CN109142575A - The detection method of Phosphine content in a kind of production of polysilicon hydrogen - Google Patents
The detection method of Phosphine content in a kind of production of polysilicon hydrogen Download PDFInfo
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- CN109142575A CN109142575A CN201811012882.8A CN201811012882A CN109142575A CN 109142575 A CN109142575 A CN 109142575A CN 201811012882 A CN201811012882 A CN 201811012882A CN 109142575 A CN109142575 A CN 109142575A
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- Prior art keywords
- hydrogen
- sample
- gas
- detection method
- polysilicon
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- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 57
- 239000001257 hydrogen Substances 0.000 title claims abstract description 57
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 41
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- 229910000073 phosphorus hydride Inorganic materials 0.000 title claims abstract description 34
- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 72
- 238000005070 sampling Methods 0.000 claims abstract description 31
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 26
- 239000010959 steel Substances 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 14
- 238000004817 gas chromatography Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 4
- 230000004044 response Effects 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 13
- 238000010790 dilution Methods 0.000 claims description 11
- 239000012895 dilution Substances 0.000 claims description 11
- 238000005516 engineering process Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005984 hydrogenation reaction Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 5
- 230000008859 change Effects 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002438 flame photometric detection Methods 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N2030/685—Electrical detectors flame photometry
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The present invention discloses a kind of detection method of Phosphine content in production of polysilicon hydrogen, comprising: is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, obtains sample gas；Directly using the content of hydrogen phosphide in flame luminosity gas chromatography test sample gas to get；Sample time is short, reduces the introducing of impurity, and obtained sample gas representativeness is good, improves working efficiency.
Description
Technical field
The present invention relates to technical field of polysilicon production, and in particular to Phosphine content in a kind of production of polysilicon hydrogen
Detection method.
Background technique
Hydrogen is a kind of indispensable raw materials for production, the production with polysilicon as the reducing agent in production of polysilicon
Cost is closely related with quality.Include: high-purity hydrogen as production of polysilicon hydrogen and is produced using improved Siemens
During polysilicon, hydrogen in reduction tail gas, hydrogenated tail gas is recycled by dry method solvent recovery technology from vent gas, what is obtained returns
Receive hydrogen；Wherein, high-purity hydrogen purity >=99.999%.Hydrogen phosphide in production of polysilicon hydrogen is in entire production of polysilicon
It is slowly enriched in the circulatory system of technique, and phosphorus, as the major impurity element in polysilicon, content is to polysilicon product
Quality has significant impact.And the prior art carries out analysis detection side to the Phosphine content in production of polysilicon tail gas recycle hydrogen
Method is less.
Summary of the invention
In view of this, this application provides a kind of detection method of Phosphine content in production of polysilicon hydrogen, sampling
Time is short, reduces the introducing of impurity, and obtained sample gas representativeness is good, improves working efficiency.
In order to solve the above technical problems, technical solution provided by the invention is hydrogen phosphide in a kind of production of polysilicon hydrogen
The detection method of content, comprising:
It is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, obtains sample gas；
Directly using the content of hydrogen phosphide in flame luminosity gas chromatography test sample gas to get.
Preferably, production of polysilicon is ppb grades with Phosphine content in hydrogen.
Preferably, the sampling steel cylinder sample time of each coating of PTFE containing liner is 10min.
Preferably, the sampling steel cylinder sampling amount of each coating of PTFE containing liner is 300mL.
Preferably, the production of polysilicon is high-purity hydrogen that purity is 99.999% or the mistake for producing polysilicon with hydrogen
Cheng Zhong recycles hydrogen in reduction tail gas, hydrogenated tail gas by dry method solvent recovery technology from vent gas, obtained recycling hydrogen.
Preferably, the flame luminosity gas chromatography detection process instrument condition are as follows: detector: flame photometric detection
Device, 140 DEG C of detector temperature, pressure precision 0.001psi；Carrier gas: hydrogen, flow 15mL/.min~20mL/.min；It is quantitative
Ring: inertia quantitative loop, quantitative loop volume 1mL；Chromatographic column: 60~70 DEG C of column temperature, stainless stee l packed column, long 2m, diameter 3mm.
Preferably, the chromatographic column is porapad-Q stainless stee l packed column.
Preferably, the detection method specifically includes:
Sampling: it is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, after obtaining sampling
Steel cylinder, acquisition has sample gas in the steel cylinder after the sampling；
Calibration: calibrating gas uses on-line dilution instrument and six-way valve sample introduction, and flame luminosity type gas chromatograph measures standard
The response peak area of hydrogen phosphide in sample repeats sample introduction twice, when two times result deviation is less than 5%, obtains in standard sample
The response average value peak area of hydrogen phosphide；
Measurement: steel cylinder after the sampling connects flame luminosity type gas chromatograph, the sample gas through six-way valve into
Sample, flame luminosity type gas chromatograph measure the response peak area of hydrogen phosphide in sample gas, repeat sample introduction twice, tie twice
When fruit deviation is less than 5%, the response average value peak area of hydrogen phosphide in sample gas is obtained；
Being calculated as follows to obtain Phosphine content in sample gas is Phosphine content in production of polysilicon hydrogen；
Φ i=Φ s × Ai/As
Φ i: Phosphine content in sample gas；
Φ s: Phosphine content in standard sample；
Ai: the response average value peak area of hydrogen phosphide in sample gas；
As: the response average value peak area of hydrogen phosphide in standard sample.
Preferably, the calibration process specifically includes: on-line dilution instrument is connect with flame luminosity type gas chromatograph, is used
The calibrating gas that the on-line dilution instrument obtains measures phosphorus in standard sample through six-way valve sample introduction, flame luminosity type gas chromatograph
Change the response peak area of hydrogen, repeat sample introduction twice, when two times result deviation is less than 5%, obtains hydrogen phosphide in standard sample
Respond average value peak area.
Preferably, the continuous mode specifically includes: the steel cylinder after the sampling connects flame luminosity type gas chromatograph,
The valve between steel cylinder and the flame luminosity type gas chromatograph after opening the sampling, the sample gas is directly through six
Port valve sample introduction, flame luminosity type gas chromatograph measure the response peak area of hydrogen phosphide in sample gas, repeat sample introduction twice,
When two times result deviation is less than 5%, the response average value peak area of hydrogen phosphide in sample gas is obtained；
Being calculated as follows to obtain Phosphine content in sample gas is Phosphine content in production of polysilicon hydrogen；
Φ i=Φ s × Ai/As
Φ i: Phosphine content in sample gas；
Φ s: Phosphine content in standard sample；
Ai: the response average value peak area of hydrogen phosphide in sample gas；
As: the response average value peak area of hydrogen phosphide in standard sample.
Preferably, the standard sample is made of hydrogen phosphide and hydrogen, and Phosphine content is 5ppb in the standard sample.
Preferably, the standard sample is obtained using on-line dilution instrument with diluted in hydrogen by standard preparation sample；It is described by
Standard prepares sample and is made of hydrogen phosphide and hydrogen, and Phosphine content is 10ppm in the standard sample.
Compared with prior art, detailed description are as follows by the application:
The present invention provides a kind of detection method of Phosphine content in production of polysilicon hydrogen, PTFE coating is poly- four
Vinyl fluoride coating obtains non-adhering surfaces, prevents the absorption of microelement, improve the antiseptic property of sampler, using containing liner
The sampling steel cylinder of PTFE coating is as samplers sample production of polysilicon hydrogen, and sample time is short, and step is simple, reduces impurity
Introducing, sample is stablized, representative good, improves working efficiency, is adopted especially relative to using the absorption bottle with absorbing liquid
Collect sample gas, sample time is shorter, and step is simple, reduces the introducing of impurity, and sample is more stable, and representativeness is not glued more preferably
Surface.Further, since stablized using the sample gas sample that the above method collects, it is representative good, it can directly utilize flame
The content of hydrogen phosphide, does not need after sample gas is concentrated in the sample gas that the detection of luminosity gas chromatography collects
It is detected again, on the one hand refers to working efficiency, on the other hand, the fluctuation range of data is smaller, and the accuracy of data is higher,
The accuracy rate of detection is improved, and reduces the loss of testing cost and instrument.
Specific embodiment
It is right combined with specific embodiments below in order to make those skilled in the art more fully understand technical solution of the present invention
The present invention is described in further detail.
Embodiment 1
The detection method of Phosphine content in a kind of production of polysilicon hydrogen, comprising:
Sampling: it is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, after obtaining sampling
Steel cylinder, acquisition has sample gas in the steel cylinder after the sampling；
Calibration: on-line dilution instrument is connect with flame luminosity type gas chromatograph, the mark obtained using the on-line dilution instrument
For quasi- gas through six-way valve sample introduction, flame luminosity type gas chromatograph measures the response peak area of hydrogen phosphide in standard sample, weight
Multiple sample introduction twice, when two times result deviation is less than 5%, obtains the response average value peak area of hydrogen phosphide in standard sample；
Measurement: steel cylinder after the sampling connects flame luminosity type gas chromatograph, steel cylinder after opening the sampling and
Valve between the flame luminosity type gas chromatograph, the sample gas is directly through six-way valve sample introduction, flame luminosity type gas
Chromatography measures the response peak area of hydrogen phosphide in sample gas, repeats sample introduction twice, two times result deviation is less than 5%
When, obtain the response average value peak area of hydrogen phosphide in sample gas；
Being calculated as follows to obtain Phosphine content in sample gas is Phosphine content in production of polysilicon hydrogen；
Φ i=Φ s × Ai/As
Φ i: Phosphine content in sample gas；
Φ s: Phosphine content in standard sample；
Ai: the response average value peak area of hydrogen phosphide in sample gas；
As: the response average value peak area of hydrogen phosphide in standard sample；
Wherein, production of polysilicon is ppb grades with Phosphine content in hydrogen；The sampling of each coating of PTFE containing liner
Steel cylinder sample time is 10min, and the sampling steel cylinder sampling amount of each coating of PTFE containing liner is 300mL；The standard sample
Product are prepared sample by standard and are obtained using on-line dilution instrument with diluted in hydrogen；It is described that sample is prepared by hydrogen phosphide and hydrogen by standard
It forms, Phosphine content is 10ppm in the standard sample；Phosphine content is 5ppb in the obtained standard sample.
Above-mentioned detection method instrument and equipment:
Chromatograph: huge rock promise A91plus gas chromatograph；
Detector: commercially available flame photometric detector, 140 DEG C of detector temperature, pressure precision 0.001psi；
Six-way valve: commercially available electronic automatic six-way valve, using U.S.'s RESTEK house journal Silcotek surface vacuum silane
Change coating technology (thickness of coating: 30nm-1.5um) and carry out surface inertness processing)；
Carrier gas: hydrogen, flow 15mL/.min~20mL/.min；
Quantitative loop: commercially available inertia quantitative loop, quantitative loop volume 1mL；
Chromatographic column: 60~70 DEG C of column temperature, commercially available porapad-Q stainless stee l packed column, long 2m, diameter 3mm.
During using the high-purity hydrogen that purity is 99.999% as production of polysilicon hydrogen and production polysilicon
The recycling hydrogen arrived is respectively adopted above-mentioned detection method separately detect 11 times, as production of polysilicon hydrogen as a result such as table 1
It is shown.
Table 1
As shown in Table 1, the relative standard deviation (RSD) of detection method is 0.030%~0.056%, shows this
Method has good accuracy and precision.Hydrogen phosphide in production of polysilicon hydrogen can be accurately measured using this method to contain
Amount.
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
It also should be regarded as protection scope of the present invention into retouching.
Claims (10)
1. the detection method of Phosphine content in a kind of production of polysilicon hydrogen characterized by comprising
It is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, obtains sample gas；
Directly using the content of hydrogen phosphide in flame luminosity gas chromatography test sample gas to get.
2. detection method according to claim 1, which is characterized in that production of polysilicon is with Phosphine content in hydrogen
Ppb grades.
3. detection method according to claim 1, which is characterized in that the sampling steel cylinder of each coating of PTFE containing liner
Sample time is 10min.
4. detection method according to claim 1, which is characterized in that the sampling steel cylinder of each coating of PTFE containing liner
Sampling amount is 300mL.
5. detection method according to claim 1, which is characterized in that the production of polysilicon is that purity is with hydrogen
During 99.999% high-purity hydrogen or production polysilicon, by dry method solvent recovery technology from vent gas to reduction tail gas, hydrogenation tail
Hydrogen is recycled in gas, obtained recycling hydrogen.
6. detection method according to claim 1, which is characterized in that the flame luminosity gas chromatography detection process instrument
Device condition are as follows: detector: flame photometric detector, 140 DEG C of detector temperature, pressure precision 0.001psi；Carrier gas: hydrogen, stream
Measure 15mL/.min~20mL/.min；Quantitative loop: inertia quantitative loop, quantitative loop volume 1mL；Chromatographic column: 60~70 DEG C of column temperature, no
Become rusty steel packed column, long 2m, diameter 3mm.
7. detection method according to claim 1, which is characterized in that the detection method specifically includes:
Sampling: it is acquired production of polysilicon hydrogen using the sampling steel cylinder of the coating of PTFE containing liner, the steel after being sampled
Bottle, acquisition has sample gas in the steel cylinder after the sampling；
Calibration: calibrating gas uses on-line dilution instrument and six-way valve sample introduction, and flame luminosity type gas chromatograph measures standard sample
The response peak area of middle hydrogen phosphide repeats sample introduction twice, when two times result deviation is less than 5%, obtains phosphatization in standard sample
The response average value peak area of hydrogen；
Measurement: the steel cylinder after the sampling connects flame luminosity type gas chromatograph, and the sample gas is through six-way valve sample introduction, fire
Flame luminosity classes gas chromatograph measures the response peak area of hydrogen phosphide in sample gas, repeats sample introduction twice, two times result is inclined
When difference is less than 5%, the response average value peak area of hydrogen phosphide in sample gas is obtained；
Being calculated as follows to obtain Phosphine content in sample gas is Phosphine content in production of polysilicon hydrogen；
Φ i=Φ s × Ai/As
Φ i: Phosphine content in sample gas；
Φ s: Phosphine content in standard sample；
Ai: the response average value peak area of hydrogen phosphide in sample gas；
As: the response average value peak area of hydrogen phosphide in standard sample.
8. detection method according to claim 7, which is characterized in that the calibration process specifically includes: on-line dilution instrument
It is connect with flame luminosity type gas chromatograph, the calibrating gas obtained using the on-line dilution instrument is through six-way valve sample introduction, flame
Luminosity classes gas chromatograph measures the response peak area of hydrogen phosphide in standard sample, repeats sample introduction twice, two times result deviation
When less than 5%, the response average value peak area of hydrogen phosphide in standard sample is obtained.
9. detection method according to claim 7, which is characterized in that the standard sample is made of hydrogen phosphide and hydrogen,
Phosphine content is 5ppb in the standard sample.
10. detection method according to claim 9, which is characterized in that the standard sample prepares sample by standard and uses
On-line dilution instrument is obtained with diluted in hydrogen；It is described to be made of standard preparation sample hydrogen phosphide and hydrogen, in the standard sample
Phosphine content is 10ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811012882.8A CN109142575A (en) | 2018-08-31 | 2018-08-31 | The detection method of Phosphine content in a kind of production of polysilicon hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811012882.8A CN109142575A (en) | 2018-08-31 | 2018-08-31 | The detection method of Phosphine content in a kind of production of polysilicon hydrogen |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2799116B2 (en) * | 1993-01-08 | 1998-09-17 | 大陽東洋酸素株式会社 | Method and apparatus for highly sensitive analysis of impurities in gaseous hydride |
| CN203811587U (en) * | 2014-04-22 | 2014-09-03 | 福建中烟工业有限责任公司 | A device for determining residual phosphine in a sample |
| CN203870077U (en) * | 2014-05-21 | 2014-10-08 | 华南理工大学 | Secondary cold trap enrichment device and GC-FID (Gas Chromatography-Flame Ionization Detector) combined device for detecting trace phosphine |
| CN106526015A (en) * | 2016-10-28 | 2017-03-22 | 中国南玻集团股份有限公司 | Apparatus for detecting trace phosphor impurity in hydrogen and detection method thereof |
-
2018
- 2018-08-31 CN CN201811012882.8A patent/CN109142575A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2799116B2 (en) * | 1993-01-08 | 1998-09-17 | 大陽東洋酸素株式会社 | Method and apparatus for highly sensitive analysis of impurities in gaseous hydride |
| CN203811587U (en) * | 2014-04-22 | 2014-09-03 | 福建中烟工业有限责任公司 | A device for determining residual phosphine in a sample |
| CN203870077U (en) * | 2014-05-21 | 2014-10-08 | 华南理工大学 | Secondary cold trap enrichment device and GC-FID (Gas Chromatography-Flame Ionization Detector) combined device for detecting trace phosphine |
| CN106526015A (en) * | 2016-10-28 | 2017-03-22 | 中国南玻集团股份有限公司 | Apparatus for detecting trace phosphor impurity in hydrogen and detection method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王敢峰等: "火焰光度气相色谱法测定空气中磷化氢的规范化研究", 《卫生研究》 * |
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