CN105388230A - Dichlorosilane component detection method - Google Patents
Dichlorosilane component detection method Download PDFInfo
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- CN105388230A CN105388230A CN201510992381.0A CN201510992381A CN105388230A CN 105388230 A CN105388230 A CN 105388230A CN 201510992381 A CN201510992381 A CN 201510992381A CN 105388230 A CN105388230 A CN 105388230A
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- sealer
- detection method
- dichlorosilane
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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
- G01N30/06—Preparation
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
A dichlorosilane component detection method adopts a meteorological chromatography-mass spectrometry combined instrument to perform component detection, uses a sampling device in the detection process, wherein the sampling device comprises a sealing device and a water bath. By the adoption of the dichlorosilane component detection method, sample and air contact can be effectively avoided, and detection results are accurate.
Description
Technical field
The present invention relates to a kind of detection method of dichloro-dihydro silicon components.
Background technology
At present, dichlorosilane, in the semiconductor industry as epitaxial deposited silicon source, has the features such as rate of sedimentation is fast, epitaxial wafer thickness is even, is widely used.But because the trace impurity in dichlorosilane can bring harmful effect to semiconductor devices, harm is very large, and the trace impurity thus in dichlorosilane detects particularly important.Head-space sampler is one conveniently sample-pretreating method in vapor-phase chromatography, its principle is inserted by testing sample in an airtight container, by heat temperature raising, volatile constituent is evaporated from sample matrices, balance is reached in gas-liquid (or gas-solid) two-phase, direct extraction top gas carries out stratographic analysis, thus the composition of volatile constituent and content in check sample.Because dichlorosilane to suffocate smell and corrosive colourless toxic gas for having pungency at normal temperatures and pressures, boiling point (101.325kPa): 8.2 DEG C.Inflammable in air, the spontaneous combustion of more than 44 DEG C energy, hydrogen chloride and monox is generated after combustion oxidation, understand disintegrate when being heated to more than 100 DEG C and generate hydrogen chloride, chlorine, hydrogen and ambiguity silicon, also can produce corrosive fumes by disintegrate in soft air when imposing strong shock, meet water hydrolysis and generate hydrochloric acid and polysiloxane (SiH2O) 4.As can be seen from above, when carrying out dichloro-dihydro silico analysis, air must be completely cut off completely, and must carry out at low temperatures.Adopt traditional head-space sampler and extract its top gas by micro syringe and carry out stratographic analysis, this is the method adopted when more extensive detection, a kind of method for quick when dichloro-dihydro silicon components result only probably need be known, the method meeting ingress of air, cause metrical error, seem it is not very applicable when Water demand goes out component content in dichlorosilane.
Summary of the invention
The object of the invention is to overcome in prior art the problem of the metrical error caused because of ingress of air when adopting headspace sampling mode to analyze dichlorosilane composition, provide a kind of and can effectively avoid sample to contact with air, the detection method of testing result dichloro-dihydro silicon components accurately.
For realizing above object, technical solution of the present invention is: a kind of detection method of dichloro-dihydro silicon components, uses chromatography of gases-GC-MS to carry out component detection, employs sampling device in testing process, sampling device comprises sealer and water bath, comprises the following steps:
1) use nitrogen to carry out emptying process in sealer, nitrogen carries out purging 10 minutes to sealer inside, to drain the air in sealer completely;
2) the solid-state dichlorosilane via cooled with liquid nitrogen is put in sealer, extracting vacuum, make the vacuum tightness of sealer inside be 0Pa;
3) sealer is placed in water bath, the pure water of flowing is used to carry out water-bath, water temperature is between 0-25 DEG C, after the complete liquefy of solid-state dichlorosilane in device to be sealed, a small amount of liquid nitrogen is passed in water bath, make temperature control at about 0 DEG C, wait for 3-8 minute, make the gas-liquid in sealer reach balance;
4) pass into carrier gas pressurization with conduit, sample is along with carrier gas together sample introduction;
5) adopt Shimadzu GC-2014 type gas chromatograph, thermal conductivity detector (TCD) to carry out detection to sample introduction to analyze, wherein:
Chromatographic condition: RTX-VMS(30m*0.25mm*1.4 μm); Temperature: detecting device 200 DEG C, injection port 150 DEG C, column temperature 80 DEG C; Shunting mode sample introduction, split ratio: 10:1, sample introduction 10 μ l; Post flow: high-pure helium 2ml/min; Tail blows: high-pure helium 30ml/min;
6) sealer obtained after step 4) being sampled processes, and repeats step 3)-step 5), determine that it goes out peak position according to retention time, qualitative test.
Carrier gas in described step 4) is helium.
Water bath bottom described sampling device is provided with three conduits, one for importing liquid nitrogen, one for importing the pure water under normal temperature, one for draining; Sealer is provided with three conduits, one in order to access pure nitrogen, one for emptying, one for extracting vacuum.
Described conduit is stainless steel pipe.
Beneficial effect of the present invention is:
Employ a set of brand-new sampling device in this detection method, install three stainless steel pipes additional at bottom water bath, one for importing liquid nitrogen, one for importing the pure water under normal temperature, one for draining; Sealer installs three stainless steels additional, the nitrogen that an access is pure, when analyzing, first opening nitrogen conduit, opening evacuated tube for one, purge 10 minutes, drain the air in sealer completely for one for emptying for extracting vacuum.Again the solid-state dichlorosilane through cooled with liquid nitrogen is placed in sealer, extracting vacuum, reach after 0Pa until vacuum tightness, then sealer is placed in water bath, water-bath is carried out with the pure water of flowing, after solid-state dichlorosilane becomes liquid state completely, a small amount of liquid nitrogen is passed in water bath, temperature is made to control at about 0 DEG C, wait for about 5 minutes, after gas-liquid in sealer reaches balance, carrier gas pressurization is passed into conduit, sample is with carrier gas sample introduction, thus effectively avoid sample and contact with air, it also avoid because sample boiling point is too low, be difficult to process the situations such as the testing result caused is inaccurate.
Accompanying drawing explanation
Fig. 1 is the structure diagram of sampling device in the present invention.
In figure, sampling device 1, sealer 2, water bath 3, conduit 4.
Embodiment
Below in conjunction with accompanying drawing 1 and embodiment, the present invention is further detailed explanation:
A detection method for dichloro-dihydro silicon components, use chromatography of gases-GC-MS to carry out component detection, employ sampling device 1 in testing process, sampling device 1 comprises sealer 2 and water bath 3, comprises the following steps:
1) use nitrogen to carry out emptying process in sealer 2, nitrogen carries out purging 10 minutes to sealer 2 inside, to drain the air in sealer 2 completely;
2) the solid-state dichlorosilane via cooled with liquid nitrogen is put in sealer 2, extracting vacuum, make the vacuum tightness of sealer 2 inside be 0Pa;
3) sealer 2 is placed in water bath 3, the pure water of flowing is used to carry out water-bath, water temperature is between 0-25 DEG C, after the complete liquefy of solid-state dichlorosilane in device 2 to be sealed, a small amount of liquid nitrogen is passed in water bath 3, make temperature control at about 0 DEG C, wait for 3-8 minute, make the gas-liquid in sealer 2 reach balance;
4) pass into carrier gas pressurization with conduit 4, sample is along with carrier gas together sample introduction;
5) adopt Shimadzu GC-2014 type gas chromatograph, thermal conductivity detector (TCD) to carry out detection to sample introduction to analyze, wherein:
Chromatographic condition: RTX-VMS(30m*0.25mm*1.4 μm); Temperature: detecting device 200 DEG C, injection port 150 DEG C, column temperature 80 DEG C; Shunting mode sample introduction, split ratio: 10:1, sample introduction 10 μ l; Post flow: high-pure helium 2ml/min; Tail blows: high-pure helium 30ml/min;
6) sealer 2 obtained after step 4) being sampled processes, and repeats step 3)-step 5), determine that it goes out peak position according to retention time, qualitative test.
Carrier gas in described step 4) is helium.
Water bath 3 bottom described sampling device 1 is provided with 4, one, three conduits for importing liquid nitrogen, one for importing the pure water under normal temperature, one for draining; Sealer 2 is provided with 4, one, three conduits in order to access pure nitrogen, one for emptying, one for extracting vacuum.
Described conduit 4 is stainless steel pipe.
Employing a set of brand-new sampling device 1 in this detection method, installing 4, one, three conduits additional for importing liquid nitrogen at bottom water bath 3, one for importing the pure water under normal temperature, one for draining; Sealer 2 installs the pure nitrogen of 4, one, three conduits access additional, when analyzing, first opening nitrogen conduit, opening evacuated tube for one, purge 10 minutes, drain the air in sealer 2 completely for one for emptying for extracting vacuum.Again the solid-state dichlorosilane through cooled with liquid nitrogen is placed in sealer 2, extracting vacuum, reach after 0Pa until vacuum tightness, then sealer 2 is placed in water bath 3, water-bath is carried out with the pure water of flowing, after solid-state dichlorosilane becomes liquid state completely, a small amount of liquid nitrogen is passed in water bath 3, temperature is made to control at about 0 DEG C, wait for about 5 minutes, after gas-liquid in sealer 2 reaches balance, carrier gas pressurization is passed into conduit 4, sample is with carrier gas sample introduction, thus effectively avoid sample and contact with air, it also avoid because sample boiling point is too low, be difficult to process the situations such as the testing result caused is inaccurate.Also need in this method to use dichlorosilane (chromatographically pure), Trichloromethyl silane (chromatographically pure), dimethyldichlorosilane (chromatographically pure) is as standard substance, identical with the using method in traditional detection method.Trichloromethyl silane and dimethyldichlorosilane two kinds of materials are impurity common in dichlorosilane, and be mainly used to carry out qualitative to impurity peaks in dichlorosilane, carrier gas is helium.Dichlorosilane (chromatographically pure) effect is that to carry out contrast with the retention of standard substance to sample qualitative.The present invention can effectively avoid sample to contact with air, testing result is accurate.
Claims (4)
1. a detection method for dichloro-dihydro silicon components, use chromatography of gases-GC-MS to carry out component detection, employ sampling device (1) in testing process, sampling device (1) comprises sealer (2) and water bath (3), comprises the following steps:
1) use nitrogen to carry out emptying process in sealer (2), nitrogen carries out purging 10 minutes to sealer (2) inside, to drain the air in sealer (2) completely;
2) put in sealer (2) by the solid-state dichlorosilane via cooled with liquid nitrogen, extracting vacuum, the vacuum tightness making sealer (2) inner is 0Pa;
3) sealer (2) is placed in water bath (3), the pure water of flowing is used to carry out water-bath, water temperature is between 0-25 DEG C, after the complete liquefy of solid-state dichlorosilane in device to be sealed (2), a small amount of liquid nitrogen is passed in water bath (3), make temperature control at about 0 DEG C, wait for 3-8 minute, make the gas-liquid in sealer (2) reach balance;
4) pass into carrier gas pressurization with conduit (4), sample is along with carrier gas together sample introduction;
5) adopt Shimadzu GC-2014 type gas chromatograph, thermal conductivity detector (TCD) to carry out detection to sample introduction to analyze, wherein:
Chromatographic condition: RTX-VMS(30m*0.25mm*1.4 μm); Temperature: detecting device 200 DEG C, injection port 150 DEG C, column temperature 80 DEG C; Shunting mode sample introduction, split ratio: 10:1, sample introduction 10 μ l; Post flow: high-pure helium 2ml/min; Tail blows: high-pure helium 30ml/min;
6) sealer (2) obtained after step 4) being sampled processes, and repeats step 3)-step 5), determine that it goes out peak position according to retention time, qualitative test.
2. the detection method of a kind of dichloro-dihydro silicon components according to claim 1, is characterized in that: the carrier gas in described step 4) is helium.
3. the detection method of a kind of dichloro-dihydro silicon components according to claim 1, it is characterized in that: the water bath (3) of described sampling device (1) bottom is provided with three conduits (4), one for importing liquid nitrogen, one for importing the pure water under normal temperature, one for draining; Sealer (2) is provided with three conduits (4), one in order to access pure nitrogen, one for emptying, one for extracting vacuum.
4. the detection method of a kind of dichloro-dihydro silicon components according to claim 3, is characterized in that: described conduit (4) is stainless steel pipe.
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| CN201510992381.0A CN105388230B (en) | 2015-12-25 | 2015-12-25 | Dichlorosilane component detection method |
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| CN201510992381.0A CN105388230B (en) | 2015-12-25 | 2015-12-25 | Dichlorosilane component detection method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413430A (en) * | 2020-04-16 | 2020-07-14 | 浙江西亚特电子材料有限公司 | Dichlorosilane metal ion analysis device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090060820A1 (en) * | 2007-09-05 | 2009-03-05 | Shin-Etsu Chemical Co., Ltd. | Method for producing trichlorosilane and method for producing polycrystalline silicon |
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- 2015-12-25 CN CN201510992381.0A patent/CN105388230B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090060820A1 (en) * | 2007-09-05 | 2009-03-05 | Shin-Etsu Chemical Co., Ltd. | Method for producing trichlorosilane and method for producing polycrystalline silicon |
Non-Patent Citations (4)
| Title |
|---|
| 修先运: "二氯二氢硅的气相色谱法分析", 《低温与特气》 * |
| 孙福楠等: "电子级二氯二氢硅的气相色谱分析", 《辽宁化工》 * |
| 杨裴等: "三氯氢硅气相色谱分析条件研究", 《无机盐工业》 * |
| 温文兵等: "影响气相色谱法分析三氯氢硅的因素讨论", 《中国氯碱》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413430A (en) * | 2020-04-16 | 2020-07-14 | 浙江西亚特电子材料有限公司 | Dichlorosilane metal ion analysis device |
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