EP1052672A1 - Source ionique pour spectromètre de masse à temps de vol analysant des echantillons gazeux - Google Patents
Source ionique pour spectromètre de masse à temps de vol analysant des echantillons gazeux Download PDFInfo
- Publication number
- EP1052672A1 EP1052672A1 EP00401028A EP00401028A EP1052672A1 EP 1052672 A1 EP1052672 A1 EP 1052672A1 EP 00401028 A EP00401028 A EP 00401028A EP 00401028 A EP00401028 A EP 00401028A EP 1052672 A1 EP1052672 A1 EP 1052672A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- electron
- ion source
- electrons
- flow
- mass spectrometer
- 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
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J27/00—Ion beam tubes
- H01J27/02—Ion sources; Ion guns
- H01J27/04—Ion sources; Ion guns using reflex discharge, e.g. Penning ion sources
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/08—Electron sources, e.g. for generating photo-electrons, secondary electrons or Auger electrons
-
- 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
- H01J43/00—Secondary-emission tubes; Electron-multiplier tubes
- H01J43/04—Electron multipliers
- H01J43/06—Electrode arrangements
- H01J43/18—Electrode arrangements using essentially more than one dynode
- H01J43/24—Dynodes having potential gradient along their surfaces
- H01J43/246—Microchannel plates [MCP]
Definitions
- the present invention relates to ionization means gas samples for analysis in a mass spectrometer.
- ions produced by the ion source are launched at the entrance of a tube of flight in which they maintain a constant speed, and we detect at the outlet of the flight tube, the flight time corresponding to each type of gas sample ions to be analyzed, to deduce their nature. This requires launching at the entrance of the flight tube a ion accelerated packet, locate the start time of the packet of ions, and identify the times of arrival of the different ions at the other end of the flight tube.
- the ion sources usually used in mass spectrometers include an electron gun having a electron source and one or more electrodes of conditioning the flow of electrons to generate a flow of suitable electrons directed to a gas ionization zone in which form ions subjected to one or more electrodes ion flow conditioning.
- the electron flow is generally directed towards the gas ionization zone in a direction perpendicular to the direction of the flight tube of the mass spectrometer. This results in significant bulk, and integration difficulty.
- the quantity of ions produced is relatively low, which limits the sensitivity of the device.
- the problem proposed by the present invention is to design a new ion source structure for mass spectrometer, with greater compactness and greater sensitivity, being easily integrated with other components of a mass spectrometer.
- a source ion for mass spectrometer comprises a electron gun having an electron source and one or more electron flow conditioning electrodes to generate a appropriate electron flow directed to a gas ionization zone in which are formed ions subjected to one or more ion flow conditioning electrodes; downstream of electron flow conditioning electrodes, we interpose in the electron flow one or more microchannel pancakes, so that from a pulsed primary electron beam containing relatively few electrons, we generate a beam secondary pulsed electronics containing a lot of electrons.
- microchannel pancakes ensure a multiplication of the flow of electrons, so the subsequent ionization of the gas sample is also multiplied.
- the sensitivity and resolving power of the device are found as well considerably increased.
- At least one additional electrode adapted to scatter the beam secondary electronics in order to maintain its qualities while improving its spatial qualities.
- the gas ionization zone is located between an upstream repulsion electrode, crossed by the beam secondary electronics and retaining the electrons by repelling them ions, and a downstream acceleration electrode that attracts ions.
- the source can be placed ionic in alignment with the axis of the flight tube at the entrance of the tube time of flight mass spectrometer. We thus obtain better integration of the ion source, and greater compactness of the device.
- the ionization zone should preferably be near immediate of the microchannel pancake (s), so that the beam secondary electronics keeps its temporal qualities and stays dense, so that all the ions in a packet of ions penetrate substantially at the same time in the flight tube.
- a filament can be used as an electron source heated to a suitable temperature to generate a flow of electrons by thermoemission, in the traditional way.
- the primary electron beam is then pulse modulated by a deflection electrode.
- the electron source can advantageously be a microtip field emission cathode, producing a pulse modulated primary electron beam.
- the invention may find particular application in the production of time-of-flight spectrometers incorporating such a ion source.
- a mass spectrometer at flight time comprises of generally an electron gun 1, followed by an ion gun 2, itself followed by a flight tube 3 whose output communicates with a ion detector 4.
- the electron gun 1 includes an electron source 5.
- the electron source 5 is a filament such as a tungsten filament fed by a heating generator 6 to be brought to a temperature sufficient ensuring thermal emission of ions.
- the emitted electrons by the electron source 5 are requested by one or more electron flow conditioning electrodes 7, for example an acceleration electrode 71 and one or more electrodes of focus 72.
- a deflection electrode 73 allows impulse modulating the outgoing electron flow 8.
- a microtip field emission cathode comprising a conductive substrate on which microtips are produced conductors engaged in cavities of an insulating layer interposed between the substrate and a positively polarized grid.
- a microtip field emission cathode makes it possible to modulate by itself the outgoing flow of electrons, without requiring deflection electrode 73.
- microchannel wafers 9 and 10 Downstream of the flow conditioning electrodes of electrons 7, according to the invention interposed in the flow of electrons 8 one or more microchannel wafers.
- the primary electron beam can be equivalent to an electric current of the order of 1 to 10 ⁇ A, and the secondary electron beam can correspond to several milliamps, depending on the gain of the microchannel pancakes 9 and 10.
- Primary 8 and secondary 12 electronic harnesses can for example be formed by pulses whose duration is the nanosecond order.
- a microchannel pancake 9 is a generally flat element, having a thickness E of of the order of 0.5 mm, and consisting of the juxtaposition side by side of a very large number of very small glass capillary tubes diameter, including for example the tube 13, oriented according to axes perpendicular to the general plane of the wafer 9.
- the tubes capillaries can have a diameter e of about 12 microns, and they are open at their two ends on the faces principal of the pancake 9.
- the principal faces of the pancake 9 are metallized, to constitute, as illustrated in FIG. 3, an input electrode 14 and an output electrode 15, subjected to a potential difference VD.
- the potential of the electrode output 15 is greater than the potential of the input electrode 14.
- the inner wall of capillary tube 13 is treated to present an appropriate resistance, and forms an electron multiplier independent secondary.
- an electron in the beam primary electronics 8 enters tube 13 it can come strike the wall of tube 13 and unhook one or more others electrons which are accelerated by the electric field present between the input 14 and output 15 electrodes.
- the electrons thus detached will strike themselves on the opposite wall of the tube 13, picking up other electrons which are accelerated themselves, and it gradually the multiplication of the electrons in movement, producing a secondary electron beam 12 containing a lot of electrons.
- the beam secondary electronics 12 spreads to an ionization zone 16 inside the ion gun 2.
- the electrons strike the atoms of the gas sample at analyze, and turn them into ions.
- the gas ionization zone 16 is located between an upstream repulsion electrode 17 crossed by the secondary electron beam 12 and which retains the electrons by repelling ions, and an accelerating electrode downstream 18 which attracts the ions.
- the ion flow 19 thus produced is sent to input 20 of flight tube 3, then travels the length of flight tube 3 to exit through its outlet 21 and enter the ion detector 4.
- the ion source is arranged in line at the entrance of flight tube 3 of the spectrometer time-of-flight mass.
- the ion detector 4 may include pancakes with microchannels 22 and 23, generating a multiplied electron flow coming strike a target electrode 24. The measurement is carried out by detecting the electrical pulses collected by the target electrode 24.
- At least one electrode additional 25 adapted to disperse the electron beam secondary 12 in order to preserve its temporal qualities while by improving its spatial qualities. So we increase ionization in the ionization zone 16.
- the ionization zone 16 is close immediately of the microchannel pancake 10, from which it is separated by a reduced distance, for example from 1 to 2 mm approximately.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Combustion & Propulsion (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
- Electron Sources, Ion Sources (AREA)
Abstract
Description
- la figure 1 illustre le schéma de principe d'un spectromètre de masse à temps de vol selon un mode de réalisation de la présente invention ;
- la figure 2 est une vue schématique en perspective en partie découpée d'une galette à microcanaux pour amplification du flux d'électrons ; et
- la figure 3 est une coupe longitudinale d'un canal de la galette à microcanaux de la figure 2, illustrant le principe de l'amplification du flux d'électrons.
Claims (8)
- Source ionique pour spectromètre de masse, comprenant un canon à électrons (1) ayant une source d'électrons (5) et une ou plusieurs électrodes de conditionnement de flux d'électrons (7) pour générer un flux d'électrons approprié dirigé vers une zone d'ionisation de gaz (16) dans laquelle se forment des ions soumis à une ou plusieurs électrodes de conditionnement de flux d'ions (17, 18), caractérisée en ce que, en aval des électrodes de conditionnement de flux d'électrons (7), on interpose dans le flux d'électrons (8) une ou plusieurs galettes à microcanaux (9, 10), de sorte que, à partir d'un faisceau électronique primaire (8) pulsé contenant relativement peu d'électrons, on génère un faisceau électronique secondaire (12) pulsé contenant beaucoup d'électrons.
- Source ionique selon la revendication 1, caractérisée en ce qu'on dispose, en aval de la zone occupée par la ou les galettes à microcanaux (9, 10), au moins une électrode supplémentaire (25) adaptée pour disperser le faisceau électronique secondaire (12) afin de lui conserver ses qualités temporelles tout en améliorant ses qualités spatiales.
- Source ionique selon l'une des revendications 1 ou 2, caractérisée en ce que la zone d'ionisation de gaz (16) est située entre une électrode de répulsion (17) amont traversée par le faisceau électronique secondaire (12) et qui retient les électrons en repoussant les ions, et une électrode d'accélération (18) aval qui attire les ions.
- Source ionique selon l'une quelconque des revendications 1 à 3, caractérisée en ce qu'elle est disposée en alignement à l'entrée du tube de vol (3) d'un spectromètre de masse à temps de vol.
- Source ionique selon l'une quelconque des revendications 1 à 4, caractérisée en ce que la zone d'ionisation de gaz (16) est à proximité immédiate de la ou des galettes à microcanaux (9, 10).
- Source ionique selon l'une quelconque des revendications 1 à 5, caractérisée en ce que la source d'électrons (5) est un filament chauffé à une température appropriée pour générer un flux d'électrons par thermoémission, et le faisceau électronique primaire (8) est modulé en impulsion par une électrode de déviation (73).
- Source ionique selon l'une quelconque des revendications 1 à 5, caractérisée en ce que la source d'électrons (5) est une cathode à émission de champ à micropointes, produisant un faisceau électronique primaire modulé en impulsion.
- Spectromètre de masse à temps de vol, caractérisé en ce qu'il comprend une source ionique selon l'une quelconque des revendications 1 à 7.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9905088 | 1999-04-22 | ||
FR9905088A FR2792773B1 (fr) | 1999-04-22 | 1999-04-22 | Source ionique pour spectrometre de masse a temps de vol analysant des echantillons gazeux |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1052672A1 true EP1052672A1 (fr) | 2000-11-15 |
EP1052672B1 EP1052672B1 (fr) | 2004-10-13 |
Family
ID=9544732
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP00401028A Expired - Lifetime EP1052672B1 (fr) | 1999-04-22 | 2000-04-13 | Source ionique pour spectromètre de masse à temps de vol analysant des echantillons gazeux |
Country Status (6)
Country | Link |
---|---|
US (1) | US6545269B1 (fr) |
EP (1) | EP1052672B1 (fr) |
JP (1) | JP4395584B2 (fr) |
AT (1) | ATE279783T1 (fr) |
DE (1) | DE60014758T2 (fr) |
FR (1) | FR2792773B1 (fr) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6806467B1 (en) * | 2003-07-24 | 2004-10-19 | The Regents Of The University Of California | Continuous time-of-flight ion mass spectrometer |
US7420472B2 (en) * | 2005-10-16 | 2008-09-02 | Bao Tran | Patient monitoring apparatus |
JP6238978B2 (ja) | 2012-06-29 | 2017-11-29 | エフ・イ−・アイ・カンパニー | 多種イオン源 |
KR101786950B1 (ko) | 2014-12-30 | 2017-10-19 | 한국기초과학지원연구원 | 비행시간 질량분석기 |
US9899181B1 (en) | 2017-01-12 | 2018-02-20 | Fei Company | Collision ionization ion source |
US9941094B1 (en) | 2017-02-01 | 2018-04-10 | Fei Company | Innovative source assembly for ion beam production |
CN109461642B (zh) * | 2018-12-07 | 2024-04-02 | 中国烟草总公司郑州烟草研究院 | 一种离子引发电子轰击电离源 |
US11854777B2 (en) * | 2019-07-29 | 2023-12-26 | Thermo Finnigan Llc | Ion-to-electron conversion dynode for ion imaging applications |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2294539A1 (fr) * | 1974-12-13 | 1976-07-09 | Labo Electronique Physique | Dispositif ioniseur incluant une galette de microcanaux a emission electronique secondaire |
JPH1140069A (ja) * | 1997-07-24 | 1999-02-12 | Hamamatsu Photonics Kk | マイクロチャネルプレートを用いたイオン源 |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3852595A (en) * | 1972-09-21 | 1974-12-03 | Stanford Research Inst | Multipoint field ionization source |
US3819941A (en) * | 1973-10-15 | 1974-06-25 | Bendix Corp | Mass dependent ion microscope having an array of small mass filters |
US5659170A (en) * | 1994-12-16 | 1997-08-19 | The Texas A&M University System | Ion source for compact mass spectrometer and method of mass analyzing a sample |
-
1999
- 1999-04-22 FR FR9905088A patent/FR2792773B1/fr not_active Expired - Fee Related
-
2000
- 2000-04-13 AT AT00401028T patent/ATE279783T1/de not_active IP Right Cessation
- 2000-04-13 EP EP00401028A patent/EP1052672B1/fr not_active Expired - Lifetime
- 2000-04-13 DE DE60014758T patent/DE60014758T2/de not_active Expired - Fee Related
- 2000-04-14 US US09/550,171 patent/US6545269B1/en not_active Expired - Fee Related
- 2000-04-18 JP JP2000116162A patent/JP4395584B2/ja not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2294539A1 (fr) * | 1974-12-13 | 1976-07-09 | Labo Electronique Physique | Dispositif ioniseur incluant une galette de microcanaux a emission electronique secondaire |
JPH1140069A (ja) * | 1997-07-24 | 1999-02-12 | Hamamatsu Photonics Kk | マイクロチャネルプレートを用いたイオン源 |
Non-Patent Citations (1)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 1999, no. 05 31 May 1999 (1999-05-31) * |
Also Published As
Publication number | Publication date |
---|---|
ATE279783T1 (de) | 2004-10-15 |
JP4395584B2 (ja) | 2010-01-13 |
DE60014758D1 (de) | 2004-11-18 |
US20030057378A1 (en) | 2003-03-27 |
FR2792773A1 (fr) | 2000-10-27 |
DE60014758T2 (de) | 2006-03-09 |
FR2792773B1 (fr) | 2001-07-27 |
US6545269B1 (en) | 2003-04-08 |
EP1052672B1 (fr) | 2004-10-13 |
JP2000348665A (ja) | 2000-12-15 |
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