CN111141505A - Non-invasive vacuum partial pressure rapid measuring instrument - Google Patents

Non-invasive vacuum partial pressure rapid measuring instrument Download PDF

Info

Publication number
CN111141505A
CN111141505A CN201911362626.6A CN201911362626A CN111141505A CN 111141505 A CN111141505 A CN 111141505A CN 201911362626 A CN201911362626 A CN 201911362626A CN 111141505 A CN111141505 A CN 111141505A
Authority
CN
China
Prior art keywords
frequency comb
vacuum
optical frequency
optical
light
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201911362626.6A
Other languages
Chinese (zh)
Inventor
代虎
李得天
李毅
高文生
王永军
李居平
郭睿
嘉露娟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lanzhou Institute of Physics of Chinese Academy of Space Technology
Original Assignee
Lanzhou Institute of Physics of Chinese Academy of Space Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lanzhou Institute of Physics of Chinese Academy of Space Technology filed Critical Lanzhou Institute of Physics of Chinese Academy of Space Technology
Priority to CN201911362626.6A priority Critical patent/CN111141505A/en
Publication of CN111141505A publication Critical patent/CN111141505A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M13/00—Testing of machine parts
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L15/00—Devices or apparatus for measuring two or more fluid pressure values simultaneously
    • G—PHYSICS
    • 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
    • G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths

Landscapes

  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention relates to a non-invasive vacuum partial pressure rapid measuring instrument, and belongs to the technical field of vacuum partial pressure measurement. The instrument adopts the optical frequency comb as a gas probe, combines the double-optical comb heterodyne spectrum technology with the cavity enhancement technology, effectively increases the working waveband and the spectral resolution, improves the signal-to-noise ratio and the sensitivity, shortens the test time, and realizes the non-contact, high-precision, high-speed and wide-range measurement of the vacuum partial pressure of various gases.

Description

Non-invasive vacuum partial pressure rapid measuring instrument
Technical Field
The invention relates to a non-invasive vacuum partial pressure rapid measuring instrument, and belongs to the technical field of vacuum partial pressure measurement.
Background
The vacuum partial pressure measurement technology can analyze gas components in vacuum and measure component pressure of the gas components, is an indispensable technology in a plurality of research and production fields, and provides a large amount of effective information for a vacuum system. In recent years, with the rapid development of advanced high and new technologies in China, partial pressure measurement technology has urgent needs in the fields of aerospace, high-energy nuclear physics, semiconductor industry, nano material technology and the like.
The mass spectrometry is the most widely used and longest-used vacuum partial pressure measurement method, and the commonly used partial pressure mass spectrometers comprise a magnetic deflection mass spectrometer, a flight time mass spectrometer, a quadrupole mass spectrometer and the like, wherein the quadrupole mass spectrometer firmly occupies the dominant position of the partial pressure measurement instrument due to the advantages of no use of a magnetic field, linear scale and simple and efficient ion source, the calibrated quadrupole mass spectrometer has low precision and uncertain measurement of about 10 percent, and has four difficult-to-overcome principle defects of limited application range of ① ionization measurement, difficult ② calibration and inconvenient use, no resolution of molecules with the same mass number by ③, limited working pressure of ④ and no direct measurement of rough and low vacuum (10)-2Pa～105Pa)。
In view of the dilemma faced by the traditional mass spectrometry for measuring partial pressure, the german Federal physical technology research institute proposed in 2005 a technology for measuring vacuum partial pressure by adopting a tuned diode laser absorption spectroscopy, which measures the spectral intensity attenuation of laser passing through gas by using spectroscopy, and then deduces the partial pressure of target gas in mixed gas according to the lambert-beer law, the laser absorption spectroscopy is a very potential vacuum partial pressure measuring method, has high measuring precision and good traceability, but the tuned diode absorption spectroscopy has the obvious defects that ① does not have multi-gas detection capability, ② speed is slow, and cannot adapt to dynamic measurement, ③ spectral resolution is low, so that the potential of laser absorption spectroscopy cannot be fully exerted, and the fundamental reason that the light source wave band of TDLAS (tuned diode laser absorption spectroscopy) is too narrow and the spectrum information acquisition mode is very tedious and slow, however, the acquisition of broadband, ultrahigh resolution and spectral data is always a difficult problem in the technical field of traditional spectral analysis, and the requirements of filtered, scanned, dispersive and Fourier transform spectrometers cannot be met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a non-invasive vacuum partial pressure rapid measuring instrument, which adopts an optical frequency comb as a gas probe, combines a double-optical comb heterodyne spectrum technology with a cavity enhancement technology, effectively increases the working waveband and the spectrum resolution, improves the signal-to-noise ratio and the sensitivity, shortens the testing time, and realizes the non-contact, high-precision, high-speed and wide-range measurement of the vacuum partial pressure of various gases.
The purpose of the invention is realized by the following technical scheme.
A non-invasive vacuum partial pressure rapid measuring instrument comprises an optical frequency comb I-I, an optical comb self-reference module, a beam splitter I-I, a photoelectric detector I-I, a resonant reflector I-I, a temperature sensor, a pressure sensor, a vacuum sample cavity, a vacuum pumping system, a sample feeding system and a data processing module;
the optical frequency comb I and the optical frequency comb I have the same reference frequency and different repetition frequencies, and the repetition frequency difference value is preferably not more than 1 MHz;
the resonant reflector I and the resonant reflector I are symmetrically arranged at two ends of a cavity of the vacuum sample cavity and are used for amplifying the effective acting distance between a light beam and sample gas, namely the effective optical path; the temperature sensor and the pressure sensor are arranged in the vacuum sample cavity and are used for measuring the temperature and the total pressure of sample gas in the vacuum sample cavity; the sample introduction system is connected with the vacuum sample cavity and provides sample gas for the vacuum sample cavity; the vacuum pumping system is connected with the vacuum sample cavity to ensure the vacuum degree of the vacuum sample cavity; the optical frequency comb self-reference module is used for controlling the output reference frequency and the repetition frequency of the optical frequency comb I and the optical frequency comb I; the light-frequency comb I is characterized in that a beam splitter I is arranged on an emergent light path of the light-frequency comb I and used for dividing an emergent light beam into two beams of light of a sampling light beam and two beams of light of a reference light beam, and a beam splitter I is arranged on the emergent light path of the light-frequency comb I and used for dividing the emergent light beam into two beams of light of the sampling light beam and the two beams of; the optical frequency comb I is characterized in that a vacuum sample cavity, a beam splitter III and a photoelectric detector I are sequentially arranged on a light path of a sampling light beam of the optical frequency comb I, the beam splitter III and the photoelectric detector I are sequentially located on the light path of the sampling light beam of the optical frequency comb I, the sampling light beam of the optical frequency comb I is coupled into the vacuum sample cavity to be fully acted with sample gas, and then is coupled with the sampling light beam of the optical frequency comb I to generate interference, and a beat frequency signal generated after the sampling light beam is received by the photoelectric detector I; a beam splitter I and a photoelectric detector I are sequentially arranged on the light path of the reference beam of the optical frequency comb I, the beam splitter I and the photoelectric detector I are sequentially located on the light path of the reference beam of the optical frequency comb I, and beat frequency signals generated after the reference beam of the optical frequency comb I and the reference beam of the optical frequency comb I are coupled and interfered by the beam splitter I are received by the photoelectric detector I; the data processing module calculates the partial pressure of the target gas according to the received signals from the photoelectric detector I, the temperature sensor and the pressure sensor.
Further, before the sample gas is filled into the vacuum sample cavity, the vacuum degree in the vacuum sample cavity is less than 1 multiplied by 10-5Pa。
Has the advantages that:
(1) the invention uses the optical frequency comb (namely the optical frequency comb) as the gas probe, and the gas can be measured without ionizing the gas, thereby realizing non-invasive detection;
(2) the invention utilizes the broadband characteristic of the optical frequency comb to effectively widen the effective working waveband of the instrument and realize the synchronous measurement of various gases;
(3) the invention adopts a double-frequency comb heterodyne interference method to obtain spectral information, so that the time consumed by one-time measurement of an instrument is only tens of milliseconds;
(4) the optical path is improved by more than 3 orders of magnitude by adopting the cavity enhancement technology, and the sensitivity and the signal-to-noise ratio of the measuring instrument are effectively improved.
Drawings
FIG. 1 is a schematic optical path diagram of the non-invasive vacuum partial pressure rapid measurement instrument according to the embodiment.
The optical frequency comb comprises a 1-optical frequency comb I, a 2-optical frequency comb self-reference module, a 3-optical frequency comb I, a 4-beam splitter I, a 5-resonant reflector I, a 6-vacuum sample cavity, a 7-gas molecule, an 8-beam splitter III, a 9-photoelectric detector I, a 10-photoelectric detector I, an 11-optical path reflector I, a 12-beam splitter I, a 13-beam splitter I and a 14-optical path reflector I.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1
As shown in figure 1, a non-invasive vacuum partial pressure rapid measuring instrument comprises an optical frequency comb I1, an optical frequency comb I3, an optical comb self-reference module 2, a beam splitter I12, a beam splitter I4, a beam splitter III 8, a beam splitter I13, an optical path reflector I11, an optical path reflector I14, a photoelectric detector I9, a photoelectric detector I10, a resonant reflector I5, a resonant reflector I, a temperature sensor, a pressure sensor, a vacuum sample cavity 6, a vacuumizing system, a sample introduction system and a data processing module;
the optical frequency comb I1 and the optical frequency comb I3 have the same reference frequency, and the repetition frequency difference value is 0.5 MHz;
the resonance reflector I5 and the resonance reflector I are symmetrically arranged at two ends of a vacuum sample cavity 6, the temperature sensor and the pressure sensor are arranged in the vacuum sample cavity 6, and the vacuum sample cavity 6 is respectively connected with a sample introduction system and a vacuum pumping system; the optical frequency comb I1 and the optical frequency comb I3 are respectively connected with the optical comb self-reference module 2; a beam splitter I12 is arranged on an emergent light path of the light frequency comb I1 and used for dividing an emergent light beam into two beams of light of a sampling light beam and two beams of light of a reference light beam, and a beam splitter I4 is arranged on an emergent light path of the light frequency comb I3 and used for dividing the emergent light beam into two beams of light of the sampling light beam and the two beams of light of the reference light beam; a vacuum sample cavity 6, a beam splitter III 8 and a photoelectric detector I9 are sequentially arranged on the light path of the sampling light beam of the light frequency comb I3, and a light path reflector I11, the beam splitter III 8 and the photoelectric detector I10 are sequentially arranged on the light path of the sampling light beam of the light frequency comb I1; an optical path reflector I14, a beam splitter I13 and a photoelectric detector I10 are sequentially arranged on an optical path of a reference beam of the optical frequency comb I3, and meanwhile, the beam splitter I13 and the photoelectric detector I10 are sequentially located on an optical path of the reference beam of the optical frequency comb I1; photoelectric detector I9, photoelectric detector I10, temperature sensor and pressure sensor are connected with data processing module respectively.
The operation of measuring the partial pressure of the target gas by using the non-invasive vacuum partial pressure rapid measuring instrument according to the embodiment is as follows:
firstly, pumping the air pressure in the vacuum sample cavity 6 to 1 x 10 by a vacuum pumping system-5Below Pa, mixing gas (containing CH) with standard sample to be measured by sample injection system4、C2H4、C2H6And N2) Is introduced into the vacuum sample cavity 6; wherein, CH4Partial pressure of 1.75X 10-2Pa、C2H4Partial pressure of 6Pa, C2H6The partial pressure of (A) is 20 Pa;
step two, after the optical frequency comb I1 and the optical frequency comb I3 are started, the photoelectric detector I9 and the photoelectric detector I10 start to synchronously record light intensity signals, the signal period is 2 microseconds, 1000 periods are collected for improving the signal to noise ratio, the time is consumed for 2 milliseconds, the collected light intensity signals are subjected to Fourier transform through the data processing module, and the frequency spectrum distribution I of the beat frequency signals is obtained0(v) and I (v);
step three, detecting the light intensity I of the incident sample gas by the photoelectric detector I100(v) carrying out spectrum calibration on light intensity I (v) emitted from the sample gas and detected by a photoelectric detector I9;
step four, preprocessing the spectral absorption data to filter out low-frequency and high-frequency noises, normalizing the spectral data after baseline correction, extracting characteristic absorption peaks and solving the integral absorption A of the target gasabs；
Figure 1
Step five, calculating the molecular number density n of the target gas according to the Lambert-beer law, and then calculating the partial pressure P of the target gas according to an ideal gas formulapartial；
Figure BDA0002337606230000042
Ppartial＝n·k·T
CH4、C2H4And C2H6The partial pressures were calculated separately using a number of absorptions and averaged as a measurement. CH (CH)4、C2H4And C2H6The partial pressure measurement results of (1.7X 10)-2Pa, 5.91Pa and 20.3Pa, which are highly consistent with the preparation concentration of the standard sample mixed gas. The whole measurement process takes about 2ms, the spectral resolution is 100MHz, and the signal-to-noise ratio can reach 35 dB; in addition, the length of the vacuum sample cavity 6 is only 10cm in the embodiment, but under the action of the resonant mirror I5 and the resonant mirror I, the light can be reflected for more than 100 times in the vacuum sample cavity 6, so that the effective absorption length can reach 10 m.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. A non-invasive vacuum partial pressure rapid measurement instrument is characterized in that: the instrument comprises an optical frequency comb I-I, an optical comb self-reference module, a beam splitter I-I, a photoelectric detector I-I, a resonant reflector I-I, a temperature sensor, a pressure sensor, a vacuum sample cavity, a vacuum pumping system, a sample introduction system and a data processing module; the optical frequency comb I and the optical frequency comb I have the same reference frequency and different repetition frequencies;
the resonant reflector I and the resonant reflector I are symmetrically arranged at two ends of a cavity of the vacuum sample cavity, the temperature sensor and the pressure sensor are arranged in the vacuum sample cavity, and the sample introduction system and the vacuum pumping system are respectively connected with the vacuum sample cavity; the optical frequency comb self-reference module is used for controlling the output reference frequency and the repetition frequency of the optical frequency comb I and the optical frequency comb I; the light-frequency comb I is characterized in that a beam splitter I is arranged on an emergent light path of the light-frequency comb I and used for dividing an emergent light beam into two beams of light of a sampling light beam and two beams of light of a reference light beam, and a beam splitter I is arranged on the emergent light path of the light-frequency comb I and used for dividing the emergent light beam into two beams of light of the sampling light beam and the two beams of; the optical frequency comb I is characterized in that a vacuum sample cavity, a beam splitter III and a photoelectric detector I are sequentially arranged on the optical path of a sampling light beam of the optical frequency comb I, and the beam splitter III and the photoelectric detector I are sequentially positioned on the optical path of the sampling light beam of the optical frequency comb I; the optical frequency comb I is characterized in that a beam splitter I and a photoelectric detector I are sequentially arranged on the optical path of a reference beam of the optical frequency comb I, and the beam splitter I and the photoelectric detector I are sequentially located on the optical path of the reference beam of the optical frequency comb I; the data processing module calculates the partial pressure of the target gas according to the received signals from the photoelectric detector I, the temperature sensor and the pressure sensor.
2. A non-invasive vacuum partial pressure rapid measuring instrument according to claim 1, wherein: the frequency difference between the optical frequency comb I and the optical frequency comb I is not more than 1 MHz.
3. A non-invasive vacuum partial pressure rapid measuring instrument according to claim 1, wherein: before the sample gas is not filled into the vacuum sample cavity, the vacuum degree in the vacuum sample cavity is less than 1 multiplied by 10-5Pa。
CN201911362626.6A 2019-12-26 2019-12-26 Non-invasive vacuum partial pressure rapid measuring instrument Pending CN111141505A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911362626.6A CN111141505A (en) 2019-12-26 2019-12-26 Non-invasive vacuum partial pressure rapid measuring instrument

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911362626.6A CN111141505A (en) 2019-12-26 2019-12-26 Non-invasive vacuum partial pressure rapid measuring instrument

Publications (1)

Publication Number Publication Date
CN111141505A true CN111141505A (en) 2020-05-12

Family

ID=70520220

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911362626.6A Pending CN111141505A (en) 2019-12-26 2019-12-26 Non-invasive vacuum partial pressure rapid measuring instrument

Country Status (1)

Country Link
CN (1) CN111141505A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111624169A (en) * 2020-06-03 2020-09-04 华东师范大学 Heterodyne detection-based ultraviolet double-optical-comb absorption spectrum measurement device and method
CN114674486A (en) * 2021-12-24 2022-06-28 兰州空间技术物理研究所 Rapid vacuum partial pressure measuring device and method
CN116625946A (en) * 2023-05-29 2023-08-22 电子科技大学 CMOS frequency comb Fourier transform rotation spectrum detector

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102183486A (en) * 2011-01-28 2011-09-14 清华大学 Gas refractive index measurer and measuring method thereof based on optical frequency comb
CN102346140A (en) * 2011-06-17 2012-02-08 清华大学 Air refractive index measurement system and measurement method thereof
CN110411650A (en) * 2019-07-31 2019-11-05 中国科学院微电子研究所 Vacuum measurement method and device based on frequency comb

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102183486A (en) * 2011-01-28 2011-09-14 清华大学 Gas refractive index measurer and measuring method thereof based on optical frequency comb
CN102346140A (en) * 2011-06-17 2012-02-08 清华大学 Air refractive index measurement system and measurement method thereof
CN110411650A (en) * 2019-07-31 2019-11-05 中国科学院微电子研究所 Vacuum measurement method and device based on frequency comb

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CODDINGTON I 等: "Coherent multiheterodyne spectroscopy using stabilized optical frequency combs", 《PHYSICAL REVIEW LETTERS》 *
董贺伟 等: "光梳光谱仪技术及其应用", 《计量技术》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111624169A (en) * 2020-06-03 2020-09-04 华东师范大学 Heterodyne detection-based ultraviolet double-optical-comb absorption spectrum measurement device and method
CN114674486A (en) * 2021-12-24 2022-06-28 兰州空间技术物理研究所 Rapid vacuum partial pressure measuring device and method
CN114674486B (en) * 2021-12-24 2023-06-20 兰州空间技术物理研究所 Quick vacuum partial pressure measuring device and method
CN116625946A (en) * 2023-05-29 2023-08-22 电子科技大学 CMOS frequency comb Fourier transform rotation spectrum detector
CN116625946B (en) * 2023-05-29 2024-03-19 电子科技大学 CMOS frequency comb Fourier transform rotation spectrum detector

Similar Documents

Publication Publication Date Title
CN106802288B (en) Gas-detecting device and method based on tunable laser and super continuous spectrums laser
CN101105446B (en) Differential optical absorption spectroscopy air quality detection system
CN111141505A (en) Non-invasive vacuum partial pressure rapid measuring instrument
CN110044824B (en) Quartz tuning fork-based dual-spectrum gas detection device and method
JP6022456B2 (en) Method and system for determining the decay constant of a time domain signal
CN107063553B (en) A kind of device and method using Wavelength modulation spectroscopy measurement gas pressure intensity and concentration of component
CN108709871B (en) TDLAS-based gas concentration detection method
CN102262075B (en) Method for measuring elemental concentration through laser-induced breakdown spectroscopy based on spectrophotometry
CN111077110B (en) Temperature field and concentration field measuring system and method based on double-optical comb spectrum
CN103115894B (en) Stable isotopic abundance ratio real-time online monitoring device and method
CN102788771B (en) Method for measuring content of powdery substantial elements based on laser-induced breakdown spectroscopy
CN106568507B (en) Feature based absorption line measures the method and device of F P chamber Free Spectral Ranges
CN106872402A (en) Gas-detecting device and method based on super continuous spectrums laser
CN111650127A (en) High-resolution photoacoustic spectroscopy gas detection system and method based on optical frequency comb frequency calibration
CN116399850B (en) Spectrum detection and identification system for optical signal processing and detection method thereof
CN114018829B (en) Double-optical comb multicomponent gas detection system with tuning fork resonance enhancement
WO2020130942A1 (en) A non-destructive system and method for determining the quality of chinese herb using terahertz time-domain spectroscopy
JP2004020539A (en) Infrared circular dichroism measuring instrument and infrared circular dichroism measuring method
CN108181261A (en) Device based on terahertz time-domain spectroscopy detection mixed gas each component content
CN106769878B (en) Photoacoustic spectrum-based traditional Chinese medicine decoction component detection method and device
CN101403687A (en) Method for detecting infrared spectrometer stability based on monocrystaline silicon piece
CN111272736B (en) Breakdown spectrum and absorption spectrum combined measurement system and method
CN110346346B (en) Raman gas detection method based on compressed sensing correlation algorithm
CN111751317A (en) Novel method and system for determining components of gynostemma pentaphylla by utilizing terahertz spectrum technology
Wang et al. A measurement method in near infrared spectroscopy for reference correction with the homologous optical beams

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20200512

WD01 Invention patent application deemed withdrawn after publication