EP1052672A1 - Flugzeitmassenspektrometerionenquelle zur Analyse von Gasproben - Google Patents

Flugzeitmassenspektrometerionenquelle zur Analyse von Gasproben Download PDF

Info

Publication number: EP1052672A1
Authority: EP; European Patent Office
Prior art keywords: electron; ion source; electrons; flow; mass spectrometer
Prior art date: 1999-04-22
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

Application number

EP00401028A

Other languages

English (en)

French (fr)

Other versions

EP1052672B1 (de

Inventor

Didier Pierrejean

Bruno Galland

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Alcatel Lucent SAS

Nokia Inc

Original Assignee

Alcatel SA

Nokia Inc

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

1999-04-22

Filing date

2000-04-13

Publication date

2000-11-15

2000-04-13 Application filed by Alcatel SA, Nokia Inc filed Critical Alcatel SA

2000-11-15 Publication of EP1052672A1 publication Critical patent/EP1052672A1/de

2004-10-13 Application granted granted Critical

2004-10-13 Publication of EP1052672B1 publication Critical patent/EP1052672B1/de

2020-04-13 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

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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)

EP00401028A 1999-04-22 2000-04-13 Flugzeitmassenspektrometerionenquelle zur Analyse von Gasproben Expired - Lifetime EP1052672B1 (de)

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 (de)	2000-11-15
EP1052672B1 EP1052672B1 (de)	2004-10-13

Family

ID=9544732

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP00401028A Expired - Lifetime EP1052672B1 (de)	1999-04-22	2000-04-13	Flugzeitmassenspektrometerionenquelle zur Analyse von Gasproben

Country Status (6)

Country	Link
US (1)	US6545269B1 (de)
EP (1)	EP1052672B1 (de)
JP (1)	JP4395584B2 (de)
AT (1)	ATE279783T1 (de)
DE (1)	DE60014758T2 (de)
FR (1)	FR2792773B1 (de)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
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
US8575542B1 (en) *	2012-04-18	2013-11-05	Bruker Daltonics, Inc.	Method and device for gas-phase ion fragmentation
EP2867915B1 (de)	2012-06-29	2016-07-13	FEI Company	Multispezies-ionenquelle
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)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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 DE DE60014758T patent/DE60014758T2/de not_active Expired - Fee Related
- 2000-04-13 AT AT00401028T patent/ATE279783T1/de not_active IP Right Cessation
- 2000-04-13 EP EP00401028A patent/EP1052672B1/de not_active Expired - Lifetime
- 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)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 1999, no. 05 31 May 1999 (1999-05-31) *

Also Published As

Publication number	Publication date
JP2000348665A (ja)	2000-12-15
ATE279783T1 (de)	2004-10-15
DE60014758T2 (de)	2006-03-09
FR2792773B1 (fr)	2001-07-27
FR2792773A1 (fr)	2000-10-27
US6545269B1 (en)	2003-04-08
EP1052672B1 (de)	2004-10-13
DE60014758D1 (de)	2004-11-18
US20030057378A1 (en)	2003-03-27
JP4395584B2 (ja)	2010-01-13

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