CN109461642B - Ion-initiated electron bombardment ionization source - Google Patents

Ion-initiated electron bombardment ionization source Download PDF

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Publication number
CN109461642B
CN109461642B CN201811491709.0A CN201811491709A CN109461642B CN 109461642 B CN109461642 B CN 109461642B CN 201811491709 A CN201811491709 A CN 201811491709A CN 109461642 B CN109461642 B CN 109461642B
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electron
photoionization
vacuum ultraviolet
area
ionization
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CN109461642A (en
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崔华鹏
陈黎
樊美娟
秦亚琼
王晓瑜
李翔
潘立宁
蔡君兰
刘绍锋
谢复炜
刘惠民
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Zhengzhou Tobacco Research Institute of CNTC
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Zhengzhou Tobacco Research Institute of CNTC
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/14Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/08Electron sources, e.g. for generating photo-electrons, secondary electrons or Auger electrons

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

An ion-initiated electron bombardment ionization source, characterized by: the vacuum ultraviolet light source is arranged in the cavity, and the vacuum ultraviolet light source is positioned in the cavity and sequentially comprises a photoionization area, an electron generation area and an electron bombardment ionization area along the light emitting direction; the vacuum ultraviolet light source is used for generating vacuum ultraviolet photons, and photoionization is carried out on the introduced standard gas molecules in the photoionization region so as to generate primary ions; after the primary ions are accelerated by an electric field, the primary ions enter an electron generation region and bombard the surface of an electron amplification microchannel plate to generate a large number of electrons; after the electrons are accelerated by an electric field, the electrons enter an electron bombardment ionization region, and the electrons bombard and ionize introduced gas molecules to generate ions; ions enter the mass analyzer of the mass spectrum through the ion transport region. The invention has the beneficial effects that the electron amplification effect of the electron amplification microchannel plate is utilized, and the electron number of the electron bombardment ionization source can be greatly improved, so that the ionization efficiency of the ionization source is improved.

Description

Ion-initiated electron bombardment ionization source
Technical Field
The invention belongs to the field of mass spectrometry, and particularly relates to an ion-initiated electron bombardment ionization source. The method utilizes vacuum ultraviolet photons to photoionization of standard gas to generate primary ions; electron bombardment is carried out on the electron amplification microchannel plate to generate electrons; the electrons are accelerated for electron bombardment ionization of the sample gas molecules.
Background
Electron bombardment ionization sources are the most widely used ionization means for gas molecules at present. The working principle is as follows: under a certain vacuum condition, when current passes through the filament, the temperature of the filament is up to 2000 ℃, the random movement of free electrons in the filament is aggravated, when the kinetic energy of electrons is larger than the work function of the metal surface, thermionic emission can be generated, the emitted electrons are accelerated under the ionization voltage to obtain energy, and gas molecules are ionized by collision gas. The ionization source has the advantages of simple structure and convenient operation. The ionization efficiency of an electron bombardment ionization source is directly related to the number of electrons emitted, which is mainly determined by the current intensity. Too low a current level directly affects the ionization efficiency of the ionization source, while too high a current level affects the lifetime of the ionization source.
Disclosure of Invention
The invention aims to develop an ion-initiated electron bombardment ionization source, which utilizes vacuum ultraviolet photons to photoionization standard gas to generate primary ions; electron bombardment is carried out on the electron amplification microchannel plate to generate electrons; the electrons are accelerated for electron bombardment ionization of the sample gas molecules. The method utilizes the electron amplification effect of the electron amplification microchannel plate, and can greatly improve the electron number of the electron bombardment ionization source, thereby improving the ionization efficiency.
The aim of the invention is realized by the following technical scheme:
an ion-initiated electron bombardment ionization source comprises a metal cavity, a vacuum ultraviolet light source arranged in the cavity, and a photoionization area, an electron generation area and an electron bombardment ionization area which are sequentially arranged in the cavity along the light emergent direction;
the connection parts among the photoionization area, the electron generation area and the electron bombardment ionization area are respectively provided with an air pressure difference port, and the photoionization area and the electron generation area are respectively provided with an extraction port which are connected with a vacuum pump;
an electron amplifying microchannel plate combination is arranged in the electron generating region, and the number of the electron amplifying microchannel plate combination is 2-4; a direct-current voltage is arranged between the electron amplification microchannel plates so as to form an electric field gradient;
a standard gas sample injection pipeline is arranged in the photoelectric ionization region, and a sample injection pipeline is arranged in the electron bombardment ionization region;
the vacuum ultraviolet light source generates vacuum ultraviolet photons, the introduced standard gas molecules are photoionization in the photoionization region to generate primary ions, the primary ions enter the electron generation region after being accelerated by an electric field, bombarding electrons to amplify the surface of the microchannel plate to generate a large number of electrons, and the electrons enter the electron bombardment ionization region after being accelerated by the electric field to carry out electron bombardment ionization on the introduced gas sample molecules to generate ions.
The vacuum ultraviolet light source is a vacuum ultraviolet lamp or an ultraviolet laser light source, the photon energy of the vacuum ultraviolet light source is higher than the ionization energy of the standard gas, and the vacuum ultraviolet light source can photoionization the standard gas molecules.
The repulsion electrode of the photoelectric separation area is provided with a repulsion electrode which can accelerate ions into the electron generation area. The DC voltage between the electron amplifying micro-channel plates is 500-800V to form 2.5×10 5 -4×10 5 V/m electric field gradient.
The mechanism or working process of the invention is as follows: photon beams of the vacuum ultraviolet light source are directly injected into the photoionization area, and a standard gas sample injection pipeline is arranged at the side of the photoionization area and can be a quartz capillary or a metal capillary; standard gas enters a photoionization area through a sample injection pipeline and reaches a beam area of vacuum ultraviolet light, and vacuum ultraviolet photons are used for photoionization of standard gas molecules to generate primary ions. The molecular ionization energy of the standard gas is lower than the photon energy of vacuum ultraviolet light, and benzene compounds with low boiling point generally have higher sensitivity in a photoionization mode and can be used as the preferable standard gas of a photon-induced electron bombardment ionization source. The repulsion electrode of the ionization region is provided with a repulsion voltage, so that primary ions ionized by the standard gas can be accelerated into the electron generation region under the action of an acceleration electric field.
The electron generation area is internally provided with electron amplification microchannel plate combinations, the number of which is 2-4; direct-current voltage is arranged between the electron amplification microchannel plates to form an electric field gradient. The electron amplification microchannel plate has the function of electron amplification gain, and when ions bombard the surface of the first-stage electron amplification microchannel plate, the ions repeatedly collide with the first-stage electron amplification microchannel plate in the microchannel plate, and a large amount of electrons are sputtered; then, the electrons move to a second-stage electron amplification microchannel plate under the action of an accelerating electric field, and the number of electrons is further amplified; and finally forming a large number of electrons through multistage electron amplification. The electrons are accelerated to move to an electron ionization region under the action of an accelerating electric field.
A gas sample injection pipeline is arranged at the side of the electron ionization region and used for introducing a gas sample to be tested; the gas sample enters an electron bombardment ionization region, and gas molecules collide with electrons which accelerate to make the gas molecules generate electron bombardment ionization.
The beneficial effects of the invention are as follows: the invention uses vacuum ultraviolet photon to photoionization of standard gas to generate primary ion; electron bombardment is carried out on the electron amplification microchannel plate to generate electrons; the use of electron-amplifying microchannel plates greatly increases the number of available electrons, which is beneficial to providing ionization efficiency of the ionization source. Compared with the mode of directly irradiating the microchannel plate by ultraviolet light to generate electrons, which is introduced by a vacuum ultraviolet lamp mass spectrum ionization source capable of switching photoelectric modes (patent number 201721124168.9), the invention adopts the mode of ion bombardment of the microchannel plate, and the generation efficiency of electrons of the microchannel plate can be greatly improved due to the increase of ion collision cross sections, so that the ionization source has higher ionization efficiency.
Drawings
Fig. 1 is a schematic view of an ionization source of the present invention.
1. The vacuum ultraviolet light source comprises a metal cavity, a vacuum ultraviolet light source, a photoionization region, an electron generation region, an electron amplification microchannel plate, an electron bombardment ionization region, a standard gas sample injection pipeline, a repulsion electrode, a gas pressure differential port and an extraction port.
Detailed Description
The invention is further described below with reference to the embodiments of the accompanying drawings:
as shown in fig. 1: an ion-initiated electron bombardment ionization source comprises a metal cavity 1, a vacuum ultraviolet light source 2 arranged in the cavity, and a photoionization region 4, an electron generation region 4 and an electron bombardment ionization region 6 which are positioned in the cavity in sequence along the light emitting direction;
the connection parts between the photoionization area 3 and the electron generation area 4 and between the electron generation area 4 and the electron bombardment ionization area 6 are respectively provided with an air pressure difference port 10, and the photoionization area 3 and the electron generation area 4 are respectively provided with an air extraction port 11 which is connected with a vacuum pump;
an electron amplifying microchannel plate 5 is arranged in the electron generating region 4, and the number of the electron amplifying microchannel plates is 3; the DC voltage of 500V is arranged between the electron amplifying micro-channel plates to form 2.5×10 5 V/m electric field gradient.
A standard gas sample injection pipeline 7 is arranged in the photoionization region 4, and a gas sample injection pipeline 8 is arranged in the electron bombardment ionization region 6;
more specifically, the vacuum ultraviolet light source 2 may be a vacuum ultraviolet lamp filled with krypton gas, and when excited by high pressure, the vacuum ultraviolet photons can be emitted through the optical window to form photon beams. The energy of the photons emitted by the krypton vacuum ultraviolet lamp is 10.6eV, which is higher than the ionization energy of most volatile organic compounds, and is favorable for ionizing standard gas molecules to form primary ions.
Photon beams of the vacuum ultraviolet light source 2 are directly injected into the photoionization region 3, and a standard gas sample injection pipeline 7 which can be a quartz capillary is arranged at the side of the photoionization region 3; standard gas enters the photoionization zone 3 through a sample injection pipeline and reaches a beam region of vacuum ultraviolet light, and vacuum ultraviolet photons are used for photoionization of standard gas molecules to generate primary ions. The molecular ionization energy of the standard gas is lower than the photon energy of vacuum ultraviolet light, and benzene compounds with low boiling point generally have higher sensitivity in a photoionization mode and can be used as the preferable standard gas of a photon-induced electron bombardment ionization source. The repulsion electrode 9 of the photoionization region 3 is provided with a repulsion voltage, so that primary ions ionized by the standard gas can be accelerated into the electron generation region 4 under the action of an acceleration electric field.
The electron generation area 4 is internally provided with the combination of electron amplification microchannel plates 5, the number of which is 3; a dc voltage is applied between the electron-amplifying microchannel plates 5 to form an electric field gradient. The electron amplification microchannel plate 5 has the function of electron amplification gain, and when ions bombard the surface of the first-stage electron amplification microchannel plate 5, the ions repeatedly collide with the first-stage electron amplification microchannel plate in the microchannel to sputter a large amount of electrons; then, the electrons move to the second-stage electron amplifying micro-channel plate 5 under the action of the accelerating electric field, and the number of electrons is further amplified; and finally forming a large number of electrons through multistage electron amplification. The electrons are accelerated towards the electron bombardment ionization region 6 under the action of the accelerating electric field.
A gas sample injection pipeline 8 is arranged at the side of the electron bombardment ionization region 6 and used for introducing a gas sample to be detected; the gas sample enters the electron bombardment ionization region 6, and gas molecules collide with electrons which accelerate to make the gas molecules generate electron bombardment ionization.
In the ionization source, the connection parts among the photoionization area 3, the electron generation area 4 and the electron bombardment ionization area 6 are respectively provided with an air pressure difference port 10, and the photoionization area 3 and the electron generation area 4 are respectively provided with an extraction port 11 which is connected with a vacuum pump so as to adjust the vacuum degree of different areas.

Claims (2)

1. An ion-initiated electron bombardment ionization source, characterized by: the vacuum ultraviolet light source is arranged in the cavity, and the vacuum ultraviolet light source is positioned in the cavity and sequentially comprises a photoionization area, an electron generation area and an electron bombardment ionization area along the light emitting direction;
the connection parts among the photoionization area, the electron generation area and the electron bombardment ionization area are respectively provided with an air pressure difference port, the photoionization area and the electron generation area are respectively provided with an extraction port which are connected with a vacuum pump, and a repulsion electrode which can accelerate ions into the electron generation area is arranged at the repulsion electrode of the photoionization area;
a standard gas sample injection pipeline is arranged in the photoelectric ionization region, and a sample injection pipeline is arranged in the electron bombardment ionization region;
an electron amplifying microchannel plate combination is arranged in the electron generating region, and the number of the electron amplifying microchannel plate combination is 2-4; a direct-current voltage is arranged between the electron amplification microchannel plates so as to form an electric field gradient;
the vacuum ultraviolet light source is a vacuum ultraviolet lamp or an ultraviolet laser light source, the photon energy of the vacuum ultraviolet light source is higher than the ionization energy of standard gas, standard gas molecules can be photoionization, and the standard gas is a benzene series with a low boiling point and higher sensitivity in a photoionization mode;
the vacuum ultraviolet light source generates vacuum ultraviolet photons, the introduced standard gas molecules are photoionization in the photoionization region to generate primary ions, the primary ions enter the electron generation region after being accelerated by an electric field, bombarding electrons to amplify the surface of the microchannel plate to generate a large number of electrons, and the electrons enter the electron bombardment ionization region after being accelerated by the electric field to carry out electron bombardment ionization on the introduced gas sample molecules to generate ions.
2. The ion-initiated electron bombardment ionization source of claim 1 wherein: the DC voltage between the electron amplifying micro-channel plates is 500-800V to form 2.5×10 5 -4×10 5 V/m electric field gradient.
CN201811491709.0A 2018-12-07 2018-12-07 Ion-initiated electron bombardment ionization source Active CN109461642B (en)

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CN112151352B (en) * 2020-09-24 2024-01-26 中国科学院合肥物质科学研究院 Mass spectrum sample injection ionization device and working method thereof

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