 is inserted in liquid nitrogen, 20~100 microlitres of chlorosilane is then drawn using microsyringe and enters detection
Vaporizer 3 in system.
Finally, step S5 is performed, i.e., methane is adsorbed and is desorbed using the methane adsorption desorption device in detecting system,
And parsing test is carried out to the methane after desorption using gas chromatograph 12, while methane is recorded using data output device 13
Peak area.Specifically, in step S5, after the injection port into detecting system is passed through 10~20min of chlorosilane, six-way valve 9 is rotated
To analytical model, enriching column 10 is inserted parsing test is carried out in boiling water, while methane is recorded by data output device 13
Peak area；After step s 5, detection method also includes：Enriching column 10 is taken out from boiling water, swivel tee valve 5 is lazy to be passed through
Property gas cools to chlorosilane reduction apparatus 6；Hydrogen feeding mechanism 1 and data output device 13 are closed, and works as chlorosilane
Reduction apparatus 6 closes inert gas feeding mechanism 2 when being cooled to less than 200 DEG C.
Detecting system and detection method provided by the invention are further illustrated below in conjunction with specific steps.
It is as follows with nitrogen as inert gas, its specific implementation step in the detection method：
1. opening Nitrogen source gases, regulation nitrogen depressurizes pressure regulator to 2.0MPa；Swivel tee valve is to " nitrogen " position.To being
System carries out nitrogen displacement 5min；
2. in a dehydrating tube insertion liquid nitrogen, six-way valve is adjusted to " analysis " position；
3. setting the reduction temperature of quartz ampoule as 800~1200 DEG C, the temperature-rise period time is 40~60min, to quartz ampoule
Heated；
4. after temperature reaches, hydrogen source is opened, triple valve is rotated to " hydrogen " position so that hydrogen enters mixing chamber
And in subsequent instrumentation；
5. connecting the gas circuit of gas chromatograph, gas chromatograph is opened；, when temperature, pressure, flow of gas chromatograph etc.
Parameter in normal range (NR) (i.e. in gas chromatograph injector temperature be 80~120 DEG C, 180~200 DEG C of the temperature of chromatographic column,
The temperature of detector is 200~250 DEG C, and nebulizer gas pressure be 0.395~0.405MPa, the flow of hydrogen be 30ml/min~
50ml/min), then control hydrogen decompression pressure regulator to make total hydrogen pressure control in 2.0Mpa；
6. lighting the fid detector of gas chromatograph, and start computer record program and data processor；
7. six-way valve is rotated to Enrichment Mode, while enriching column is inserted in liquid nitrogen；
8. determine the sample of content carbon, and standard with microsyringe 20~100 microlitres of chlorosilanes of absorption of drying
Sample, from vaporizer；Injection port injection, start simultaneously at and clock；
9. after 10~20min, rotation six-way valve inserts enriching column to parse in boiling water and tested to analytical model；
10. detecting the peak area of methane by the program software record in computer, the response of standard sample is calculated；
11. continuously parallel sample introduction at least 2 times, until response relative deviation is less than 5%, averaging, standard sample is surveyed
Examination finishes；
12. draw 20~100 microlitres of chlorosilane samples, 8~step 11 of repeat step, combined standard sample with microscale sampler
The response and content of product, calculate total carbon content in sample；
13. end of operation, enriching column；From boiling water；In take out；By triple valve；" nitrogen " position is threaded to, is dropped to quartz ampoule
Temperature；Close hydrogen source；Close computer record program and data processor；Liquid nitrogen is refunded in liquid nitrogen biological container and preserved；When
Furnace tube temperature is down to less than 200 DEG C, closes source nitrogen.
As can be seen from the above embodiments, the above-mentioned example of the present invention realizes following technique effect：The present invention passes through chlorine
Carbon hydro-reduction in chlorine-containing silane is methane by silane reduction apparatus, and it is in gas chromatograph and right to be then sent into methane
Carbon content in methane is measured, it is achieved thereby that the total carbon content in detection chlorine-containing silane.
The preferred embodiments of the present invention are these are only, are not intended to limit the invention, for those skilled in the art
For member, the present invention can have various modifications and variations.Any modification within the spirit and principles of the invention, being made,
Equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (4)
1. a kind of detection method, it is characterised in that the detection method is using detecting system to the total carbon content in chlorine-containing silane
Detected,
The detecting system includes hydrogen feeding mechanism, inert gas feeding mechanism, vaporizer (3) and mixing chamber (4), the vapour
Changing room (3) has the injection port for being used for being passed through chlorosilane, the first entrance of the mixing chamber (4) and going out for the vaporizer (3)
Mouth is connected, and the outlet of the hydrogen feeding mechanism and the outlet of the inert gas feeding mechanism are connected in parallel in the mixed gas
The second entrance of room (4)；
The detecting system also includes being sequentially connected in series the chlorosilane reduction apparatus (6) of setting, removing means, methane adsorption desorption dress
Put, gas chromatograph (12) and data output device (13), and the entrance of the chlorosilane reduction apparatus (6) and the mixing chamber
(4) outlet, the removing means are used to remove hydrogen chloride and the unreacted chlorosilane,
The removing means includes the hydrogen chloride removing pipe (7) being sequentially connected and condenser, and the condenser includes filling liquid nitrogen
Condensing container and the dehydrating tube (8) that is placed in the liquid nitrogen,
The detection method comprises the following steps：
Step S1, the inert gas feeding mechanism in the detecting system is opened, the detecting system is entered using inert gas
Row gas displacement；
Step S2, the chlorosilane reduction apparatus (6) in the detecting system is warming up to preset temperature；
Step S3, hydrogen feeding mechanism, gas chromatograph (12) and the data output device (13) in the detecting system are opened,
And it is passed through hydrogen into the detecting system；
Step S4, the injection port into the detecting system is passed through chlorosilane, makes the chlorosilane and the hydrogen in the inspection
Chlorosilane reduction apparatus (6) reaction in examining system forms methane；
Step S5, the methane is adsorbed and is desorbed using the methane adsorption desorption device in the detecting system, and utilized
The gas chromatograph (12) carries out parsing test to the methane after desorption, while using the data output device (13)
The peak area of the methane is recorded,
The inert gas feeding mechanism include inert gas decompression pressure regulator (2), the outlet of the inert gas feeding mechanism,
Triple valve is provided between the outlet of the hydrogen feeding mechanism and the second entrance of the mixing chamber (4) in the detecting system
(5)；
In the step S1, adjust inert gas decompression pressure regulator (2) to 1~5MPa, and rotate the triple valve (5) with
Make the inert gas to 3~10min of gas displacement in the detecting system,
The hydrogen feeding mechanism includes hydrogen source and the hydrogen being connected with hydrogen source decompression pressure regulator (1), the gas
Chromatography (12) includes flame ionization ditector；
In the step S3, the hydrogen source is opened, and rotates the triple valve and causes hydrogen to enter the detecting system, then
The gas chromatograph (12) is opened, injector temperature is 80~120 DEG C into the gas chromatograph (12), the temperature of chromatographic column
180~200 DEG C of degree, the temperature of detector are 200~250 DEG C, the nebulizer gas pressure of the gas chromatograph (12) for 0.395~
0.405MPa, the flow of hydrogen is 30ml/min~50ml/min described in the gas chromatograph (12), and controls the hydrogen
Gas decompression pressure regulator (1) makes Hydrogen Vapor Pressure control in 2.0Mpa, finally lights the flame ionization ditector and starts institute
Data output device (13) is stated,
The chlorine-containing silane is reacted by the raw material including hydrogen and tetrachloro silicane to be formed, and the key component of the chlorine-containing silane is two
Chlorine dihydro silicon, trichlorosilane and silicon tetrachloride,
The detecting system also includes exhausting pipeline, and the exporting of the removing means, the entrance of the methane adsorption desorption device,
The exporting of the inert gas feeding mechanism, the outlet of the entrance of the gas chromatograph (12), the methane adsorption desorption device
It is linked in sequence with the exhausting pipeline on six-way valve (9)；When the six-way valve (9) is adjusted to Enrichment Mode, the removing dress
Between the outlet put and the entrance of the methane adsorption desorption device, the outlet of the inert gas feeding mechanism and the gas phase color
Turned between the entrance of spectrometer (12) and between the outlet of the methane adsorption desorption device and the exhausting pipeline；When described
When six-way valve (9) is adjusted to analytical model, between the outlet of the removing means and the exhausting pipeline, the methane adsorption desorption dress
Between the outlet of the entrance and the inert gas feeding mechanism put, the outlet of the methane adsorption desorption device and the gas phase color
Turned between the entrance of spectrometer (12),
The inert gas feeding mechanism is exported, is provided between the outlet of the hydrogen feeding mechanism and the second entrance
Triple valve (5),
The chlorosilane reduction apparatus (6) includes quartz ampoule and heater,
The methane adsorption desorption device includes filling the adsorption desorption container of solvent and the enriching column (10) being arranged in the solvent；
When the methane adsorption desorption device is used for adsorbed methane, the solvent is liquid nitrogen, when the methane adsorption desorption device is used to be desorbed
The solvent is boiling water during methane,
The hydrogen feeding mechanism includes hydrogen source and the hydrogen being connected with hydrogen source decompression pressure regulator (1)；It is described lazy
Property gas supply device include inert gas source and the inert gas that is connected with the inert gas source depressurizes pressure regulator (2)；
The gas chromatograph (12) includes flame ionization ditector；The data output device (13) is computer or data record
Device.
2. detection method according to claim 1, it is characterised in that
Removing means in the detecting system includes the hydrogen chloride removing pipe (7) being sequentially connected and condenser, the detection system
System also includes six-way valve (9), and the methane adsorption desorption device includes enriching column (10)；
In the step S2, the dehydrating tube (8) is inserted in the liquid nitrogen, the six-way valve (9) is adjusted to analytical model,
Then the chlorosilane reduction apparatus (6) is warming up to 800~1100 DEG C, the heating-up time is 40~60min.
3. detection method according to claim 2, it is characterised in that in the step S4, the six-way valve (9) is rotated
Inserted to Enrichment Mode, while the enriching column (10) in liquid nitrogen, then draw 20~100 microlitres using microsyringe
The vaporizer (3) that the chlorosilane enters in the detecting system.
4. detection method according to claim 2, it is characterised in that
In the step S5, after the injection port into the detecting system is passed through the 10~20min of chlorosilane, rotation described six
Port valve (9) inserts the enriching column (10) in boiling water to analytical model and carries out parsing test, while pass through the data output
Device (13) records the peak area of the methane；
After the step S5, the detection method also includes：The enriching column (10) is taken out from boiling water, described in rotation
Triple valve (5) is cooled with being passed through inert gas to the chlorosilane reduction apparatus (6)；Close the hydrogen feeding mechanism and
Data output device (13), and inert gas supply dress is closed when the chlorosilane reduction apparatus (6) is cooled to below 200 DEG C
Put.
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