CN105699512B - The detection method of ethane impurity in pure diborane - Google Patents
The detection method of ethane impurity in pure diborane Download PDFInfo
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- CN105699512B CN105699512B CN201610048206.0A CN201610048206A CN105699512B CN 105699512 B CN105699512 B CN 105699512B CN 201610048206 A CN201610048206 A CN 201610048206A CN 105699512 B CN105699512 B CN 105699512B
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- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000012535 impurity Substances 0.000 title claims abstract description 36
- 238000001514 detection method Methods 0.000 title claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 57
- 238000001179 sorption measurement Methods 0.000 claims abstract description 29
- 239000012159 carrier gas Substances 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004817 gas chromatography Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000010812 external standard method Methods 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 230000004907 flux Effects 0.000 claims abstract description 5
- 230000008016 vaporization Effects 0.000 claims abstract description 5
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 4
- 238000009834 vaporization Methods 0.000 claims abstract description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000011089 carbon dioxide Nutrition 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000011324 bead Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- -1 ethane hydrocarbon Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to the detection technique fields of trace impurity in gas, specifically disclose a kind of detection method of ethane impurity in pure diborane：Using gas chromatography, detector is hydrogen flame ionization detector (FID), and carrier gas is high pure nitrogen；Porapak Q columns are as chromatographic column, 104 columns of GDX are as adsorption column, control 35 DEG C~25 DEG C of adsorption column column temperature, 70 ± 2 DEG C of chromatographic column column temperature, carrier gas flux is 30 ± 5ml/min, is carried after quantitative sample vaporization through carrier gas along gas circuit and first passes through the adsorption column, then pass through the chromatographic column, it is detected into FID, obtains sample gas chromatogram；Qualitative and quantitative analysis is carried out to ethane in sample gas according to sample gas chromatogram using external standard method again.The method of the present invention can carry out the ethane impurity in pure diborane qualitative and quantitative detection, and detection method is simple, quick, demand for control of the enterprise to pure diborane impurity is disclosure satisfy that, suitable for promoting the use of.
Description
Technical field
The present invention relates to the detection technique field of trace impurity in gas, more particularly, to pure diborane technical field.
Background technology
Pure diborane is the important source material used in semiconductor technology, and purity has important shadow to the quality of semiconductor devices
It rings, therefore, it is necessary to control the type and content of impurity in diborane.There is semiconductor technology to require phosphorus content in pure diborane low
In limit value, prior art detection determines that wherein methane content is significantly lower than the limit value, thus it is speculated that wherein also contain ethane, however it is existing
There are no the analyzing detecting methods of ethane impurity in pure diborane for technology.
The analyzing detecting method of impurity is more difficult in pure diborane, and various countries are without point for impurity in pure diborane
Analysis detection formulation standard, and relevant paper report is less.Main reason is that：Diborane is dangerous special gas, safety wind
Danger is high, and impurity composition separation is difficult in diborane, and the diborane of high-content interferes the detection of trace impurity, in chromatogram
Impurity peaks are covered by diborane peak.
Invention content
The technical problem to be solved in the present invention is to provide a kind of detection methods of ethane impurity in pure diborane, can be in reality
It tests and carries out qualitative and quantitative detection under the normal condition of room to the ethane impurity in pure diborane, detection method is simple, quick, can
Meet demand for control of the enterprise to pure diborane impurity, suitable for promoting the use of.
In order to solve the above technical problems, the technical solution used in the present invention is：The detection of ethane impurity in pure diborane
Method, using gas chromatography, detector is hydrogen flame ionization detector (FID), and carrier gas is high pure nitrogen；Chromatographic column specification：
The Porapak Q columns of long 2m, internal diameter 3mm；Adsorption column specification：The GDX-104 columns of long 2m, internal diameter 4mm；
- 35 DEG C~-25 DEG C of adsorption column column temperature, 70 ± 2 DEG C of chromatographic column column temperature are controlled, carrier gas flux is 30 ± 5ml/min, fixed
It is carried after amount sample vaporization through carrier gas along gas circuit and first passes through the adsorption column, then by the chromatographic column, detected into FID, obtain sample
Product complexion spectrogram；
Qualitative and quantitative analysis is carried out to ethane in sample gas according to sample gas chromatogram using external standard method.
The low absorption for being conducive to diborane of adsorption column column temperature, but column temperature is too low diborane to be made to liquefy, and can also reduce instrument
The sensitivity of device.- 35 DEG C~-25 DEG C of adsorption column column temperature is controlled, relatively good constant temperature, cooling and heating are easy to operate also than very fast.
Preferably, control adsorption column column temperature is -30 DEG C, 70 DEG C of chromatographic column column temperature, carrier gas flux 30ml/min.
The adsorption column is placed in alcohol bath, is cooled down with dry ice.
Preferably, the vapourizing temperature of quantitative sample is 100 ± 2 DEG C.
The FID temperature is 150 DEG C, and combustion-supporting gas used is hydrogen and air.
Further, quantified by external standard method analysis method is as follows：
By quantitative ethane Standard Gases according to the identical chromatographic condition of sample, adsorption column and chromatographic column are passed sequentially through, into FID
Detection, obtains Standard Gases chromatogram；It determines therewith to go out in sample gas chromatogram according to ethane peak appearance time in Standard Gases chromatogram
The same or similar peak of peak time is ethane peak in sample gas chromatogram, according to the peak area at ethane peak and ethane content into just
Than ethane impurity content in sample vapour is calculated.
It is using advantageous effect caused by above-mentioned technical proposal：The present invention provides ethane in a kind of pure diborane is miscellaneous
The detection method of matter can carry out qualitative and quantitative detection under the normal condition of laboratory to the ethane impurity in pure diborane,
The blank of the prior art has been filled up, detection method is simple, quick, disclosure satisfy that demand for control of the enterprise to pure diborane impurity,
Suitable for promoting the use of.
Description of the drawings
Fig. 1 is gas chromatography of embodiment of the present invention sampling gas circuit schematic diagram；
Fig. 2 is gas chromatography sample introduction gas circuit schematic diagram of the embodiment of the present invention；
Fig. 3 is the chromatography that gas chromatography of the embodiment of the present invention measures ethane in ethane Standard Gases and pure diborane sample gas
Figure.
Specific embodiment
The present invention is detected the micro ethane impurity in pure diborane using gas chromatography, by adsorption column to second
The absorption of borine reduces its interference of detection to micro ethane impurity so that ethane hydrocarbon impurities can be detected by FID, finally
The qualitative of impurity and quantitative determination are completed by external standard method.The method of the present invention is easy to operate, quick, and testing conditions are content with very little,
Requirement to chromatograph devices is low, has filled up the technological gap that the prior art detects the micro ethane impurity in pure diborane,
It is easy to enterprise's production and scientific research uses.
The present invention will be further described for citing below.
Embodiment
Using gas chromatography, qualitative and quantitative analysis is carried out to the Analysis of Hydrocarbon Impurities in pure diborane.
Detection device and testing conditions are as follows：
Detector is FID, instrument model 3400, Monitoring lower-cut 1ppm, and temperature is 150 DEG C, combustion-supporting gas for hydrogen and
Air；
100 DEG C of temperature of vaporization chamber；
Carrier gas be nitrogen (5N), flow 30ml/min；
Adsorption column is porous polymer bead carrier packed column：GDX-104,2m × Φ 4；
Chromatographic column is PQ chromatographic columns：Fill the Porapak Q, 2m × Φ 3 of 60-80 mesh；
Adsorption column column temperature is -30 DEG C, 70 DEG C of chromatographic column column temperature.
Standard Gases and sample gas are respectively obtained into Standard Gases chromatogram and sample complexion successively by chromatograph gas circuit respectively
Spectrogram determines that appearance time is same or similar therewith in sample gas chromatogram according to ethane peak appearance time in Standard Gases chromatogram
Peak be ethane peak in sample gas chromatogram, it is directly proportional to ethane content further according to the peak area at ethane peak, sample is calculated
Ethane impurity content in vapour.
In Standard Gases chromatogram ethane appearance time for 6 points 18 seconds.
Chromatograph gas circuit is illustrated by taking sample as an example, Standard Gases are identical with sample gas dataway operation.
Sample samples sample gas after vaporizing chamber vaporizes, and pneumatic diagram is shown in Fig. 1, wherein, sample gas side indicated by arrows
To, into valve 1, quantity tube is crossed, goes out valve 1, discharge；Carrier gas direction indicated by arrows into valve 1, goes out valve 1, into valve 2, goes out valve 2, crosses and inhale
Attached column into valve 2, goes out valve 2, chromatographic column is crossed, into fid detector；Nitrogen direction indicated by arrows goes out valve 2, discharges into valve 2.
During sampling, sample is crossed quantity tube and is expelled directly out, and will not enter detector.
After the completion of sample gas sampling, by sample gas sample introduction, the sample gas that carrier gas is carried in quantity tube passes through gas circuit to detection
Device.Sample introduction pneumatic diagram is shown in Fig. 2, wherein, sample gas direction indicated by arrows into valve 1, goes out valve 1, discharge；Carrier gas is indicated by arrows
Direction into valve 1, crosses quantity tube, goes out valve 1, into valve 2, goes out valve 2, crosses adsorption column, into valve 2, goes out valve 2, crosses chromatographic column, is detected into FID
Device；Nitrogen direction indicated by arrows goes out valve 2, discharges into valve 2.
Sample introduction and sampling are controlled by valve 1, and valve 2 does not have to switching.After the completion of sample gas analysis, switching valve 2 will be adsorbed with nitrogen
Diborane is blown out in column, and adsorption column is gradually warmed to room temperature in purge.Adsorption column is used for multiple times rear adsorption effect and can reduce, and needs
It regularly replaces.
After adsorption column long-time use, make adsorbate desorption effect poor using high-temperature activation.It is changed in the present invention
Adsorption column carry out with the following method cleaning can again continue to use, adsorption column cost can be reduced：
The GDX-104 fillers of failure from adsorption column are poured out, are cleaned with the NaOH solution of 1mol/L, GDX-104 is white
The bead of color can become faint yellow after absorption diborane failure, first be impregnated 12 hours with the NaOH solution of 1mol/L, rear to stir
2 hours, the diborane of absorption can be made to be dissolved into solution, GDX-104 becomes white again, then it is 7 to be cleaned with clear water to PH,
It refills.GDX-104 prices are relatively low, and shape is more regular, convenient for cleaning.
Practical pure diborane production detection, generally by ethane Standard Gases and pure diborane sample gas interval 3min successively
It is detected by chromatograph gas circuit, obtains chromatogram and see Fig. 3.
In Fig. 3, first peak (peak height is about 42mv) is Standard Gases ethane peak in chromatogram, peak area AMarkIt is 2319, the
Two peaks (peak height is about 50mv) are sample gas ethane peak, peak area ASampleIt is 2759, Standard Gases are ethane concentration CMarkFor 50.6ppm
Ethane/helium mix gas, be calculated as follows to obtain sample gas ethane content：
CSample=(ASample/AMark)×CMark=60.2ppm.
It is miscellaneous by above-mentioned gas chromatography detection wherein ethane to the diborane product of Baoding north Te Qi Co., Ltds production
The content of matter, the results are shown in table below.
| Sample number into spectrum (steel cylinder) | Volume | Filling weight | Detection project | Concentration |
| 001184 | 40L | 2.09kg | C2H6 | 27.4ppm |
| 001353 | 40L | 1.93kg | C2H6 | 18.5ppm |
| 001196 | 40L | 1.99kg | C2H6 | 26.7ppm |
| 001310 | 40L | 2.05kg | C2H6 | 25.4ppm |
| 001195 | 40L | 2.08kg | C2H6 | 24.3ppm |
The method of the present invention can exclude the interference of other hydrocarbon impurities such as methane, chloromethanes in diborane, can be quickly accurate
True measure wherein ethane content, easy to operate, cost of determination is low, suitable for the detection of batch sample.
Claims (6)
1. the detection method of ethane impurity in pure diborane, it is characterised in that：Using gas chromatography, detector is hydrogen flame ion
Change detector (FID), carrier gas is high pure nitrogen；Chromatographic column specification：The Porapak Q columns of long 2m, internal diameter 3mm；Adsorption column specification：
The GDX-104 columns of long 2m, internal diameter 4mm, the GDX-104 fillers of failure are poured out from adsorption column, clear with the NaOH solution of 1mol/L
It washes, then it is 7 to be cleaned with clear water to pH；
- 35 DEG C~-25 DEG C of adsorption column column temperature, 70 ± 2 DEG C of chromatographic column column temperature are controlled, carrier gas flux is 30 ± 5ml/min, quantitative sample
It is carried after product vaporization through carrier gas along gas circuit and first passes through the adsorption column, then by the chromatographic column, detected into FID, obtain sample gas
Chromatogram；
Qualitative and quantitative analysis is carried out to ethane in sample gas according to sample gas chromatogram using external standard method.
2. the detection method of ethane impurity in pure diborane according to claim 1, which is characterized in that control adsorption column column
Temperature is -30 DEG C, 70 DEG C of chromatographic column column temperature, carrier gas flux 30ml/min.
3. the detection method of ethane impurity in pure diborane according to claim 2, which is characterized in that the adsorption column is put
In alcohol bath, cooled down with dry ice.
4. the detection method of ethane impurity in pure diborane according to claim 1, which is characterized in that the vapour of quantitative sample
It is 100 ± 2 DEG C to change temperature.
5. the detection method of ethane impurity in pure diborane according to claim 1, which is characterized in that the FID temperature
It it is 150 DEG C, combustion-supporting gas used is hydrogen and air.
6. the detection method of ethane impurity in pure diborane according to claim 1, which is characterized in that quantified by external standard method point
Analysis method is as follows：
By quantitative ethane Standard Gases according to the identical chromatographic condition of sample, adsorption column and chromatographic column are passed sequentially through, is examined into FID
It surveys, obtains Standard Gases chromatogram；Appearance therewith is determined in sample gas chromatogram according to ethane peak appearance time in Standard Gases chromatogram
Time same or similar peak is ethane peak in sample gas chromatogram, directly proportional to ethane content according to the peak area at ethane peak,
Ethane impurity content in sample vapour is calculated.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5531971A (en) * | 1993-06-29 | 1996-07-02 | Millipore Investment Holdings Limited | Process for purifying semiconductor process gases to remove lewis acid and oxidant impurities therefrom |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5531971A (en) * | 1993-06-29 | 1996-07-02 | Millipore Investment Holdings Limited | Process for purifying semiconductor process gases to remove lewis acid and oxidant impurities therefrom |
Non-Patent Citations (5)
| Title |
|---|
| 乙烷氧化脱氢反应产物的气相色谱分析;梁奇 等;《石油与天然气化工》;19991231;第28卷(第2期);第139页左栏 * |
| 低浓度乙硼烷成分的气相色谱分析;董玉莲 等;《低温与特气》;20051031;第23卷(第5期);全文 * |
| 吸附/热脱附气相色谱分析痕量 C1-C5烃;崔兆杰 等;《分析测试技术与仪器》;19940630(第2期);第25-26页 * |
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Denomination of invention: Detection method for ethane impurities in pure ethylborate Effective date of registration: 20231207 Granted publication date: 20180706 Pledgee: Bank of China Limited Hebei xiong'an branch Pledgor: BAODING NORTH SPECIAL GAS Co.,Ltd. Registration number: Y2023980069927 |