CN113125372A - Impurity gas detection device and method for electronic-grade boron trichloride purification system - Google Patents
Impurity gas detection device and method for electronic-grade boron trichloride purification system Download PDFInfo
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- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 238000001514 detection method Methods 0.000 title claims abstract description 80
- 239000012535 impurity Substances 0.000 title claims abstract description 57
- 238000000746 purification Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 52
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 45
- 239000000047 product Substances 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims description 96
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 30
- 239000003513 alkali Substances 0.000 claims description 27
- 239000001307 helium Substances 0.000 claims description 22
- 229910052734 helium Inorganic materials 0.000 claims description 22
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 22
- 238000003860 storage Methods 0.000 claims description 17
- 230000003287 optical effect Effects 0.000 claims description 14
- 229910001632 barium fluoride Inorganic materials 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims description 7
- 229910003910 SiCl4 Inorganic materials 0.000 claims description 7
- 229910003818 SiH2Cl2 Inorganic materials 0.000 claims description 7
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 238000006386 neutralization reaction Methods 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 13
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 13
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 13
- 230000009102 absorption Effects 0.000 description 11
- 238000005259 measurement Methods 0.000 description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 8
- 239000004327 boric acid Substances 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 238000013461 design Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000004445 quantitative analysis Methods 0.000 description 4
- 239000002912 waste gas Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000011897 real-time detection Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000012886 linear function Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
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- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses an impurity gas detection device and method of an electronic grade boron trichloride purification system. The first Fourier infrared spectrum detection system can detect impurity gas in a boron trichloride crude product, the second Fourier infrared spectrum detection system can detect impurity gas in an electronic grade boron trichloride finished product generated by a boron trichloride purification system, the two systems can work simultaneously, simultaneous detection of impurity gas in the boron trichloride crude product and the finished product is realized, and a base solution cylinder can be used for carrying out neutralization absorption on the detected boron trichloride crude product and the detected finished product.
Description
Technical Field
The invention relates to the technical field of special gas detection, in particular to an impurity gas detection device and method of an electronic-grade boron trichloride purification system.
Background
Boron trichloride is a gaseous or colorless fuming liquid with pungent odor. The electronic grade boron trichloride is mainly used in the technical field of semiconductors such as IC, OLED, LED and the like, and is a high-purity semiconductor material with excellent performance. Boron trichloride is used as a basic material with large dosage and high purity requirement in the fields of integrated circuits and electronic devices, is a product and industry which are mainly encouraged to develop in China, and accords with the national middle and long-term science and technology development program (2021-.
With the progress of integrated circuit technology, the technical node reaches 7 nanometers, the wafer manufacture reaches 12 inches, the requirement on the purity of the electronic grade boron trichloride is higher and higher, correspondingly, higher requirements are provided for the detection of impurity gases in the electronic grade boron trichloride special gas, and at present, China has no mature detection technology in related fields and is limited by people. CH in boron trichloride impurity gas4、CO、CO2、HCl、COCl2、SiCl4And SiH2Cl2The patent CN108821302A discloses a method and a device for purifying boron trichloride, which comprises a decomposition section, a rectification section, a storage and filling section and a recovery section, wherein the recovery section is as follows: the waste gas treatment device is provided with a recovery tank, the recovery tank can collect waste gas discharged from a rectification working section, a three-way pipe is arranged at the bottom of the recovery tank, one discharge port of the three-way pipe is communicated with a waste gas treatment tower, and the waste gas treatment tower comprises an alkaline washing section and a water washing section which are arranged in series; in the process of continuously collecting by the recovery tank, some gas impurities comprise small amounts of CO and Cl2And N2And the gas impurities are gradually enriched at the bottom and the top of the recovery tank respectively, and then are discharged periodically. The problems with this technique are as follows: only heavy components and light components discharged from the rectifying section are recovered, and the real-time detection of impurity gases in the crude product and the finished product of boron trichloride cannot be realized.
Disclosure of Invention
The invention aims to solve the technical problem that the existing boron trichloride purification system cannot realize real-time detection of impurity gases in a boron trichloride crude product and a boron trichloride finished product.
In order to solve the technical problems, the invention provides the following technical scheme: an impurity gas detection device of an electronic grade boron trichloride purification system comprises a crude product storage tank, a first pipeline, a second pipeline, a first Fourier infrared spectrum detection system, a first buffer tank, a first vacuum pump, a boron trichloride purification system, a third pipeline, a second Fourier infrared spectrum detection system, a second buffer tank, a second vacuum pump and an alkali liquor cylinder; the first pipeline and the second pipeline are arranged in parallel, and the inlet of the first pipeline and the inlet of the second pipeline are communicated with the discharge hole of the crude product storage tank through a three-way valve; the first Fourier infrared spectrum detection system comprises a first sample tank, a feed inlet of the first sample tank is communicated with an outlet of the first pipeline, a feed inlet of the first buffer tank is communicated with a discharge outlet of the first sample tank, a feed inlet of the first vacuum pump is communicated with a discharge outlet of the first buffer tank, and a discharge outlet of the first vacuum pump is communicated into the alkali liquor cylinder; a feed inlet of the boron trichloride purification system is communicated with an outlet of the second pipeline; the inlet of the third pipeline is communicated with the discharge hole of the boron trichloride purification system; the second Fourier infrared spectrum detection system comprises a second sample cell, a feed inlet of the second sample cell is communicated with an outlet of the third pipeline, a feed inlet of the second buffer tank is communicated with a discharge outlet of the second sample cell, a feed inlet of the second vacuum pump is communicated with a discharge outlet of the second buffer tank, and a discharge outlet of the second vacuum pump is communicated into the alkali liquor cylinder;
the optical path of the first sample cell is 60mm, and the optical path of the second sample cell is 10 m.
According to the invention, through the arrangement of the first Fourier infrared spectrum detection system and the second Fourier infrared spectrum detection system, the first Fourier infrared spectrum detection system can detect impurity gases of a boron trichloride crude product, the second Fourier infrared spectrum detection system can detect impurity gases in an electronic grade boron trichloride finished product generated by a boron trichloride purification system, the two systems can work simultaneously, so that the simultaneous detection of the impurity gases in the boron trichloride crude product and the impurity gases in the boron trichloride finished product is realized, and the alkali liquor cylinder can be simultaneously utilized to neutralize and absorb the boron trichloride crude product and the boron trichloride finished product.
As the concentration of the impurity gas in the boron trichloride crude product is higher and the infrared fingerprint characteristic absorption is stronger, the optical path of the first sample pool is designed to be 60mm, the concentration of the impurity gas in the electronic grade boron trichloride finished product is lower, and the infrared fingerprint characteristic absorption is weaker, so that the optical path of the second sample pool is designed to be 10 m.
Preferably, the window sheets on the left and right sides of the first sample cell and the window sheets on the left and right sides of the second sample cell are both BaF2A window piece; the window sheets passing through the left side and the right side of the first sample cell and the window sheets passing through the left side and the right side of the second sample cell are designed as BaF2Window piece, BaF2The window does not react with boron trichloride to avoid corrosion.
Preferably, a temperature and pressure control system is arranged in each of the first sample cell and the second sample cell, the temperature of the gas in each of the first sample cell and the second sample cell is constant at 42 +/-0.2 ℃, and the pressure of the gas in each of the first sample cell and the second sample cell is constant at 1 +/-0.1 standard atmospheric pressure.
Preferably, the first fourier infrared spectrum detection system further comprises a first detector, a first FTIR spectrometer, a first infrared light source and first control analysis software; the first detector is arranged on one side of the first sample pool; the first FTIR spectrometer is arranged on the other side of the first sample cell; the first infrared light source is arranged on the other side of the first FTIR spectrometer; the first control analysis software is electrically connected with the first detector, the first FTIR spectrometer and the first infrared light source.
Preferably, the first fourier infrared spectrum detection system detects impurity gas components and concentration ranges as follows: CH (CH)4：100-200ppm、CO：100-150ppm、CO2：100-200ppm，HCl：100-300ppm、COCl2：1-200ppm、SiCl4：100-300ppm、SiH2Cl2：1-200ppm。
Preferably, the second fourier infrared spectrum detection system further comprises a second detector, a second FTIR spectrometer, a second infrared light source and second control analysis software; the second detector is arranged on one side of the second sample cell; the second FTIR spectrometer is arranged on the other side of the second sample cell; the second infrared light source is arranged on the other side of the second FTIR spectrometer; and the second control analysis software is electrically connected with the second detector, the second FTIR spectrometer and the second infrared light source.
Preferably, the component and concentration range of the impurity gas detected by the second fourier infrared spectrum detection system are as follows: CH (CH)4：0.01-0.5ppm、CO：0.1-0.5ppm、CO2：0.1-2ppm、HCl：0.1-1ppm、COCl2：0.1-1ppm、SiCl4：0.05-2ppm、SiH2Cl2：0.1-1ppm。
Preferably, the device further comprises a helium tank, wherein a gas outlet of the helium tank is respectively communicated with the first pipeline and the third pipeline through a three-way valve to form a gas path system, and the gas path system is constant in heat tracing at 42 +/-0.2 ℃; because boron trichloride is very easy to hydrolyze when meeting water to generate hydrogen chloride and boric acid, the hydrogen chloride has very strong corrosivity and is easy to corrode various parts on an instrument, and the boric acid is very easy to block pipelines, the helium tank is respectively communicated with the first pipeline and the third pipeline through the three-way valve to form a gas path system, and the whole gas path system is swept by high-purity helium; and in order to prevent boron trichloride from adsorbing, the whole gas path system is constant at 42 +/-0.2 ℃ for heat tracing.
Preferably, the first pipeline and the third pipeline are both provided with a pressure reducing valve and a flow meter.
The invention also discloses a detection method of the impurity gas detection device of the electronic grade boron trichloride purification system, which comprises the following steps: starting a first vacuum pump, filling a part of boron trichloride crude products in a crude product storage tank into a first sample tank of a first Fourier infrared spectrum detection system through a first pipeline, after detection and analysis, leading the boron trichloride crude products into an alkali liquid cylinder through an outlet of the first sample tank and a first buffer tank, and neutralizing the detected boron trichloride crude products by the alkali liquid cylinder; starting a second vacuum pump, introducing the other part of the boron trichloride crude product in the crude product storage tank into a boron trichloride purification system through a second pipeline to further generate a high-purity electronic-grade boron trichloride finished product, introducing the electronic-grade boron trichloride finished product into a second sample pool of a second Fourier infrared spectrum detection system through a third pipeline, introducing the electronic-grade boron trichloride finished product into an alkali liquid cylinder through an outlet of the second sample pool and a second buffer tank, and neutralizing the detected electronic-grade boron trichloride finished product by the alkali liquid cylinder; or the first vacuum pump and the second vacuum pump are started simultaneously to realize the simultaneous detection of impurity gases in the boron trichloride crude product and the finished product, and the alkali liquor cylinder neutralizes the detected boron trichloride crude product and the finished product simultaneously.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the first Fourier infrared spectrum detection system and the second Fourier infrared spectrum detection system, the first Fourier infrared spectrum detection system can detect impurity gases in a boron trichloride crude product, the second Fourier infrared spectrum detection system can detect impurity gases in an electronic grade boron trichloride finished product generated by the boron trichloride purification system, the two systems can work simultaneously, so that the simultaneous detection of the impurity gases in the boron trichloride crude product and the impurity gases in the finished product is realized, and the detected boron trichloride crude product and the detected finished product can be neutralized and absorbed by the alkali liquor cylinder.
2. As the concentration of the impurity gas in the boron trichloride crude product is higher and the infrared fingerprint characteristic absorption is stronger, the optical path of the first sample pool is designed to be 60mm, the concentration of the impurity gas in the electronic grade boron trichloride finished product is lower, and the infrared fingerprint characteristic absorption is weaker, so that the optical path of the second sample pool is designed to be 10 m.
3. The invention designs the window sheets on the left and right sides of the first sample cell and the window sheets on the left and right sides of the second sample cell as BaF2Window piece, BaF2The window does not react with boron trichloride to avoid corrosion.
4. Because boron trichloride is very easy to hydrolyze when meeting water to generate hydrogen chloride and boric acid, the hydrogen chloride has very strong corrosivity and is easy to corrode various parts on an instrument, and the boric acid is very easy to block pipelines, the invention designs the helium tank which is respectively communicated with the first pipeline and the third pipeline through the three-way valve to form a gas path system, and the whole gas path system is swept by high-purity helium; and in order to prevent boron trichloride from adsorbing, the whole gas path system is constant at 42 +/-0.2 ℃ for heat tracing.
Drawings
FIG. 1 is a schematic structural diagram of an impurity gas detection device of an electronic grade boron trichloride purification system;
FIG. 2 is a standard infrared absorption spectrum of an impurity gas in accordance with an embodiment of the present invention.
The reference numbers illustrate:
1. a crude product storage tank; 2. a first pipeline; 3. a second pipeline; 4. a first Fourier infrared spectrum detection system; 401. a first sample tank; 402. a first detector; 403. a first FTIR spectrometer; 404. a first infrared light source; 405. first control analysis software; 5. a first buffer tank; 6. a first vacuum pump; 7. a boron trichloride purification system; 8. a third pipeline; 9. a second Fourier infrared spectrum detection system; 901. a second sample cell; 902. a second detector; 903. a second FTIR spectrometer; 904. a second infrared light source; 905. second control analysis software; 10. a second buffer tank; 11. a second vacuum pump; 12. an alkaline liquid cylinder; 13. a helium tank.
Detailed Description
In order to facilitate the understanding of the technical solutions of the present invention for those skilled in the art, the technical solutions of the present invention will be further described with reference to the drawings attached to the specification.
The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
Example one
As shown in fig. 1, the embodiment discloses an impurity gas detection device of an electronic grade boron trichloride purification system, which comprises a crude product storage tank 1, a first pipeline 2, a second pipeline 3, a first fourier infrared spectrum detection system 4, a first buffer tank 5, a first vacuum pump 6, a boron trichloride purification system 7, a third pipeline 8, a second fourier infrared spectrum detection system 9, a second buffer tank 10, a second vacuum pump 11, an alkali cylinder 12 and a helium tank 13.
As shown in fig. 1, a crude boron trichloride product is stored in the crude product storage tank 1 of the present embodiment, a discharge port of the crude product storage tank 1 is respectively communicated with an inlet of a first pipeline 2 and an inlet of a second pipeline 3 through a three-way valve, a feed port of the three-way valve is connected with a discharge port of the crude product storage tank 1 through a pipeline, one port of the pipeline is welded and fixed with and communicated with the discharge port of the crude product storage tank 1, and the other port of the pipeline is welded and fixed with and communicated with the feed port; one discharge port of the three-way valve is fixedly welded and communicated with an inlet of the first pipeline 2, and the other discharge port of the three-way valve is fixedly welded and communicated with an inlet of the second pipeline 3; the first pipeline 2 and the second pipeline 3 of the embodiment are both equipped with electromagnetic valves, and the first pipeline 2 is also equipped with a pressure reducing valve and a flow meter.
As shown in fig. 1, and with particular reference to the orientation of fig. 1, the first fourier transform infrared spectroscopy detection system 4 comprises a first sample cell 401, a first detector 402, a first FTIR spectrometer 403, a first infrared light source 404, and first control analysis software 405;
a feed inlet of the first sample tank 401 is fixedly welded and communicated with an outlet of the first pipeline 2; a first detector 402 is mounted to the left of the first sample cell 401; a first FTIR spectrometer 403 is mounted to the right of the first sample cell 401; a first infrared light source 404 is mounted to the right of the first FTIR spectrometer 403; the first control analysis software 405 is electrically connected with the first detector 402, the first FTIR spectrometer 403 and the first infrared light source 404;
as shown in FIG. 1, the optical length of the first sample cell 401 of this embodiment is 60mm, and the window pieces on the left and right sides of the first sample cell 401 are BaF2A window, in this embodiment, a temperature and pressure control system is further installed in the first sample cell 401, and the temperature of the gas in the first sample cell 401 is constant at 42 ± 0.2 ℃,the air pressure is constant at 1 +/-0.1 standard atmospheric pressure, and the components and concentration range of the detected impurity gas are as follows: CH (CH)4：100-200ppm、CO：100-150ppm、CO2：100-200ppm，HCl：100-300ppm、COCl2：1-200ppm、SiCl4：100-300ppm、SiH2Cl2：1-200ppm。
As shown in fig. 1, the feed inlet of the first buffer tank 5 is communicated with the discharge outlet of the first sample tank 401 through a pipeline, two ends of the pipeline are respectively welded and fixed with the feed inlet of the first buffer tank 5 and the discharge outlet of the first sample tank 401 and are communicated with each other, and the pipeline is further equipped with an electromagnetic valve.
As shown in fig. 1, the feed inlet of the first vacuum pump 6 is communicated with the discharge outlet of the first buffer tank 5 through a pipeline, the pipeline and the two ports are respectively welded and fixed with the feed inlet of the first vacuum pump 6 and the discharge outlet of the first buffer tank 5 and communicated, the pipeline is provided with an electromagnetic valve, the discharge outlet of the first vacuum pump 6 is communicated to the alkali liquor cylinder 12 through a pipeline, one port of the pipeline is welded and fixed with the discharge outlet of the first vacuum pump 6 and communicated, and the other port of the pipeline directly extends into the alkali liquor of the alkali liquor cylinder 12.
As shown in fig. 1, the feed inlet of the boron trichloride purification system 7 of the present embodiment is welded and fixed to and communicated with the discharge outlet of the second pipeline 3.
As shown in fig. 1, and specifically with reference to the orientation of fig. 1, the second fourier infrared spectroscopy detection system 9 includes a second sample cell 901, a second detector 902, a second FTIR spectrometer 903, a second infrared light source 904, and second control analysis software 905;
the feed inlet of the second sample cell 901 is communicated with the discharge outlet of the boron trichloride purification system 7 through a third pipeline 8, one port of the third pipeline 8 is welded, fixed and communicated with the feed inlet of the second sample cell 901, the other port of the third pipeline 8 is welded, fixed and communicated with the feed inlet of the second sample cell 901, and the third pipeline 8 of the embodiment is also provided with a pressure reducing valve and a flowmeter; a second detector 902 is mounted on the left side of the second sample cell 901; a second FTIR spectrometer 903 is mounted to the right of the second sample cell 901; a second infrared light source 904 is mounted to the right of the second FTIR spectrometer 903; the second control analysis software 905 is electrically connected with the second detector 902, the second FTIR spectrometer 903 and the second infrared light source 904;
as shown in FIG. 1, the optical length of the second sample cell 901 of this embodiment is 10m, and the window sheets on both the left and right sides of the second sample cell 901 are BaF2The window piece, and be provided with accuse temperature accuse pressure system in the second sample cell 901, the gaseous temperature is all invariable 42 + -0.2 ℃ in the second sample cell 901, and atmospheric pressure is all invariable 1 + -0.1 standard atmospheric pressure, and it is: CH (CH)4：0.01-0.5ppm、CO：0.1-0.5ppm、CO2：0.1-2ppm、HCl：0.1-1ppm、COCl2：0.1-1ppm、SiCl4：0.05-2ppm、SiH2Cl2：0.1-1ppm。
As shown in fig. 1, the feed inlet of the second buffer tank 10 is communicated with the discharge outlet of the second sample cell 901 through a pipeline, two ports of the pipeline are respectively welded and fixed with the feed inlet of the second buffer tank 10 and the discharge outlet of the second sample cell 901 and are communicated, and the pipeline is further equipped with an electromagnetic valve.
As shown in fig. 1, a feed inlet of the second vacuum pump 11 is communicated with a discharge outlet of the second buffer tank 10 through a pipeline, the pipeline and two ports are welded, fixed and communicated with the feed inlet of the second vacuum pump 11 and the discharge outlet of the second buffer tank 10 respectively, an electromagnetic valve is assembled on the pipeline, the discharge outlet of the second vacuum pump 11 is communicated into the alkali liquor cylinder 12 through a pipeline, one port of the pipeline is welded, fixed and communicated with the discharge outlet of the second vacuum pump 11, and the other port of the pipeline directly extends into the alkali liquor of the alkali liquor cylinder 12.
As shown in fig. 1, an air outlet of a helium tank 13 is respectively communicated with a first pipeline 2 and a third pipeline 8 through a three-way valve to form an air path system, an air inlet of the three-way valve is connected with an air outlet of the helium tank 13 through a pipeline, two ports of the pipeline are respectively welded and fixed with the air outlet of the helium tank 13 and the air inlet of the three-way valve, one air outlet of the three-way valve is communicated with the inside of the first pipeline 2 through a pipeline, the other air outlet of the three-way valve is communicated with the inside of the third pipeline 8 through a pipeline, and electromagnetic valves are; this gas circuit system is invariable 42 + -0.2 ℃ heat tracing, because boron trichloride is extremely easily hydrolyzed when meeting water, produces hydrogen chloride and boric acid, and hydrogen chloride corrosivity is extremely strong easily to corrode various parts on the instrument, and the boric acid is extremely easily blockked up the pipeline, consequently, design helium gas pitcher 13 passes through the three-way valve respectively with first pipeline 2, third pipeline 8 intercommunication and form the gas circuit system, whole gas circuit system sweeps with high-purity helium, the invariable 42 + -0.2 ℃ heat tracing of way system is in order to prevent that boron trichloride from adsorbing.
The invention also discloses a method of the impurity gas detection device of the electronic grade boron trichloride purification system, which comprises the following steps: respectively starting a first vacuum pump 6 and a second vacuum pump 11, wherein the first vacuum pump 6 and the second vacuum pump 11 vacuumize two gas paths; controlling a part of the boron trichloride crude product in the crude product storage tank 1 to be filled into a first sample cell 401 of a first Fourier infrared spectrum detection system 4 through a first pipeline 2 by a flow meter on the first pipeline 2, after detection and analysis, enabling the boron trichloride crude product to pass through an outlet of the first sample cell 401, ensuring the temperature and the pressure of gas filled into the first sample cell 401 to be constant by temperature control and pressure control, further improving the measurement accuracy, after the measurement is finished, starting a first vacuum pump 6 again to pump the measurement gas into an alkali liquor cylinder 12 for neutralization, opening an electromagnetic valve on a helium tank 13 and a first pipeline 2 passage after the measurement is finished, introducing high-purity helium gas into a gas path system for purging, flushing a gas path and the first sample cell 401 by using the high-purity helium gas, and preventing gas adsorption; similarly, another part of the boron trichloride crude product in the crude product storage tank 1 is introduced into the boron trichloride purification system 7 through the second pipeline 3, so as to generate a high-purity electronic grade boron trichloride finished product, the flow meter on the third pipeline 8 controls the electronic grade boron trichloride finished product to be introduced into the second sample cell 901 of the second Fourier infrared spectrum detection system 9 through the third pipeline 8, after detection and analysis, the electronic grade boron trichloride finished product passes through the outlet of the second sample cell 901, the temperature and pressure of the gas introduced into the second sample cell 901 are ensured to be constant through temperature control and pressure control, so as to improve the measurement accuracy, after the measurement is finished, the second vacuum pump 11 is started again to pump the measurement gas into the alkali cylinder 12 for neutralization, after the completion, the electromagnetic valve on the passage between the helium tank 13 and the third pipeline 8 is opened, the high-purity helium gas is introduced into the gas path system for purging, and the gas path and the second sample cell 901 are flushed by the high-purity, preventing the formation of gas adsorption.
The principle of measuring and analyzing the boron trichloride crude product and the electronic grade boron trichloride finished product in the first Fourier infrared spectrum detection system 4 and the second Fourier infrared spectrum detection system 9 respectively is as follows:
take the impurity gas detection and analysis of the boron trichloride crude product as an example.
1. And (3) spectral measurement:
(1) filling a boron trichloride crude product into a first sample cell 401 with multiple reflections;
(2) a first infrared light source 404 is collimated by an optical system and then led into a first FTIR spectrometer 403, and an infrared radiation signal is subjected to interference modulation by the first FTIR spectrometer 403 and then led into a multi-reflection first sample cell 401;
(3) the infrared radiation signal after the interference modulation derived from the first sample pool 401 carries the absorption information of the sample to be detected and is converged on the first detector 402;
(4) the first control analysis software 405 converts the interferogram acquired by the first detector 402 into a spectrogram, thereby obtaining an absorption spectrum of the infrared absorption characteristic of the polluted gas to be detected.
2. Quantitative analysis
(1) Establishing a characteristic spectrum database: a database of characteristic spectra of the gas (impurity gas to be measured) adapted to the measurement parameters of the FTIR device is established (different gases have different characteristic absorptions of infrared, as shown in fig. 2, which gives the characteristic absorptions of infrared of different impurity gases). And establishing an infrared spectrum database which accords with the measurement parameters (spectrum resolution, field angle and apodization function) of the researched and developed equipment and can correct temperature and air pressure by utilizing the high-resolution infrared spectrum database for quantitative analysis.
(2) A multi-component quantitative analysis algorithm based on a synthetic calibration spectrum: extracting absorption line parameters of the target gas by using the established infrared spectrum database; by correcting the ambient temperature and the atmospheric pressure, inputting the optical path length and the preset gas components and concentrations, generating an atmospheric transmittance spectrum in an ideal state according to a single-layer atmospheric radiation transmission model, and performing convolution with an instrument linear function ILS of measuring equipment to generate a quantitative analysis calibration spectrum.
(3) And performing multiple iterative fitting on the synthesized calibration spectrum and the measured spectrum by applying a nonlinear least square fitting quantitative inversion algorithm to obtain the optimal value of the concentration of the gas to be measured.
Compared with the prior art, the invention has the following advantages: the detection method comprises the steps that through the arrangement of a first Fourier infrared spectrum detection system 4 and a second Fourier infrared spectrum detection system 9, the first Fourier infrared spectrum detection system 4 can detect impurity gases in a boron trichloride crude product, the second Fourier infrared spectrum detection system 9 can detect impurity gases in an electronic grade boron trichloride finished product generated by a boron trichloride purification system 7, the two systems can work simultaneously, the simultaneous detection of the impurity gases in the boron trichloride crude product and the finished product is realized, and an alkaline solution cylinder 12 can be used for neutralizing and absorbing the impurity gases in the boron trichloride crude product and the finished product; secondly, because the concentration of impurity gas in the boron trichloride crude product is higher, and the infrared fingerprint characteristic absorption is stronger, the optical path of the first sample cell 401 is designed to be 60mm, the concentration of impurity gas in the electronic grade boron trichloride finished product is lower, and the infrared fingerprint characteristic absorption is weaker, so the optical path of the second sample cell 901 is designed to be 10 m; thirdly, the invention designs the window sheets at the left and right sides of the first sample cell 401 and the window sheets at the left and right sides of the second sample cell 901 as BaF2Window piece, BaF2The window slice does not react with boron trichloride to avoid corrosion; fourthly, because boron trichloride is very easy to hydrolyze when meeting water to generate hydrogen chloride and boric acid, the hydrogen chloride has very strong corrosivity and is easy to corrode various parts on the instrument, and the boric acid is very easy to block pipelines, the invention designs the helium tank 13, the helium tank 13 is respectively communicated with the first pipeline 2 and the third pipeline 8 through the three-way valve to form a gas path system, and the whole gas path system is swept by high-purity helium; and in order to prevent boron trichloride from adsorbing, the whole gas path system is constant at 42 +/-0.2 ℃ for heat tracing.
Example two
The present embodiment differs from the above embodiments in that: as shown in fig. 1, the feed inlet of the first buffer tank 5 in this embodiment may also be directly communicated with the outlet of the first pipeline 2 through a pipeline, two ports of the pipeline are respectively welded and fixed with and communicated with the feed inlet of the first buffer tank 5 and the outlet of the first pipeline 2, and the pipeline is further equipped with an electromagnetic valve;
the feed inlet of the second buffer tank 10 in this embodiment may also be directly communicated with the outlet of the third pipeline 8 through a pipeline, two ports of the pipeline are respectively welded and fixed with the feed inlet of the second buffer tank 10 and the outlet of the third pipeline 8 and are communicated with each other, and the pipeline is further equipped with an electromagnetic valve.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The above embodiments only show the embodiments of the present invention, the protection scope of the present invention is not limited to the above embodiments, and those skilled in the art can make several variations and modifications without departing from the concept of the present invention, which all fall into the protection scope of the present invention.
Claims (10)
1. The utility model provides an impurity gas detection device of electron level boron trichloride purification system which characterized in that: the device comprises a crude product storage tank, a first pipeline, a second pipeline, a first Fourier infrared spectrum detection system, a first buffer tank, a first vacuum pump, a boron trichloride purification system, a third pipeline, a second Fourier infrared spectrum detection system, a second buffer tank, a second vacuum pump and an alkali liquor cylinder; the first pipeline and the second pipeline are arranged in parallel, and the inlet of the first pipeline and the inlet of the second pipeline are communicated with the discharge hole of the crude product storage tank through a three-way valve; the first Fourier infrared spectrum detection system comprises a first sample tank, a feed inlet of the first sample tank is communicated with an outlet of the first pipeline, a feed inlet of the first buffer tank is communicated with a discharge outlet of the first sample tank, a feed inlet of the first vacuum pump is communicated with a discharge outlet of the first buffer tank, and a discharge outlet of the first vacuum pump is communicated into the alkali liquor cylinder; a feed inlet of the boron trichloride purification system is communicated with an outlet of the second pipeline; the inlet of the third pipeline is communicated with the discharge hole of the boron trichloride purification system; the second Fourier infrared spectrum detection system comprises a second sample cell, a feed inlet of the second sample cell is communicated with an outlet of the third pipeline, a feed inlet of the second buffer tank is communicated with a discharge outlet of the second sample cell, a feed inlet of the second vacuum pump is communicated with a discharge outlet of the second buffer tank, and a discharge outlet of the second vacuum pump is communicated into the alkali liquor cylinder;
the optical path of the first sample cell is 60mm, and the optical path of the second sample cell is 10 m.
2. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 1, characterized in that: the window sheets on the left side and the right side of the first sample cell and the window sheets on the left side and the right side of the second sample cell are both BaF2A window sheet.
3. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 2, characterized in that: the first sample cell with all be provided with accuse temperature and pressure control system in the second sample cell, just first sample cell with the gaseous temperature is all invariable 42 +/-0.2 ℃ in the second sample cell, and atmospheric pressure is all invariable 1 +/-0.1 standard atmospheric pressure.
4. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 3, characterized in that: the first Fourier infrared spectrum detection system further comprises a first detector, a first FTIR spectrometer, a first infrared source and first control analysis software; the first detector is arranged on one side of the first sample pool; the first FTIR spectrometer is arranged on the other side of the first sample cell; the first infrared light source is arranged on the other side of the first FTIR spectrometer; the first control analysis software is electrically connected with the first detector, the first FTIR spectrometer and the first infrared light source.
5. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 4, characterized in that: the first Fourier infrared spectrum detection system detects impurity gas components in the boron trichloride crude product and the concentration range is as follows: CH (CH)4：100-200ppm、CO：100-150ppm、CO2：100-200ppm，HCl：100-300ppm、COCl2：1-200ppm、SiCl4：100-300ppm、SiH2Cl2：1-200ppm。
6. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 3, characterized in that: the second Fourier infrared spectrum detection system also comprises a second detector, a second FTIR spectrometer, a second infrared source and second control analysis software; the second detector is arranged on one side of the second sample cell; the second FTIR spectrometer is arranged on the other side of the second sample cell; the second infrared light source is arranged on the other side of the second FTIR spectrometer; and the second control analysis software is electrically connected with the second detector, the second FTIR spectrometer and the second infrared light source.
7. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 6, characterized in that: the second Fourier infrared spectrum detection system detects impurity gas components and concentration ranges in the boron trichloride finished product as follows: CH (CH)4：0.01-0.5ppm、CO：0.1-0.5ppm、CO2：0.1-2ppm、HCl：0.1-1ppm、COCl2：0.1-1ppm、SiCl4：0.05-2ppm、SiH2Cl2：0.1-1ppm。
8. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 1, characterized in that: the gas outlet of the helium tank is communicated with the first pipeline and the third pipeline through a three-way valve respectively to form a gas path system, and the gas path system is constant at 42 +/-0.2 ℃ for heat tracing.
9. The impurity gas detection device of the electronic grade boron trichloride purification system according to claim 8, characterized in that: and the first pipeline and the third pipeline are both provided with a pressure reducing valve and a flowmeter.
10. The detection method of the impurity gas detection device of the electronic grade boron trichloride purification system according to claim 1, characterized by comprising the following steps: starting a first vacuum pump, filling a part of boron trichloride crude products in a crude product storage tank into a first sample tank of a first Fourier infrared spectrum detection system through a first pipeline, after detection and analysis, leading the boron trichloride crude products into an alkali liquid cylinder through an outlet of the first sample tank and a first buffer tank, and neutralizing the detected boron trichloride crude products by the alkali liquid cylinder; starting a second vacuum pump, introducing the other part of the boron trichloride crude product in the crude product storage tank into a boron trichloride purification system through a second pipeline to further generate a high-purity electronic-grade boron trichloride finished product, introducing the electronic-grade boron trichloride finished product into a second sample pool of a second Fourier infrared spectrum detection system through a third pipeline, introducing the electronic-grade boron trichloride finished product into an alkali liquid cylinder through an outlet of the second sample pool and a second buffer tank, and neutralizing the detected electronic-grade boron trichloride finished product by the alkali liquid cylinder; or the first vacuum pump and the second vacuum pump are started simultaneously to realize the simultaneous detection of impurity gases in the boron trichloride crude product and the finished product, and the alkali liquor cylinder neutralizes the detected boron trichloride crude product and the finished product simultaneously.
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