CN108318592A - The detection device and detection method of trace silane in a kind of production of polysilicon tail gas - Google Patents
The detection device and detection method of trace silane in a kind of production of polysilicon tail gas Download PDFInfo
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- CN108318592A CN108318592A CN201810006973.4A CN201810006973A CN108318592A CN 108318592 A CN108318592 A CN 108318592A CN 201810006973 A CN201810006973 A CN 201810006973A CN 108318592 A CN108318592 A CN 108318592A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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Abstract
The present invention provides the detection device and detection method of trace silane in a kind of production of polysilicon tail gas, belongs to production of polysilicon detection technique field.The injection port of detection device, the first chromatographic column, the second chromatographic column and detector are sequentially communicated, and control valve is set to the connection and disconnection for controlling the first chromatographic column and the second chromatographic column between the first chromatographic column and the second chromatographic column.Detection method is first to be passed through the first chromatographic column from injection port with quantitative production of polysilicon tail gas, after detector detects that silane peak has gone out, adjusting control valve makes the separated of the first chromatographic column and the second chromatographic column, silane peak and standard silane peak are compared, the amount of trace silane in production of polysilicon tail gas is calculated.Testing result using the detection method of above-mentioned detection device is more accurate, eliminates the other impurities gas in tail gas, such as：Hydrogen chloride, chlorosilane etc., avoid foreign gas from entering detector, keep the detection of silane more accurate, reliable, reproducible.
Description
Technical field
The present invention relates to production of polysilicon detection technique fields, in particular to trace in a kind of production of polysilicon tail gas
Measure the detection method of silane.
Background technology
With the rapid development of solar energy industry, demand of the whole world to polysilicon is growing, domestic and international large polycrystalline silicon
Manufacturer continuously improves production technology and enhances production capacities, and takes Optimizing Process Parameters, reduces energy consumption, reduces cost, maximum can
It can recycle in tail gas using ingredient, improve in Siemens's polysilicon production process, trichlorosilane synthesis, high temperature hydrogenation and polycrystalline
The processes such as Si reduction have a large amount of tail gas to generate, and main component has H in tail gas2、HCl、SiHCl3、SiH2Cl2、SiCl4, remove this
Except also have SiH4In the presence of main component uses Dry recovery technology, leads to pressurization condensation, the technologies such as gas-liquid separation, absorption and sorption
The above component is separated and recovered, return system uses.Because of the SiH contained in tail gas4Property is active, meets air burning, sampling point
If silane contents are higher when constituent content in analysis detection tail gas certain measure is not taken there are certain danger, for this purpose,
Silane contents in tail gas need to be carried out with quantitative analysis and take corresponding precautionary measures.
In the prior art, the device and method for quantitative detection accurately not being carried out to silane contents to tail gas.
Invention content
The purpose of the present invention is to provide a kind of detection devices of trace silane in production of polysilicon tail gas, can accurately examine
Silane contents in tail gas are surveyed, keep testing result more accurate, reliable.
Another object of the present invention is to provide a kind of detection method of trace silane in production of polysilicon tail gas, Neng Gouzhun
Really silane contents in detection tail gas, keep testing result more accurate, reliable, reproducible.
Realization that the present invention adopts the following technical solutions：
The detection device of trace silane in a kind of production of polysilicon tail gas, is suitable for gas chromatograph, including injection port, the
One chromatographic column, the second chromatographic column, control valve and detector, injection port, the first chromatographic column, the second chromatographic column and detector connect successively
Logical, control valve is set between the first chromatographic column and the second chromatographic column for controlling being connected to for the first chromatographic column and the second chromatographic column
With disconnection.
Further, in preferred embodiments of the present invention, above-mentioned control valve is ten-way valve, and there are two types of connected states for ten-way valve tool
State, the first connected state make the outlet of the first chromatographic column be connected to the injection port of the second chromatographic column, second of connected state
The injection port of the outlet and the second chromatographic column that make the first chromatographic column disconnects.
Further, in preferred embodiments of the present invention, above-mentioned detection device further includes quantitative loop, and quantitative loop is set to ten
Port valve, when ten-way valve is located under the first connected state, quantitative loop is connected to the first chromatographic column.
The detection method of trace silane in a kind of production of polysilicon tail gas, is suitable for above-mentioned detection device, with quantitative more
Crystal silicon production tail gas is first passed through the first chromatographic column from injection port, and adjusting control valve brings detector by carrier gas, when detector detects
After having gone out to silane peak, adjusting control valve makes the separated of the first chromatographic column and the second chromatographic column, by silane peak and standard silicon
Alkane peak compares, and the amount of trace silane in production of polysilicon tail gas is calculated.
Further, in preferred embodiments of the present invention, production of polysilicon tail gas includes silane, hydrogen chloride and chlorosilane.
Further, in preferred embodiments of the present invention, quantitative production of polysilicon tail gas samples as follows：Make
Production of polysilicon tail gas is sampled with quantitative loop.
Further, in preferred embodiments of the present invention, above-mentioned quantitative loop volume is 1ml.
Further, in preferred embodiments of the present invention, above-mentioned first chromatographic column and the second chromatographic column it is separated after, make
Input end of the carrier gas from the outlet end of the first chromatographic column towards the first chromatographic column flows.
Further, in preferred embodiments of the present invention, above-mentioned carrier gas is nitrogen.
Further, it in preferred embodiments of the present invention, obtains standard silane peak and carries out as follows：By standard silicon
Alkane is passed through the first chromatographic column, the second chromatographic column and detector from injection port successively, and detection obtains standard silane peak.
The advantageous effect of the detection device of trace silane in the production of polysilicon tail gas that presently preferred embodiments of the present invention provides
It is：The first chromatographic column is connected to the second chromatographic column first, production of polysilicon tail gas is passed through the first chromatographic column from injection port and passes through
First chromatography post separation, the silane in production of polysilicon tail gas enter after first passing through the second chromatographic column in detector, work as detection
After device detects that silane peak has gone out, adjusting control valve makes the separated of the first chromatographic column and the second chromatographic column, and polysilicon is allowed to give birth to
Produce tail gas in other impurities gas (such as：Hydrogen chloride and chlorosilane) it cannot be by the second chromatographic column, foreign gas being avoided to enter
In detector, the service life of detector is extended, and keeps testing result more accurate, reliable.
The advantageous effect of the detection method of trace silane in the production of polysilicon tail gas that presently preferred embodiments of the present invention provides
It is：It first is passed through the first chromatographic column from injection port with quantitative production of polysilicon tail gas, adjusting control valve brings detection by carrier gas
Device, after detector detects that silane peak has gone out, then adjusting control valve makes the separated of the first chromatographic column and the second chromatographic column,
Allow in production of polysilicon tail gas other impurities gas (such as：Hydrogen chloride and chlorosilane) it cannot be by the second chromatographic column, avoiding miscellaneous
Matter gas enters the influence to silane detection data in detector, keeps the testing result of silane more accurate, reliable, repeated
It is good, and the sensitivity of Protective Detector is not influenced by hydrolyzing chlorosilane object, extends the service life of detector.Examination criteria
Silane sample obtains peak area/peak height of standard silane, and silane peak area/peak height and standard silane peak area/peak height are compared,
The amount of trace silane in production of polysilicon tail gas is calculated, wherein computational methods are：
In formula：φ --- the content of silane, ppm in sample gas；
φ s --- the content of silane, ppm in standard sample；
A (or h) --- the peak area (u V.s) or peak height (u V) of silane in sample；
As (or hs) --- the peak area (u V.s) or peak height (u V) of silane in standard sample.
The exact value of trace silane in production of polysilicon tail gas is obtained by the detection method, keeps testing result more accurate
Really, also, extend detector service life.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings and also belong to protection scope of the present invention.
Fig. 1 is the first connection schematic diagram of ten-way valve in the present invention；
Fig. 2 is second of connection schematic diagram of ten-way valve in the present invention.
Icon：110- injection ports；120- sample gas exports；130- quantitative loops；The first chromatographic columns of 140-；The second chromatographies of 150-
Column；160- detectors；170- ten-way valves.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The detection device to trace silane in the production of polysilicon tail gas of the embodiment of the present invention and detection method carry out below
It illustrates.
Embodiment
The detection device of trace silane in production of polysilicon tail gas is suitable for gas chromatograph, passes through gas chromatograph pair
Trace silane is detected in production of polysilicon tail gas, and testing result is more accurate, is conducive to our research.
The detection device of trace silane includes injection port 110, the first chromatographic column 140, the second color in production of polysilicon tail gas
Compose column 150, control valve and detector 160, injection port 110, the first chromatographic column 140, the second chromatographic column 150 and detector 160 according to
Secondary connection, control valve are set between the first chromatographic column 140 and the second chromatographic column for controlling the first chromatographic column 140 and the second color
Compose the connection and disconnection of column 150.
The first chromatographic column 140 is connected to the second chromatographic column 150 first, production of polysilicon tail gas is passed through from injection port, is adjusted
Control valve is saved, is brought into the first chromatographic column 140 by carrier gas 1 and is detached by the first chromatographic column 140, the silicon in production of polysilicon tail gas
Alkane enters after first passing through the second chromatographic column 150 in detector 160, after detector 160 detects that silane peak has gone out, then adjusts
Section control valve makes the separated of the first chromatographic column 140 and the second chromatographic column 150, allows other impurities gas in production of polysilicon tail gas
(such as：Hydrogen chloride and chlorosilane) it cannot enter in the second chromatographic column 150, it avoids foreign gas from entering in detector 160, extends
The service life of detector 160, and keep testing result more accurate, reliable.
In the present embodiment, control valve is used to control sample displacement and controls the first chromatographic column 140 and the second chromatographic column 150
Connection and disconnection, control valve are ten-way valve 170, and for the tool of ten-way valve 170 there are two types of connected state, the first connected state makes the first color
The outlet of spectrum column 140 is connected to the injection port of the second chromatographic column 150, and second of connected state makes going out for the first chromatographic column 140
Sample mouth and the injection port of the second chromatographic column 150 disconnect.When being detected, first by the first chromatographic column 140 and the second chromatography
Column 150 is connected to, and so that tail gas is entered the second chromatographic column 150 from the first chromatographic column 140, is entered back into detector 160, detector 160
After detection, work station will appear silane spectrogram peak, when silane peak all after rolling, then by switching ten-way valve 170, make the
One chromatographic column 140 and the second chromatographic column 150 disconnect, and remaining hydrogen chloride and chlorosilane gas cannot be into the first chromatographic column 140
Enter in the second chromatographic column 150 and detector 160, foreign gas is avoided to enter in detector 160, extends making for detector 160
With the service life, and keep testing result more accurate, reliable.
Detection device further includes quantitative loop 130, and quantitative loop 130 is set to ten-way valve 170, when ten-way valve 170 is located at first
When under kind connected state, quantitative loop 130 is connected to the first chromatographic column 140.It is sampled with quantitative loop 130, completes sample displacement,
So as to quantitative detection be carried out to trace silane in production of polysilicon tail gas, to keep testing result more accurate.
The detection method of trace silane in production of polysilicon tail gas is suitable for above-mentioned detection device, with quantitative polysilicon
Production tail gas is first passed through from injection port, and adjusting control valve brings the first chromatographic column 140 by carrier gas 1, when detector 160 detects silicon
After alkane peak has gone out, then adjusting control valve makes the separated of the first chromatographic column 140 and the second chromatographic column 150, by silane peak and mark
Eka-silicon alkane peak compares, and the amount of trace silane in production of polysilicon tail gas is calculated.
It is first passed through from the injection port with quantitative production of polysilicon tail gas, adjusting control valve brings described the by carrier gas 1
One chromatographic column 140 after the detector 160 detects that silane peak has gone out, then adjusts the control valve and makes first color
Compose the separated of column 140 and second chromatographic column 150, allow in production of polysilicon tail gas other impurities gas (such as：Hydrogen chloride and
Chlorosilane) it cannot enter in the second chromatographic column 150, it avoids foreign gas from entering in detector 160, extends detector 160
Service life.The silane peak and standard silane peak are compared, the amount of trace silane in production of polysilicon tail gas is calculated, only
It needs to be detected silane, avoids influence of other gases to silane detection data in tail gas, make the testing result of silane
It is more accurate, reliable, reproducible, and the sensitivity of Protective Detector 160 is not influenced by hydrolyzing chlorosilane object, extends detection
The service life of device 160.
Production of polysilicon tail gas includes silane, hydrogen chloride and chlorosilane.In order to more accurately carry out quantitative inspection to silane
It surveys, then hydrogen chloride and chlorosilane is separated, keep the testing result of silane more accurate.In the present embodiment, three kinds of gases, inspection
Silane elder generation appearance when survey, hydrogen chloride and chlorosilane while afterwards appearance, the i.e. appearance time at silane peak are 0.9min, hydrogen chloride and chlorine
The appearance time of silane is 2.4min, and the two appearance interval time is longer, can have time enough to carry out cutting for ten-way valve 170
It changes, to avoid hydrogen chloride and chlorosilane from entering in the second chromatographic column 150.
In the present invention, gas chromatograph is Chongqing river instrument gas chromatograph, and is detected using flame photometric detector,
Its detection data is more accurate, and flame photometric detector, which is burnt by sample in air and hydrogen flame burner, to be examined
It surveys.
Quantitative production of polysilicon tail gas samples as follows：Production of polysilicon tail gas is sampled using quantitative loop 130,
To carry out quantitative detection to trace silane in production of polysilicon tail gas.Preferably, 130 volume of quantitative loop is 1ml.
First chromatographic column 140 and the second chromatographic column 150 it is separated after, make carrier gas 2 from the outlet end of the first chromatographic column 140
It is flowed towards the input end of the first chromatographic column 140.By remaining hydrogen chloride in the first chromatographic column 140 and chlorosilane gas discharge the
One chromatographic column 140 avoids to separate at the first chromatographic column 140 when subsequent detection subsequently to carry out second of detection
Gas is passed through in the second chromatographic column 150.
Acquisition standard silane peak carries out as follows：Standard silane is passed through from injection port, adjusting control valve is by carrying
Gas 1 is brought into and is passed through the first chromatographic column 140, the second chromatographic column 150 and detector 160 successively, and detection obtains standard silane peak.
In the present embodiment, the flowing of gas is pushed by carrier gas, carrier gas is nitrogen, and indwelling is in the first chromatographic column 140
Other impurities gas is discharged by carrier gas.
In the present invention, the first chromatographic column 140 and the second chromatographic column 150 are Porapak Q columns, and 13 X molecular sieve column is internal diameter
The stainless steel column for being 1.2m for 3mm, length.The shape of its chromatographic column is identical as existing gas-chromatography post shapes, not to its into
Row improves.
Comprising the concrete steps that when detection：
1, it presses instrumentation regulation and opens instrument, setting instrument parameters to instrumental baseline are stablized.
Wherein, the parameter set as：
Air mass flow is：80mL/min
Hydrogen flowing quantity is：60mL/min
Nitrogen flow is：30mL/min
The post case temperature of first chromatographic column 140 and the second chromatographic column 150：50℃.
Flame photometric detector temperature：150℃
High pressure is set as：400V
2, the production of polysilicon tail gas that sampling bag is collected into first is entered into ten-way valve 170 as sample from injection port 110
In, such as Fig. 1, bold portion is connected between representing each valve, and dotted portion expression is not connected to, when at sample to injection port 110, is passed through
Nitrogen makes sample circulation in ten-way valve 170 as carrier gas.Sample first brings ten-way valve 170 at injection port 110 by carrier gas
The positions 9#, sample gas arrives the positions 7# by the positions 9# to the positions 10#, the positions 10# by 1mL quantitative loops 130 when displacement, then by the positions 7#
To the positions 8#, by the positions 8# from 120 discharge of sample gas outlet, in this way, being completed after so that production of polysilicon tail gas is passed through ten-way valve 170
Displacement to quantitative loop 130, ten-way valve 170 control sample into line replacement, indwelling 1ml production of polysilicon tails in quantitative loop 130
Gas.
After in sample indwelling 1ml quantitative loops 130, ten-way valve 170 is rotated, connected component becomes not connect between each valve
Logical, non-connected component becomes to be connected to, i.e., solid line becomes dotted line, and dotted line becomes solid line, such as Fig. 2, and carrier gas 1 is entered to from the positions 1#
The positions 10#, the positions 10# take the sample in quantitative loop 130 out of during entering the positions 7#, then enter 6# from the positions 7#
Set, the positions 6# enter the positions 3# after entering the first chromatographic column 140, and the positions 3# enter the positions 2#, from the gas that the positions 2# come out into
Enter in flame photometric detector.Wherein, flame photometric detector is burnt by sample in air and hydrogen flame burner internal combustion
Row detection.
Wherein, after sample enters the first chromatographic column 140, the various gases in sample can detach, and silane enters
Second chromatographic column 150 enters detector 160, will detect that peak, check work station, when occurring silane peak on work station afterwards
Wait, i.e., the time be 0.9-1min (such as：0.9min, 0.95min or 1min) when the peak that occurs, when silane peak all after rolling, turn
Dynamic ten-way valve 170, makes other impurities gas (such as：Hydrogen chloride, chlorosilane) indwelling is in the first chromatographic column 140, first from 2#
The gas for setting out is that silane enters in detector 160, detects the peak of silane in production of polysilicon tail gas, and calculate appearance
Peak area or peak height.
Other impurities gas is (such as：Hydrogen chloride, chlorosilane) indwelling is in the first chromatographic column 140, due to having rotated ten-way valve
170, connected component becomes not to be connected between making each valve, and non-connected component becomes to be connected to, i.e., solid line becomes dotted line, and dotted line becomes real
Line, such as Fig. 1, the other impurities gas in the first chromatographic column 140 is (such as：Hydrogen chloride, chlorosilane) it is entered to from the positions 4# by carrier gas 2
The positions 3#, (such as by the other impurities gas in the first chromatographic column 140：Hydrogen chloride, chlorosilane) positions 6# are blown to, then by the positions 6#
Into the positions 5#, from the positions 5# by other impurities gas (such as：Hydrogen chloride, chlorosilane) gas is expelled in exhaust collection bottle and inhales
It receives.Influence of other gases to silane detection data in tail gas is avoided, avoids foreign gas from entering flame photometric detector, makes
The detection of silane is more accurate, reliable, reproducible, and protects flame photometric detector not by the increase shadow of silicane hydrolysate
Ring its sensitivity.
3, flame photometric detector examination criteria silane gas is reused to carry out as follows：Standard silane is passed through
It in ten-way valve 170, is sampled by quantitative loop 130, then the standard silane in quantitative loop 130 is passed through flame photometric detector
In be detected.
Specifically, first the standard silane that sampling bag is collected into is entered from from injection port 110 in ten-way valve 170, such as Fig. 1,
Bold portion is connected between representing each valve, and dotted portion expression is not connected to, when at standard silane to injection port 110, passes through nitrogen
As carrier gas, make sample circulation in ten-way valve 170.Standard silane first brings ten-way valve 170 at injection port 110 by carrier gas
The positions 9#, sample gas arrives the positions 7# by the positions 9# to the positions 10#, the positions 10# by 1mL quantitative loops 130 when displacement, then by the positions 7#
To the positions 8#, by the positions 8# from 120 discharge of sample gas outlet, in this way, entering quantitative loop after so that standard silane is passed through ten-way valve 170
130, complete the displacement of quantitative loop, ten-way valve 170 controls sample into line replacement, indwelling 1ml standard silane in quantitative loop 130.
After in standard silane indwelling 1ml quantitative loops 130, ten-way valve 170 is rotated, connected component becomes not between each valve
Connection, non-connected component become to be connected to, i.e., solid line becomes dotted line, and dotted line becomes solid line, such as Fig. 2, and carrier gas 1 is entered to from the positions 1#
The positions 10#, the positions 10# take the standard silane in quantitative loop 130 out of during entering the positions 7#, then enter 6# from the positions 7#
Position, the positions 6# enter the positions 3# after entering the first chromatographic column 140, and the positions 3# enter the positions 2#, the gas come out from the positions 2#
Into the second chromatographic column 150, enters in detector 160 afterwards, detect the peak of standard silane, and calculate the peak area or peak of appearance
It is high.
4, the content of trace silane in production of polysilicon tail gas is finally calculated according to formula, wherein calculation formula is：
In formula：φ --- the content of silane, ppm in sample gas；
φ s --- the content of silane, ppm in standard sample；
A (or h) --- the peak area (u V.s) or peak height (u V) of silane in sample；
As (or hs) --- [peak area (u V.s) or the peak height (u V) of silane in standard sample.
The exact value of trace silane in production of polysilicon tail gas is obtained by the detection method, it is only necessary to be examined to silane
It surveys, avoids influence of other gases to silane detection data in tail gas, avoid foreign gas from entering detector 160, make silane
Detection it is more accurate, reliable, reproducible, and not influenced its by the increase of silicane hydrolysate sensitive for Protective Detector 160
Degree, does not influence the service life of detector 160.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. the detection device of trace silane in a kind of production of polysilicon tail gas is suitable for gas chromatograph, which is characterized in that including
Injection port, the first chromatographic column, the second chromatographic column, control valve and detector, the injection port, first chromatographic column, described
Two chromatographic columns and the detector are sequentially communicated, the control valve be set to first chromatographic column and second chromatographic column it
Between for controlling the connection and disconnection of first chromatographic column and second chromatographic column.
2. detection device according to claim 1, which is characterized in that the control valve is ten-way valve, the ten-way valve tool
There are two types of connected state, the first connected state makes the injection port of the outlet and second chromatographic column of first chromatographic column
Connection, second of connected state make the outlet of first chromatographic column be disconnected with the injection port of second chromatographic column.
3. detection device according to claim 2, the detection device further includes quantitative loop, and the quantitative loop is set to institute
Ten-way valve is stated, when the ten-way valve is located under the first described connected state, the quantitative loop connects with first chromatographic column
It is logical.
4. the detection method of trace silane in a kind of production of polysilicon tail gas is suitable for detection device described in claim 1,
It is characterized in that, first chromatographic column is first passed through from the injection port with quantitative production of polysilicon tail gas, adjusts the control
Valve brings detector by carrier gas, after the detector detects that silane peak has gone out, then adjusts the control valve and makes described
One chromatographic column is separated with second chromatographic column, and the silane peak and standard silane peak are compared, polysilicon is calculated
Produce the amount of trace silane in tail gas.
5. detection method according to claim 4, which is characterized in that the production of polysilicon tail gas includes silane, chlorination
Hydrogen and chlorosilane.
6. detection method according to claim 4, which is characterized in that quantitative production of polysilicon tail gas is as follows
Sampling：Production of polysilicon tail gas is sampled using quantitative loop.
7. detection method according to claim 6, which is characterized in that the quantitative loop volume is 1ml.
8. detection method according to claim 4, which is characterized in that first chromatographic column and second chromatographic column it
After separated, carrier gas is made to be flowed from the outlet end of first chromatographic column towards the input end of first chromatographic column.
9. detection method according to claim 8, which is characterized in that the carrier gas is nitrogen.
10. according to claim 4-9 any one of them detection methods, which is characterized in that obtain standard silane peak according to
As under type carries out：The standard silane is passed through first chromatographic column, second chromatographic column successively from the injection port
With the detector, detection obtains standard silane peak.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109507321A (en) * | 2018-11-28 | 2019-03-22 | 浙江博瑞电子科技有限公司 | A kind of method of special impurities detection sensitivity in raising high-purity hydrogen chloride |
| CN111289689A (en) * | 2018-12-07 | 2020-06-16 | 新疆新特新能材料检测中心有限公司 | Method and system for detecting content of each component in tail gas in polycrystalline silicon production |
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