EP3465732A1 - Génération non magnétique d'impulsions d'ions - Google Patents
Génération non magnétique d'impulsions d'ionsInfo
- Publication number
- EP3465732A1 EP3465732A1 EP17726938.8A EP17726938A EP3465732A1 EP 3465732 A1 EP3465732 A1 EP 3465732A1 EP 17726938 A EP17726938 A EP 17726938A EP 3465732 A1 EP3465732 A1 EP 3465732A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- ions
- anode
- electrons
- ion
- potential
- 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.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
- H01J49/147—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J27/00—Ion beam tubes
- H01J27/02—Ion sources; Ion guns
- H01J27/08—Ion sources; Ion guns using arc discharge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/40—Time-of-flight spectrometers
Definitions
- the invention relates to an apparatus for generating, storing and releasing ions from a residual gas atmosphere having the features of claim 1 and a method therefor having the features of claim 11.
- the prior art already provides apparatus and methods for
- EBIT electron beam ion trap
- a first disadvantage is the considerable expenditure on apparatus for generating and bundling the electron beam, which in particular in the magnetic field device for
- a method and an apparatus for generating, storing and releasing ions from a residual gas atmosphere are to be specified, in which the number of ions generated by the pressure of the residual gas atmosphere in
- the process should still be executable even at a low pressure in the residual gas and thereby deliver the largest possible ion quantities for a secured ion detection.
- the arrangement for carrying out the method should have a simple structure and can be carried out without the additional influence of magnetic fields.
- the method should ensure the best possible thermal energy distribution within the generated quantity of ions.
- the energy distribution of the ions should thus by the process of ion generation itself no
- the desired process for ion generation and the device used in the process should leave the molecules within the residual gas atmosphere as intact as possible during the ionization, it should as possible only be easily charged ions are generated.
- the apparatus for generating, storing and releasing ions from a residual gas atmosphere comprises an electron source for releasing electrons and an anode permeable to the electrons released by the electron source having a negative space charge formed by the electrons within an ion storage space at least partially surrounded by the anode ,
- Residual gas atmosphere generated an attractive spatial potential distribution due to the negative space charge. Furthermore, an in
- the device according to the invention is based on the idea of ionizing and storing the particles of the residual gas in the attractive potential of a negative space charge cloud.
- the negative space charge cloud or electron density is without further
- the anode is permeable to the emitted electrons.
- the emitted electrons collect in the region of the permeable anode and form the space charge cloud, in particular in its inner region.
- the negative space charge cloud fulfills a dual function: first, it ionizes the particles of the residual gas and second, it forms an attractive potential for the positive ions formed therein.
- the positive ions accumulate in this attractive potential, so that the negative space charge cloud a
- the anode and the pulse electrode are at the same potential during the storage process.
- the electron source is in the form of a hot cathode surrounding the electron-permeable anode Ring filament formed.
- the electron-permeable anode is exposed from all sides with the electrons emitted from the ring filament.
- other embodiments of the electron source in which the electrons are emitted from one or more sources and act on the anode at appropriate locations.
- the decisive factor is the generated negative space charge distribution within the anode at the end.
- the acceleration voltage for the electrons can be significantly reduced.
- the acceleration voltage applied to the hot cathode for the emitted electrons is at most 200 volts.
- the electron current can be significantly reduced.
- the electron current exiting the hot cathode is not more than 10mA, in particular, 2mA is sufficient for typical applications. This significantly reduces the power consumption and the heat input in the sensor.
- a surrounding the electron source In one embodiment, a surrounding the electron source
- the focusing electrodes and / or the repeller are used, in particular, to direct the electrons not emitted in the direction of the electron-permeable anode in the direction of the electron-permeable anode, thus assisting the formation of the negative space charge.
- the negative space charge distribution forms a potential well with respect to the anode and pulse electrode potentials, which, when the negative space charge distribution is not ion-compensated, is attractive to ions in the ionization volume and forms an omnidirectional electrostatic exit barrier for ions, thus enabling one
- the pulse electrode is switchable to a negative potential compared to the anode, whereby the collected ions are extractable in the direction of the pulse electrode.
- the frequency for switching the pulse electrode is expediently at least 0.1 Hz and at most 1 M Hz, in particular at least 1 Hz, and at most 100 kHz.
- the electron current generated by the electron source is a minimum of ⁇ and a maximum of 15 mA, in particular a minimum of 5 ⁇ and a maximum of 2mA.
- Acceleration voltage is a minimum of 30V and a maximum of 400V, in particular a minimum of 70V and a maximum of 150V.
- the anode which is permeable to the emitted electrons has a cylindrically symmetrical structure.
- the cylindrically symmetric structure promotes the multiple passing of the electrons through the
- Emission current is increased due to the increased space charge in the storage space.
- a detector arranged in the direction of flight of the ions may be used for
- Measurement of the ion current can be provided.
- the method for generating, storing and pulsed release of ions from a residual gas atmosphere is carried out with the following method steps: There is an emitting of electrons from an electron source and a
- Space charge cloud out.
- Within the negative space charge cloud occurs simultaneously an impact ionization of gas molecules and / or gas atoms.
- the generated positively charged ions are collected in the attractive potential of the negatively charged space charge cloud and form a positively charged ion reservoir stored there.
- the basic idea of the method is to use a negative space charge cloud formed from released electrons firstly for the impact ionization of neutral gas particles and secondly as the negative potential of the
- This negative potential is thus gradually filled with the generated positive ions until this potential is substantially balanced. Because the depth of the negative potential is not substantially dependent on the pressure of the surrounding gas atmosphere and this potential is always filled in the course of ionization of the gas particles, the number of ionized gas particles in the negative potential is largely independent of the pressure of the gas atmosphere, so that one of the pressure independent ion packet can be released.
- Storage potential is essentially thermal, the ions themselves are usually only positively charged due to the weak low kinetic electron energy, with larger molecules are essentially not split into smaller fragments.
- the method does not require complicated magnetic focusing of an electron beam and can be operated at comparatively low electron energies compared to the prior art. Likewise, expensive storage electrodes for collecting the generated ions are eliminated.
- the emitting of the electrons from the electron source takes place in an advantageous embodiment of the method from an annular transmissive Anode arrangement surrounding hot cathode, wherein the electrons are accelerated in the field of the transmissive anode assembly and the negative
- the transmissive anode arrangement thus pursues only the purpose of concentrating the emitted electrons in a certain area of space and thereby the ionizing and simultaneously storing
- the strength of the released ion pulse over a time interval between successive
- Ion pulse is proportional to the length of the time interval.
- Ion packets also a determination of a total pressure to be performed.
- a strength of the liberated ion current is measured at a fixed predetermined time interval between successive switching operations of the pulse electrode, wherein the strength of the ionic current is used as a measure of the total pressure to be measured.
- Ion packets also a determination of a total pressure to be performed.
- the time interval between successive switching operations of the pulse electrode is controlled to a fixed predetermined strength of the measured released ion packet, wherein the time interval between successive switching operations of the pulse electrode is a measure of the total pressure to be measured. Due to the independent of the pressure strength of the ion packet, the
- Ion source can be operated in a very wide pressure range of le-12 mbar to 2e-2 mbar. The device and the method will be described below with reference to
- FIG. 1 is an overall view of the device for ion generation, storage and release in section,
- FIG. 2 shows a representation of the device from FIG. 1 in a perspective view
- FIG. 3 shows a representation of the process of ion generation, storage and release in the device according to the invention
- FIGS. 4a and 4b show different representations of an exemplary pulse electrode with a pulse grid
- Fig. 5 shows an exemplary illustration of the device for generating ions in connection with a sensor for a time-of-flight spectroscopy
- Fig. 6 is an exemplary representation of various potential distributions in
- FIG. 7 is an illustration of the dependence of the number of storable ions on the emission current at the electron source for two different acceleration voltages acting on the electrons,
- Fig. 8 is an illustration of the dependency of the storable charge on
- Fig. 9 is an illustration of the time filling process for the attractive potential as a function of two different pressures
- Fig. 10 a representation of the simulated filling time as a function of the pressure
- Fig. 11 is a representation of a simulated collecting effect and a consequent filling time for a pressure of 10 "5 mbar
- 12 shows a representation of the experimentally determined filling time as a function of the pressure
- FIG. 14 is a representation of the flight times of ions of different masses.
- Fig. 1 shows an overall view of the apparatus for ion generation, storage and release in section.
- the device contains a
- Electron source 1 which is formed in the present example as a hot cathode in the form of a ring filament.
- the ring filament surrounds an anode 2 which is permeable to electrons.
- anode 2 which is permeable to electrons.
- a negative ionizing space charge 3 is generated by the emitted electrons, which is indicated in the present figure by a dashed line.
- the negative space charge extends in particular into an ion storage space 4, which is located in the interior of the anode 2.
- the anode 2 is electrically isolated from the pulse electrode 5.
- the arrangement is additionally of
- Focusing electrodes 6 surrounded and shielded to the outside.
- Electron source emitted electrons in the direction of the electron-permeable anode. 2
- Fig. 2 shows the arrangement shown in Fig. 1 in a perspective
- the electron-permeable anode 2 is constructed here cylindrically symmetrical. It contains a lateral surface 7, which is designed as a sufficiently fine-meshed grid, sieve or conductive fabric.
- the front of the electron-permeable anode 2 is constructed here cylindrically symmetrical. It contains a lateral surface 7, which is designed as a sufficiently fine-meshed grid, sieve or conductive fabric.
- the entire anode arrangement, including the lateral surface 7 and the pulse electrode 8, is gas-permeable and at the same time partially transparent to electrons.
- the electron source used in the present example is a ring filament 9 in the form of a ring-shaped hot cathode which extends at a certain distance parallel to the lateral surface 7 and emits electrons at high temperature by means of thermal emission.
- the electrons emitted from the hot cathode are mutually u .a. emitted in the direction of the lateral surface 7 of the anode and accelerated and penetrate the lateral surface 7, wherein these penetrate into the interior of the anode and ionize the gas particles present there via the process of impact ionization.
- the electrons form a negative space charge cloud, which represents an attractive potential for the positively charged ions.
- the ions are thus collected in this attractive potential within the ion storage space 4 of the anode.
- the extraction direction of the ion packet is illustrated by an arrow.
- the pulse electrode may be switchable to a positive potential compared to the anode in order to accelerate the collected ions against the direction of the pulse electrode.
- the collected ions can be extracted from the ion storage space counter to the direction of the pulse electrode by a repulsive electrostatic interaction.
- the pulse electrode may in such a case be impermeable to the ions and drive the positive ions out through the body of the anode.
- Fig. 3 shows the process of ion generation and storage in a series of process steps A to D.
- the electron source 1 is inactive.
- the anode 2 is at a positive potential V AN , which is above the
- Cross-section of the anode in the ion storage space 4 located therein is substantially location-independent and constant.
- the anode and the pulse electrode are at the same potential V AN , so that a constant potential V AN is established in the ionization volume.
- the electron source 1 is activated.
- the emitted electrons penetrate the anode and form, in particular in the ion storage space 4, a negative space charge cloud 3.
- the potential within the anode assumes a location-dependent value.
- State C takes into account the impact ionization of the gas particles present in the ion storage space 4 by the influence of the emitted electrons.
- the positively charged ions are moved to the local minimum of the potential in the ion storage space and accumulate within the negative
- Ionization space surrounding electrodes collide and neutralized.
- the potential is compensated with continuous time, the depth of the local potential minimum within the ion storage space decreases and the potential minimum becomes increasingly flatter.
- state D the potential minimum is filled up by the positive ions.
- the negative space charge of the electrons is completely through the positive
- the state B is again assumed, in which there is an empty unfilled potential minima within the ion storage space and which can be refilled when the states C and D are re-run and emptied by the ions stored there.
- This cyclic operation thus allows ion packets or ion pulses, ie spatially limited Ion accumulations, generate.
- the time from state B to complete space charge compensation in state D will be referred to hereafter as the fill duration. From the positive ion charge, which is stored in the state D, results in the storage capacity of the ion source.
- FIGS. 4a and 4b show a representation of the pulse electrode 8 with a pulse grid 5 incorporated therein.
- the basis for the pulse electrode 8 is a sheet-metal disk.
- a hexagonal honeycomb structure 10 is incorporated, in particular cut by means of laser radiation, which has a diameter D PG . This increases the permeability of the pulse grid and ensures adequate shielding against external fields.
- the pulse electrode Via metallic feeds, the pulse electrode can be electrically contacted.
- S of a pulse generator not shown here, which are required for the extraction of the accumulated ions, transmitted to the pulse electrode.
- the lattice structure 10 consists of honeycomb-like hexagonal openings 11, which are separated from one another by webs 12.
- the geometric dimensions of the grid structure of the pulse grid are chosen so that a loss-free as possible extraction of the ions from the anode chamber, with optimal shielding against external fields is guaranteed.
- Corresponding transmission losses, which are due to the fact that ions neutralize at the lattice webs, can be minimized by an appropriate dimensioning of the web width S and the mesh size G of the hexagonal openings 11.
- Arrangement of the ion source and the time of flight spectroscopic device consists essentially of three modules. These assemblies are the ion source, consisting of the electron source 1, the anode 2 and the pulse electrode 8. Also provided is a repeller 13 as well as a second assembly of a time-of-flight (TOF) mass separator adjoining the ion source 14 with a detector unit as the third module, which is designed here as a Farady cup 15. The entire arrangement has the compact design of conventional ionization vacuum gauge.
- TOF time-of-flight
- Ring-shaped filament of the electron source electrons are released by thermal emission, due to the attractive
- Potentials of the anode are directed into the anode compartment inside. Thereupon, by collisions of the electrons with the neutral residual gas particles, positive ions are formed which, as mentioned, can be accumulated to a certain extent in the anode.
- time-separated signals can be detected at the detector, which is designed here in the form of a Faraday cup 15.
- the advantage of the time-of-flight mass separation lies in the fact that it is thus possible to record an entire mass spectrum with one single ion pulse with one and the same detector. In this case, the time t T0F required for the ions is measured by a given distance S T OF between the
- Metal platelets are neutralized by flowing electrons.
- the current I FC flowing during discharge of the metal plate is thus directly proportional to the number of impinging ions.
- the time-of-flight mass separator separates light ions from the heavier ones. As light ions accelerate faster, they reach the Faraday Cup at an earlier point in time. In this case, according to the temporal detection at the Faraday Cup individual peaks visible. If individual masses differ sufficiently, the
- the negative space charge is subsequently assumed to be simplified as an electron density with a given radius r 0 .
- the field distribution in the presence of the electron density decays here into two areas.
- the first region is formed by the space within the electron density with the radius r ⁇ r 0
- the potential distribution V (r) for these two ranges can be calculated as a function of r. For a given distance r AN , the potential in FIG. 6 graphically.
- the potential can be set as follows:
- the depth of the potential minimum is strongly dependent on the radius of the electron density.
- the focusing electrodes 6 are indicated schematically. If the focusing electrode 6 is set to a potential smaller and equal to the potential of the electron source 1, the electrons emerging from the electron source 1 are focused in the direction of the anode.
- Anode space, and AL corresponding to the length traveled by the electrons within the anode.
- V e V AN - V FN which acts on the electrons
- the upper graph shows the progression for one
- the number of storable ions thus becomes N + 1.3 1 10 7 .
- the electron current generated by the electron source 1 is minimal ⁇ and a maximum of 15 mA, in particular minimal 5 ⁇ and a maximum of 2 mA. the heating power needed to generate this emission currents is sufficiently small to cause only a small power and heat input into the entire assembly and the adjacent vacuum chamber.
- the amounts of charge generated by Q + "2.0 1 10" 12 C are sufficiently high to be detected by simple detectors (for example, in the manner of a Faraday Cup) with sufficient signal-to-noise ratio.
- Fig. 8 shows that as the accelerating voltage is increased from 70V to 130V, the storage capacity is decreased because the faster electrons generate a smaller negative space charge.
- a charge of approx. 10 "14 C to 10 " 11 C can be stored at the selected acceleration voltages with an emission current in the range 10 ⁇ to 5mA. These amounts of charge can without additional expensive equipment, such.
- a photomultiplier can be detected with a simple Faraday Cup with a good signal-to-noise ratio.
- the filling time i. the time in which the negative electron space charge is completely compensated by stored ions depends on this
- the filling time t FÜM is also dependent on the prevailing pressure p, since at higher pressures correspondingly more neutral gas particles are present, which can fill up the potential minimum faster after ionization.
- p the prevailing pressure
- a decreasing filling time t FÜM /! ⁇ t FÜM / 2 and the qualitative course of these curves will be similar.
- the storage capacity of the ion source is determined solely by the depth of the potential formed by the negative space charge. As in the
- the maximum storable charge changes by about half, while the pressure is varied by about 3 decades from about 5E-6 mbar to about 5E-9 mbar. Furthermore, the change in the storable charge decreases with decreasing pressure. This allows the use of the ion source over a very wide pressure range without significant loss of measurement sensitivity.
- the electrical current density j which describes the ratio of the current intensity I to a cross-sectional area A available to it.
- Negative extraction potential manipulates the electric field inside the anode so that the collected ions are accelerated out of the ionization volume and detected on the Faraday cup.
- the pulse electrode is switched back to the anode potential, the original state sets in: electrons generate a potential minimum in which ions are generated and collected. The period of time ions are collected until they are extracted by the switching of the pulse electrode is the collection time.
- the storage was realized by having a
- the required collection time is, for example,.
- Total pressure sensor suitable for detecting fast pressure changes with reaction times ⁇ 1 ms. As shown in FIG. 14, it is possible to temporally separate the helium signal from the other residual gas components. Therefore it is possible the
- Total pressure sensor at the same time to use as a helium detector, whereby a helium leak test is possible.
- the flight path underlying the measured values in FIG. 14 is only 2 cm, so that the sensor has a high altitude
- the device treated here has a high compactness, a reliable total pressure determination and a helium mass separation.
- the dimension of the sensor corresponds to that of a conventional ionization vacuum gauge.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102016110495.7A DE102016110495B4 (de) | 2016-06-07 | 2016-06-07 | Vorrichtung und Verfahren zum Erzeugen, Speichern und Freisetzen von Ionen aus einer umgebenden Restgasatmosphäre |
| PCT/EP2017/063084 WO2017211627A1 (fr) | 2016-06-07 | 2017-05-31 | Génération non magnétique d'impulsions d'ions |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP3465732A1 true EP3465732A1 (fr) | 2019-04-10 |
| EP3465732B1 EP3465732B1 (fr) | 2024-06-05 |
| EP3465732C0 EP3465732C0 (fr) | 2024-06-05 |
Family
ID=58873824
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP17726938.8A Active EP3465732B1 (fr) | 2016-06-07 | 2017-05-31 | Génération non magnétique d'impulsions d'ions |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP3465732B1 (fr) |
| DE (1) | DE102016110495B4 (fr) |
| PL (1) | PL3465732T3 (fr) |
| WO (1) | WO2017211627A1 (fr) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10928265B2 (en) | 2018-05-29 | 2021-02-23 | Mks Instruments, Inc. | Gas analysis with an inverted magnetron source |
| RU2717352C1 (ru) * | 2019-07-30 | 2020-03-23 | федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский ядерный университет "МИФИ" (НИЯУ МИФИ) | Способ охлаждения ионов |
| US10948456B1 (en) | 2019-11-27 | 2021-03-16 | Mks Instruments, Inc. | Gas analyzer system with ion source |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839655A (en) * | 1973-08-24 | 1974-10-01 | Varian Associates | Bayard-alpert vacuum ionization tube |
| JPS6084758A (ja) * | 1983-10-14 | 1985-05-14 | Seiko Instr & Electronics Ltd | 熱陰極電子衝撃型イオン源 |
| JPS6093750A (ja) * | 1983-10-26 | 1985-05-25 | Seiko Instr & Electronics Ltd | 熱陰極電子衝撃型イオン源 |
| DE3718244A1 (de) | 1987-05-30 | 1988-12-08 | Grix Raimund | Speicherionenquelle fuer flugzeit-massenspektrometer |
| GB9304462D0 (en) * | 1993-03-04 | 1993-04-21 | Kore Tech Ltd | Mass spectrometer |
| EP0676792A3 (fr) * | 1994-04-05 | 1996-01-10 | Atomika Instr Gmbh | Dispositif relatif à la technique ionique. |
| DE19949978A1 (de) | 1999-10-08 | 2001-05-10 | Univ Dresden Tech | Elektronenstoßionenquelle |
| CN101303955B (zh) * | 2007-05-09 | 2010-05-26 | 清华大学 | 离子源组件 |
| JP2015515733A (ja) * | 2012-04-26 | 2015-05-28 | レコ コーポレイションLeco Corporation | 高速応答を有する電子衝撃イオン源 |
-
2016
- 2016-06-07 DE DE102016110495.7A patent/DE102016110495B4/de active Active
-
2017
- 2017-05-31 EP EP17726938.8A patent/EP3465732B1/fr active Active
- 2017-05-31 WO PCT/EP2017/063084 patent/WO2017211627A1/fr not_active Ceased
- 2017-05-31 PL PL17726938.8T patent/PL3465732T3/pl unknown
Also Published As
| Publication number | Publication date |
|---|---|
| DE102016110495B4 (de) | 2018-03-29 |
| WO2017211627A1 (fr) | 2017-12-14 |
| DE102016110495A1 (de) | 2017-12-07 |
| EP3465732B1 (fr) | 2024-06-05 |
| EP3465732C0 (fr) | 2024-06-05 |
| PL3465732T3 (pl) | 2024-10-07 |
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