CN115360079A - Electron collision ion source based on electron beam three-dimensional potential well storage - Google Patents

Electron collision ion source based on electron beam three-dimensional potential well storage Download PDF

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CN115360079A
CN115360079A CN202211034442.9A CN202211034442A CN115360079A CN 115360079 A CN115360079 A CN 115360079A CN 202211034442 A CN202211034442 A CN 202211034442A CN 115360079 A CN115360079 A CN 115360079A
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anode
electrode
grid
electron
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CN115360079B (en
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曲三标
单旭
陈向军
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University of Science and Technology of China USTC
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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
    • H01J49/147Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes

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Abstract

The invention relates to an electron impact ion source based on electron beam three-dimensional potential well storage, and belongs to the technical field of mass spectrometers. Comprises an electron gun and an ionization chamber. The electron gun comprises a delay electrode, an annular filament electrode, a grid electrode, a modulation electrode and an anode; the ionization chamber is the spatial region enclosed by the central recesses of the first and second anodes. The electron impact storage ion source of the invention firstly utilizes the space charge effect of the toroidal electron beam to prepare a narrow and deep three-dimensional potential well, and realizes high-efficiency and long-time storage of ions. The method has the characteristics of high storage efficiency, long time, small non-point source effect and the like, the sensitivity of the method is improved by 2-3 orders of magnitude compared with the ultimate sensitivity of the traditional non-storage ion source, the method is widely applied to mass spectrometry instruments, especially portable miniaturized equipment, has wide application prospect for trace substance analysis, and has potential application value in the detection field of trace substances and isotopes in the interplanetary space.

Description

Electron collision ion source based on electron beam three-dimensional potential well storage
Technical Field
The invention belongs to the technical field of mass spectrometers, and particularly relates to an electron impact ion source based on electron beam three-dimensional potential well storage, which is widely applied to trace substance detection.
Background
Mass spectrometers are one of the important instruments used to measure the composition of matter, and the ion source is the core part of the mass spectrometer, determining the mass resolution and sensitivity of the mass spectrometer. The Electron Impact (EI) ion source is a commonly used ion source in a mass spectrometer, plays an important role in the mass spectrometer, and can improve the sensitivity of the mass spectrometer by more than two orders of magnitude by the electron impact ion source with a storage function, so that the electron impact ion source can measure the substance components of trace substances and dilute gas. Currently, there are two main ways to implement ion storage: one is one-dimensional potential well formed by adopting an electrostatic field of an electrode to restrain ions; the other is to use the space charge effect of the linear electron beam to generate a potential well, restrain ions in the direction vertical to the electron beam, and cause the ions to be lost because of no restraint function in other directions. Both methods have difficulty achieving efficient long-term ion storage.
Disclosure of Invention
The electron collision ion source based on electron beam three-dimensional potential well storage has the characteristics of high storage efficiency, long time, small non-point source effect and the like, greatly improves the sensitivity of a mass spectrometer, and is widely used for detecting trace substances and isotopes.
An electron impact ion source based on electron beam three-dimensional potential well storage comprises an electron gun and an ionization chamber; the electron gun comprises an electron repulsion electrode 5, a filament electrode 10, a first grid 4, a second grid 6, a first modulation electrode 3, a second modulation electrode 7, a first anode 2 and a second anode 8; annular slits are formed between the axial corresponding ends of the first grid 4 and the second grid 6, between the axial corresponding ends of the first modulation electrode 3 and the second modulation electrode 7, and between the axial corresponding ends of the first anode 2 and the second anode 8; the ionization chamber 30 is a space region enclosed between the corresponding axial ends of the first anode 2 and the second anode 8, and the ionization chamber 30 comprises the first anode 2 and a grid 16 thereon, and the second anode 8 and a grid electrode 17 thereon; the electron repulsion electrode 5 is in a tire shape, and the improvement is as follows:
more than three insulating screws 14 and two metal screws 20 are uniformly distributed in the circumferential radial direction of the electronic repulsion electrode 5; the filament electrode 10 is fixed at the inner ends of more than three insulating screws 14; the nut ends of the two metal screws 20 are inner ends and are respectively connected with two ends of the filament electrode 10; the outer ends of the two metal screws 20 are respectively connected with the anode and the cathode of a current source;
the filament electrode 10 is a circular filament electrode with an opening, is coaxially positioned in the central hole of the electron repulsion electrode 5, and surrounds the annular slit between the first grid 4 and the second grid 6;
a gas inlet 32 is formed in the center of the axial end face of the first anode 2, an ion outlet is formed in the center of the axial end face of the second anode 8, and the gas inlet 32 and the ion outlet are coaxial;
a first grid 16 is arranged on a gas inlet 32 of the first anode 2, and a second grid 17 is arranged on an ion outlet of the second anode 8;
a first convex ring 28 is arranged on the circumference of the axial end face of the first anode 2, and a second convex ring 29 is arranged on the circumference of the axial end face of the second anode 8, so that a narrow ring groove is formed on the circumference of the ionization chamber 30;
when the ionization chamber is in work, a constant current with a typical value of 1.8A is introduced into the filament electrode 10, the filament electrode 10 can emit thermal electrons, the electrons converge towards the central region of the ionization chamber 30 and obtain 70eV energy under the combined action of electric fields of the electron repulsion electrode 5, the first grid 4, the second grid 6, the first modulation electrode 3, the second modulation electrode 7, the first anode 2 and the second anode 8, and a disk-shaped spatial distribution is formed in the ionization chamber, wherein the axial thickness of the disk-shaped spatial distribution is less than or equal to 0.5mm, and the radial radius of the disk-shaped spatial distribution is 8mm. The space charge effect of electrons forms a three-dimensional potential well in an ionization chamber, the three-dimensional potential well is very deep and narrow in the axial direction and the radial direction, the maximum depth of the potential well is 2.87V, the axial half-depth width is 0.8 to 1mm, and the radial half-depth width is 1.8 to 2mm, ions generated by electron collision can be constrained to the space size of 0.25mm multiplied by 1mm in the three directions, so that the high-efficiency long-time storage of ion clusters can be realized, and the sensitivity of a mass spectrometer is improved by 1-2 orders of magnitude; and the non-point source effect of the ion beam cluster is small, the flight time of the compressed ion cluster is dispersed by 50%, and the mass resolution of the mass spectrometer is improved.
The further technical scheme is as follows:
the distance between the axial inner end surface of the first modulation electrode 3 and the axial inner end surface of the second modulation electrode 7 in the electron gun, the distance between the axial inner end surface of the first grid 4 and the axial inner end surface of the second grid 6, and the distance L1 between the axial inner end surface of the first anode 2 and the axial inner end surface of the second anode 8 are 1mm; distances L3 between the electron repulsion electrodes 5 and the radial directions of the first grid 4 and the second grid 6, between the first grid 4 and the radial directions of the second grid 6 and the radial directions of the first modulation electrode 3 and the second modulation electrode 7, and between the first modulation electrode 3 and the radial directions of the second modulation electrode 7 and the radial directions of the first anode 2 and the second anode 8 are all 1mm.
The end of each insulating screw 14 is located in the central hole of the electron repulsion electrode 5, a radial mounting hole is formed in the end of each insulating screw 14, the middle of the filament electrode 10 penetrates through the mounting holes of more than three insulating screws 14, and the filament electrode 10 is supported by more than three insulating screws 14.
The two metal screws 20 are fixedly arranged on the electron repulsion electrode 5 through an insulating washer 23 and an insulating clamping groove 24, and cap ends of the two metal screws 20 are positioned in a central hole of the electron repulsion electrode 5 and are respectively and fixedly connected with two ends of the filament electrode 10.
The axial width L2 of the ionization chamber 30 is 3mm, and the groove width of the narrow ring groove on the circumference of the ionization chamber 30 is 1mm; the first grid 16 is fixed on the groove surface of the first anode 2 through a first metal gasket 26; the second grid 17 is fixed on the groove surface of the second anode 8 by a second metal gasket 27.
The beneficial technical effects of the invention are embodied in the following aspects:
1. the invention prepares a narrow and deep three-dimensional potential well by utilizing the space charge effect of the toroidal electron beam for the first time, and realizes the high-efficiency and long-time storage of ions. As shown in fig. 8 and fig. 9, under the condition of electron beams (flow intensity 300 μ a, energy 70 eV) which can be realized in a laboratory, the simulation experiment obtains the potential distribution of the three-dimensional potential wells XY and XZ plane formed by the electron space charge effect, the maximum depth of the three-dimensional potential well is 2.87V, the axial half-depth width is 0.8 to 1mm, and the radial half-depth width is 1.8 to 2mm.
The electron beam three-dimensional potential well improves the detection sensitivity of the ion source: the three-dimensional potential well can realize high-efficiency long-time storage of ion beam clusters, as shown in figure 10, proton clusters areThe storage efficiency in 100 mus is stored in the three-dimensional potential well, and the proton mass is stored after 100 mus, and the storage efficiency is still 90 percent. Quantitative analysis shows that the sensitivity of the instrument is improved by 1-2 orders of magnitude compared with that of a linear electron collision storage ion source, and the limit detection sensitivity is about 10 2 -10 4 /cm 3
The electron beam three-dimensional potential well reduces the time-of-flight dispersion of ion packets: the three-dimensional potential well is very narrow and deep in the axial direction and the radial direction, and can restrict the ion beam cluster to a very small size in the three directions, so that the non-point source effect of the ion beam cluster is reduced, and the mass resolution of the spectrometer is improved. After a period of storage, the space size of the particle cluster is further compressed, and simulation experiments show that the proton beam cluster with the space volume of 0.5mm × 2mm × 2mm is compressed to 0.25mm × 1mm × 1mm after being stored for 100 μ s, the corresponding time dispersion is shown in fig. 11, and the ion flight time dispersion (FWHM) after storage is about 3 ns, which is 1 time resolution higher than that before storage.
Because the voltage on the modulating electrode and the grid electrode is adjusted to focus the ring-surface electron beam at the center of the ionization chamber, the electron beam ionizes neutral gas to obtain ion clusters with smaller space size, and the space size of the ion clusters is further compressed through the storage of the three-dimensional potential well, so that the flight time resolution of the emergent ion clusters in the ion source is improved. Research shows that when the pulse voltage is 100V, the influence of the ion cluster spatial distribution and the velocity dispersion on the flight time resolution can be considered at the same time, and the optimal resolution is obtained, as shown in fig. 11. The pulse width is selected in relation to the mass range of the extracted ions, for example: ions within 50amu mass were all extracted, with a pulse width of about 280 ns.
2. The existing electron impact storage ion source can not carry out three-dimensional constraint on ions, so that the ions are easy to lose, and the long-time ion storage with high efficiency is difficult to realize. The three-dimensional potential well formed based on the electron beam has a constraint effect on ions in the ionization chamber in three directions, so that the ions can be efficiently stored for a long time, and the sensitivity of the ion source is improved by 1-2 orders of magnitude. The invention can be widely applied to mass spectrometry instruments and has wide application prospect for detecting and analyzing the trace substances.
Drawings
Fig. 1 is a perspective view of a structure of an ion source in cross section.
FIG. 2 is a schematic diagram of an ion source electrode structure.
FIG. 3 is an enlarged sectional view of the ion source structure.
Fig. 4 is a schematic view of the structure of the electron repulsion electrode.
Fig. 5 is a radial cross-sectional view of fig. 4.
Fig. 6 is a structural view of the first anode and the second anode.
Fig. 7 is a structural view of an ionization chamber formed by a first anode and a second anode.
Fig. 8 is a radial plane (XY plane) potential distribution diagram of a three-dimensional potential well according to the present invention.
Figure 9 axial plane (XZ plane) potential distribution diagram of a three-dimensional potential well of the present invention.
FIG. 10 shows the storage efficiency in the presence or absence of proton clusters in the three-dimensional potential well for 100 μ s.
Fig. 11 shows the time-of-flight dispersion of the ion packets as they are extracted from the ionization chamber before and after storage.
Numbers in fig. 1-7: the ionization device comprises a first fixed electrode 1, a first anode 2, a first modulation electrode 3, a first grid 4, an electron repulsion electrode 5, a second grid 6, a second modulation electrode 7, a second anode 8, a second fixed electrode 9, a filament electrode 10, a first ceramic gasket 11, a second ceramic gasket 12, a third ceramic gasket 13, an insulating screw 14, a conical section 15, a first grid electrode 16, a second grid electrode 17, a fixing screw 18, a gas entrance ionization chamber and ion exit ionization chamber track 19, a metal screw 20, an insulating notch 21, a small hole 22, an insulating gasket 23, an insulating clamping groove 24, a metal screw 25, a first metal gasket 26, a second metal gasket 27, a first convex ring 28, a second convex ring 29, an ionization chamber 30, an electron spatial distribution 31 and a gas entrance 32.
Detailed Description
The invention will be further described by way of example with reference to the accompanying drawings.
Referring to fig. 1, an electron impact ion source based on electron beam three-dimensional potential well storage comprises an electron gun and an ionization chamber. The electron gun comprises an electron repulsion electrode 5, a filament electrode 10, a first grid 4, a second grid 6, a first modulation electrode 3, a second modulation electrode 7, a first anode 2 and a second anode 8. Referring to fig. 2, annular slits are formed between axially corresponding ends of the first grid 4 and the second grid 6, between axially corresponding ends of the first modulating electrode 3 and the second modulating electrode 7, and between axially corresponding ends of the first anode 2 and the second anode 8.
Referring to fig. 7, the space region enclosed between the corresponding axial end surfaces of the first anode 2 and the second anode 8 is an ionization chamber 30, the ionization chamber 30 includes the first anode 2 and a grid 16 thereon, the second anode 8 and a grid electrode 17 thereon, and the first grid 16 is fixed on the axial end surface of the first anode 2 through a first metal gasket 26 and a metal screw 25; the second grid 17 is fixed at the central hole of the conical section 15 of the second anode 8 by a second metal washer 27 and a metal screw 25. The axial end face center of the first anode 2 is provided with a first gas inlet 32, the axial end face center of the second anode 8 is correspondingly provided with an ion outlet, and the first gas inlet 32 and the ion outlet are coaxial.
Referring to fig. 6, a first protruding ring 28 is provided on the circumference of the axial end face of the first anode 2, and a second protruding ring 29 is provided on the circumference of the axial end face of the second anode 8, so that a narrow annular groove is formed on the circumference of the ionization chamber 30. Referring to fig. 3, the ionization chamber 30 has an axial width L2 of 3mm, and the narrow ring groove on the circumference of the ionization chamber 30 has a groove width of 1mm.
Referring to fig. 3, the distance between the axial inner end face of the first modulation electrode 3 and the axial inner end face of the second modulation electrode 7, the distance between the axial inner end face of the first grid 4 and the axial inner end face of the second grid 6, and the distance L1 between the axial inner end face of the first anode 2 and the axial inner end face of the second anode 8 in the electron gun are 1mm. Distances L3 between the electron repulsion electrodes 5 and the radial directions of the first grid 4 and the second grid 6, between the first grid 4 and the radial directions of the second grid 6 and the radial directions of the first modulation electrode 3 and the second modulation electrode 7, and between the first modulation electrode 3 and the radial directions of the second modulation electrode 7 and the radial directions of the first anode 2 and the second anode 8 are all 1mm.
Referring to fig. 1, the outer circumference of the first anode 2 is embedded in the groove of the first ceramic washer 11, the second insulating ceramic 12 is embedded in the outer circumference of the first anode 2, and the outer circumference of the first modulation electrode 3 is embedded in the groove of the second ceramic washer 12; the first ceramic washer 11, the second ceramic washer 12, and the third ceramic washer 13 are nested with the first fixed electrode 1, the first anode 2, the first modulation electrode 3, the first grid 4, the electron repulsion electrode 5, the second grid 6, the second modulation electrode 7, and the second anode 8 in the above-described manner, and the electrodes nested inside the ion source between the first fixed electrode 1 and the second fixed electrode 9 are pressed and fixed by the fixing screws 18. The groove 21 between the first ceramic gasket 11 and the second ceramic gasket 12, or between the second ceramic gasket 12 and the third ceramic gasket 13, is used to draw a power supply line to the metal electrode.
Referring to fig. 4 and 5, the electron repulsion electrode 5 has a tire shape. Five insulating screws 14 and two metal screws 20 are uniformly arranged on the circumference of the electron repulsion electrode 5. The end of each insulating screw 14 is located in the central hole of the electron repulsion electrode 5, a radial mounting hole is formed in the end of each insulating screw 14, the middle of the filament electrode 10 penetrates through the mounting holes of the five insulating screws 14 respectively, and the filament electrode 10 is supported by the five insulating screws 14. The nut ends of the two metal screws 20 are inner ends and are respectively connected with two ends of the filament electrode 10; the outer ends of the two metal screws 20 are respectively connected with the anode and the cathode of a current source. The small hole 22 of the electron-repelling electrode 5 is used for leading out a power supply line.
Referring to fig. 5, the filament electrode 10 is a circular ring-shaped filament electrode with an opening, coaxially located in the central hole of the electron repulsion electrode 5, and surrounding the annular slit between the first grid 4 and the second grid 6.
The working principle of the invention is explained in detail as follows:
referring to fig. 2, when the invention works, a constant current with a typical value of 1.8A is supplied to the annular filament electrode 10, the filament can emit thermal electrons, the electrons are converged toward the central region of the ionization chamber under the combined action of the electric fields of the electron repulsion electrode 5, the first grid 4, the second grid 6, the first modulation electrode 3, the second modulation electrode 7, the first anode 2 and the second anode 8, the electrons are distributed in the ionization chamber 30 in a disc-shaped space, the axial thickness of the electrons is less than or equal to 0.5mm, and the radial radius of the electrons is 8mm, as shown in an electron space distribution 31 in fig. 3. Through simulation, under the condition that the thermal emission electron current of the filament electrode 10 is 300 muA, in the ionization chamber 30, an electron space charge effect forms a three-dimensional potential well as shown in fig. 8 and 9, wherein fig. 8 is the potential distribution of the three-dimensional potential well in an XY plane, fig. 9 is the potential distribution of the three-dimensional potential well in a YZ plane, the maximum depth of the potential well is 2.87V, the axial half-depth width is 0.8 to 1mm, and the radial half-depth width is about 1.8 to 2mm.
In the ionization chamber 30, electrons emitted from the circular filament electrode 10 are impact-ionized with neutral gas entering from the gas inlet 32, and electrons having an energy of 70eV are used to ionize the neutral gas since the electrons having an energy of 70eV have the largest electron impact ionization cross section. Ions generated by the electrons impacting the neutral gas are then stored in a three-dimensional potential well located in the central region of the ionization chamber 30. Because the penetration of an external electric field can reduce the storage efficiency of the electron beam three-dimensional potential well, the first grid electrode 16 and the second grid electrode 17 with the transmittance of 90 percent are arranged on the axial end surfaces of the first anode 2 and the second anode 8 to shield the external electric field, and simultaneously, the gas introduction and the efficient ion extraction can be ensured. When the ions need to be analyzed, a positive pulse voltage is applied to the first anode 2 to extract the ions in the potential well, and mass spectrometry is performed.

Claims (5)

1. An electron impact ion source based on electron beam three-dimensional potential well storage comprises an electron gun and an ionization chamber; the electron gun comprises an electron repulsion electrode (5), a filament electrode (10), a first grid (4), a second grid (6), a first modulation electrode (3), a second modulation electrode (7), a first anode (2) and a second anode (8); annular slits are formed between the axial corresponding ends of the first grid 4 and the second grid 6, between the axial corresponding ends of the first modulation electrode (3) and the second modulation electrode (7), and between the axial corresponding ends of the first anode (2) and the second anode (8); the ionization chamber (30) is a space region enclosed between the corresponding axial end parts of the first anode (2) and the second anode (8), and the ionization chamber (30) comprises the first anode (2) and a grid mesh (16) on the first anode, the second anode (8) and a grid mesh electrode (17) on the second anode; the electron repulsion electrode (5) is in a tire shape and is characterized in that:
more than three insulating screws (14) and two metal screws (20) are uniformly distributed in the circumferential radial direction of the electronic repulsion electrode (5); the inner ends of more than three insulating screws (14) are fixed with the filament electrode (10); the nut ends of the two metal screws (20) are inner ends and are respectively connected with the two ends of the filament electrode (10); the outer ends of the two metal screws (20) are respectively connected with the anode and the cathode of a current source;
the filament electrode (10) is an annular filament electrode with an opening, is coaxially positioned in a central hole of the electron repulsion electrode (5), and surrounds an annular slit between the first grid (4) and the second grid (6);
a gas inlet (32) is formed in the center of the axial end face of the first anode (2), an ion outlet is formed in the center of the axial end face of the second anode (8), and the gas inlet (32) and the ion outlet are coaxial;
a first grid mesh (16) is arranged on a gas inlet (32) of the first anode (2), and a second grid mesh (17) is arranged on an ion outlet of the second anode (8);
a first convex ring (28) is arranged on the circumference of the axial end face of the first anode (2), and a second convex ring (29) is arranged on the circumference of the axial end face of the second anode (8), so that a narrow ring groove is formed on the circumference of the ionization chamber (30);
when the annular filament electrode (10) works, the generated electron beams form a three-dimensional potential well in the ionization chamber (30).
2. The electron impact ion source based on electron beam three-dimensional potential well storage as claimed in claim 1, wherein: the distance between the axial inner end face of the first modulation electrode (3) and the axial inner end face of the second modulation electrode (7), the distance between the axial inner end face of the first grid (4) and the axial inner end face of the second grid (6), and the distance L1 between the axial inner end face of the first anode (2) and the axial inner end face of the second anode (8) in the electron gun are 1mm; the distance L3 between the electron repulsion electrode (5) and the radial direction of the first grid (4) and the second grid (6), between the first grid (4) and the radial direction of the second grid (6) and the radial direction of the first modulation electrode (3) and the radial direction of the second modulation electrode (7), and between the first modulation electrode (3) and the radial direction of the second modulation electrode (7) and the radial direction of the first anode (2) and the radial direction of the second anode (8) are all 1mm.
3. The electron impact ion source based on electron beam three-dimensional potential well storage as claimed in claim 1, characterized in that: the end part of each insulating screw (14) is positioned in the central hole of the electron repulsion electrode (5), the end part of each insulating screw (14) is provided with a radial mounting hole, the middle part of the filament electrode (10) penetrates through the mounting holes at the end parts of more than three insulating screws (14), and the annular filament electrode (10) is supported by more than three insulating screws (14).
4. The electron impact ion source based on electron beam three-dimensional potential well storage as claimed in claim 1, wherein: the two metal screws (20) are fixed on the electronic repulsion electrode (5) through insulating washers (23) and insulating clamping grooves (24), and the end parts of the two metal screws (20) are positioned in the central hole of the electronic repulsion electrode (5) and are respectively and fixedly connected with the two ends of the opening of the annular filament electrode (10).
5. The electron impact ion source based on electron beam three-dimensional potential well storage as claimed in claim 1, characterized in that: the axial width L2 of the ionization chamber (30) is 3mm, and the groove width of a narrow ring groove on the circumference of the ionization chamber (30) is 1mm; the first grid mesh (16) is fixed on the groove surface of the first anode (2) through a first metal gasket (26); the second grid mesh (17) is fixed on the groove surface of the second anode (8) through a second metal gasket (27).
CN202211034442.9A 2022-08-26 2022-08-26 Electron collision ion source based on electron beam three-dimensional potential well storage Active CN115360079B (en)

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US20120012746A1 (en) * 2010-07-19 2012-01-19 Herrero Federico A Ion source with corner cathode
CN102290315A (en) * 2011-07-21 2011-12-21 厦门大学 Ion source suitable for flight time mass spectrometer
CN109690724A (en) * 2016-11-11 2019-04-26 日新离子机器株式会社 Ion source
CN109336047A (en) * 2018-10-08 2019-02-15 东北大学 A kind of multilayered structure ion source chip and mass spectral analysis sampling system based on MEMS technology

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