EP0125950A2 - Massenspektrometer - Google Patents

Massenspektrometer Download PDF

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Publication number
EP0125950A2
EP0125950A2 EP84400707A EP84400707A EP0125950A2 EP 0125950 A2 EP0125950 A2 EP 0125950A2 EP 84400707 A EP84400707 A EP 84400707A EP 84400707 A EP84400707 A EP 84400707A EP 0125950 A2 EP0125950 A2 EP 0125950A2
Authority
EP
European Patent Office
Prior art keywords
ions
envelope
sector
magnetic sector
magnetic
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
Application number
EP84400707A
Other languages
English (en)
French (fr)
Other versions
EP0125950B1 (de
EP0125950A3 (en
Inventor
Georges Slodzian
Jean-Claude Lorin
Roger Dennebouy
Marcel Chaintreau
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.)
Cameca SAS
Original Assignee
Cameca SAS
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.)
Filing date
Publication date
Application filed by Cameca SAS filed Critical Cameca SAS
Publication of EP0125950A2 publication Critical patent/EP0125950A2/de
Publication of EP0125950A3 publication Critical patent/EP0125950A3/fr
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Publication of EP0125950B1 publication Critical patent/EP0125950B1/de
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    • 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
    • H01J49/28—Static spectrometers
    • H01J49/30—Static spectrometers using magnetic analysers, e.g. Dempster spectrometer
    • 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
    • H01J49/28—Static spectrometers
    • H01J49/32—Static spectrometers using double focusing
    • H01J49/326—Static spectrometers using double focusing with magnetic and electrostatic sectors of 90 degrees

Definitions

  • the present invention relates to a mass spectrometer comprising an ion source, means of acceleration capable of imparting to the ions an energy essentially dependent on their electric charge, means for establishing in a sector a magnetic field orthogonal to the plane of the trajectory of the ions to curve this trajectory, and means for detecting ions.
  • a mass scan can be carried out which makes it possible to pass frequently from one isotope to another or from one element to another if it is desired to obtain the precise value of a report.
  • Such mass scanning would be superfluous if the spectrometer were provided with multiple outputs allowing the simultaneous collection, on separate detectors, of several ionic species.
  • multiple output spectrometers are generally designed for particular applications so that it is often difficult, even impossible without structural transformation, to change the nature of the few elements initially provided; these multiple output spectrometers are also expensive. Mass scanning therefore remains the most widespread solution and makes it possible to work, at different times, on isotopes of different masses, with a scan fast enough in time to attenuate the drift of the ion source. .
  • the main object of the invention is to provide a mass spectrometer in which mass scanning can be carried out precisely and quickly.
  • a mass spectrometer of the kind defined above is characterized in that it comprises, at the entrance to the magnetic sector, electrostatic means capable of modifying the tangential speed of the ions, and therefore their energy, from in such a way that ions of different masses can, at different times, follow the same curved trajectory in the magnetic sector.
  • the spectrometer comprises, at the outlet of the magnetic sector, electrostatic means capable of canceling the modification. tion of tangential speed introduced by electrostatic means located at the entrance to the magnetic sector.
  • electrostatic means located at the entrance to the magnetic sector.
  • the ions after having been accelerated by the acecieration means and after having received a determined energy, describe their trajectory, under vacuum, in a metallic enclosure brought to the potential of the mass;
  • the means suitable for modifying the tangential speed of the ions can include a metallic envelope with a closed transverse contour, open at its two ends, and the mean line of which corresponds to the trajectory provided for the ions, this envelope being placed in the magnetic field and s extension of re-entry of the magnetic sector at the exit of this sector, and being brought to the same electrical potential as transverse electrodes located at the entry of the envelope and suitable for creating an electrostatic field of tangential acceleration or braking, essentially parallel to the direction of the speed of the ions at the entry of this envelope.
  • This insulated metal envelope placed in the electromagnetic field, that is to say between the poles of the electromagnet, makes it possible to keep the poles of the magnet grounded, without this resulting in an influence on the ions whose Renergy, modified at the entry of the magnetic field, remains constant in this field.
  • the electric voltage intended to create the electrostatic field of tangential acceleration, at the center of the magnetic sector could be directly applied to the poles of the magnet.
  • the electrical voltage intended to create a tangential acceleration (positive or negative) at the input of the magnetic sector is of the order of a few hundred volts, so that the control of variations in this voltage can be carried out more precise and faster than for a much higher tint.
  • the voltage increments can reach only 15 nillivclts, which allows a high precision of the pointing of a line.
  • the invention advantageously applies to mass spectrometers with double focusing.
  • the objective of which is to allow the precise measurement of the isotopic abundance ratios with a mass spectrometer and more particularly with a mass spectrometer of the ion analyzer type, generally with double focusing.
  • the ions are produced by a phenomenon of secondary ion emission, that is to say that a sample of the material to be analyzed is bombarded with ions; this bombardment causes the ejection of ions characteristic of the material to be analyzed.
  • the analysis performed by the spectrometer relates to these ejected ions.
  • the ions thus ejected exhibit a fairly large dispersion of energy at the start of the target (formed by the material to be analyzed); this energy dispersion is much higher than that which exists when the ions are emitted by thermionic effect.
  • the phenomenon of secondary ion emission produces both polyatomic ions and single ions which can have neighboring masses.
  • magnesium has three isotopes 24m g, 25 Mg, 26 Mg; the vacuum, bombardment conditions or the very nature of the sample mean that there are often ions of the MgH + type which are superimposed on the ions of the Mg + type .
  • the ion source drifts require a mass scan which makes it possible to pass frequently from one isotope to another or from one element to another if one wants to obtain the precise value of a ratio.
  • the invention specifically proposes to improve this mass scanning.
  • This spectrometer comprises an ion source 1 operating according to the phenomenon of secondary ionic emission.
  • This source 1 comprises a target 2 formed by a sample of the material to be analyzed, which is bombarded by ions coming from a source not shown.
  • the entire mass spectrometer is in a closed enclosure, not shown, in which a sufficient vacuum has been established.
  • Acceleration means A are adapted to communicate to the ions ejected from the target 2 an energy essentially dependent on their electrical charge.
  • These means A comprise an electrode E situated in a plane perpendicular to the direction ⁇ of the movement of the ions. This electrode E is disturbed, with respect to target 2, at a potential communicating the desired energy to the ions.
  • the electrostatic field of acceleration between the electrode E and the target Z is parallel to the path of the ions-
  • the electrode E can be brought to the potential of the mass, in which case the target 2 is brought to a positive potential if one wishes accelerate positive ions, or to negative potential for negative ions.
  • the acceleration potential is of the order of several thousand volts, for example of the order of 4000 volts.
  • the ions after being accelerated, circulate in a metallic tubular enclosure 3 brought to the same potential as the electrode E and serving as protection.
  • the ion beam passes through a first electrostatic optic 4 and passes through an inlet diaphragm 5 then enters an electrostatic sector 6 between two concentric curved walls 7 and 8, brought to different potentials so that the electrostatic field in sector 6 is oriented radially.
  • This electrostatic sector produces a first focusing of the ions at the opening 9 of a second diaphragm 10.
  • the direction of the trajectory of the ions, at the exit of the electrostatic sector 6, has turned by a certain angle relative to its direction of entry, this angle being 90 ° in the example of FIG. 1.
  • Means formed by an electromagnet including a pole It is schematically represented, are provided for establishing in a magnetic sector 12 a magnetic field orthogonal to the plane of the path of the ions, that is to say orthogonal to the plane of the Figure 1, suitable for bending the trajectory of the ions.
  • An electrostatic coupling lens 13 is provided between the electrostatic sector 6 and the magnetic sector 12.
  • Selection slots 14 are provided in the focusing zone created by the magnetic sector 12.
  • Ion detection means comprise a detection system 15 located downstream of a collecting lens 16.
  • the spectrometer comprises, at the input 17 of the magnetic sector 12 electrostatic means 18 suitable for modifying the tangential speed of the ions and therefore their energy, in such a way that ions of different masses can, at different instants, follow the same curved trajectory in the magnetic sector 12.
  • the fixed magnetic field, in sector 12 is adjusted so as to address the isotope 25 in the middle of the slot 14. If we also want to address the isotope 25 Mg, but the 24 Mg isotope in the middle of the slit 14, in accordance with the invention, without modifying the magnetic field, the ions are accelerated positively along the direction of their trajectory 17 in sector 12 of such so that the 24 Mg isotope can rotate along the same trajectory as that previously followed by the 25 Mg isotope.
  • the ions, at reentry 17, are subjected to a negative acceleration, that is to say braking along the direction of their trajectory, such so that the 26 Mg isotope follows the same trajectory as that previously followed by the 25 Mg isotope.
  • Electrostatic means 19 are provided at the outlet 20 of the sector 12 to cancel the modification of energy introduced by the means 18. In other words, if the means 18 have positively accelerated the ions at the entry, the means 19 exert braking to return these ions to their initial energy, and conversely, if the means 18 have exerted a braking, the means 19 exert an acceleration.
  • the means 18 comprise a metal casing 21, in particular of copper coated with gold, with a closed transverse contour (see FIG. 4), open at its two ends 22,23, and the mean line of which corresponds to the trajectory provided for the ions in sector 12.
  • This envelope 21 is placed in the magnetic field and extends from the input 17 to the output 20 of sector 12.
  • This envelope 21 is brought to the same electrical potential as transverse metal electrodes or plates 24, connected to this envelope, and located at the entrance 17 of sector 12.
  • These plates 24 are located opposite other transverse plates 25 of the end of the tubular enclosure 3 and brought to the same potential as this enclosure 3, that is to say -Tell the potential of the mass or potential 0.
  • the plates 24 and 25 are located in planes orthogonal to the mean direction of the trajectory of the ions at the level of these plates and form electrodes whose axis is aligned with that of the beam ions.
  • the electric field between these plates is oriented parallel to the axis of the beam.
  • the means 19 comprise other transverse plates, or electrodes, 26 provided at the end 23 of the envelope. These plates 26 are at the same potential as the envelope 21 and as the plates 24. Plates 27, at ground potential, are located opposite the plates 26, the planes of these plates being perpendicular to the axis of the beam d ions leaving sector 12. The electric field created between the plates 26 and 27 exerts an opposite effect, but of the same amplitude, as that produced by the plates 24, 25.
  • the plates 27 are integral with a metallic tubular screen e which is at the same potential as the plates 27 and which extends to the detection system.
  • the metal casing 21 protects the electrically charged ions in the magnetic sector 12 against external parasitic electrostatic influences. Therefore, the poles such as 11 of the electromagnet can be at ground potential without disadvantage.
  • the poles such as 11 of the electromagnet could be brought to the potential of the plates 24 and 26, in which case the metal casing 21 could be eliminated.
  • the cross section 28 (FIG. 4) of this casing is given a flattened shape, substantially in diamond shape, the major axis of which is located in the mediating plane of the air gap field, while the minor axis is located halfway across the air gap.
  • the lateral edges 28a, 28b of the envelope, which are radially spaced from the trajectory of interest, are more distant from the poles of the electromagnet than the central part 28c of the envelope 21; this results in a reduction in the stray capacitance which limits the switching time of the voltages applied to the envelope 21.
  • This envelope 21 advantageously includes, in its wall, steps 29 (FIG. 3) so that baffles are formed inside the envelope 21 to stop the ions whose masses are different from that at which one s' is of particular interest.
  • the magnetic poles 11a, and the magnetic sector 12a can have a shape substantially in Y, constituted by two arcs of a circle 30, 31, turning their convexity towards one another, tangent at one end and symmetrical to one another with respect to the tangent.
  • One of the branches, formed by the arc 30 located on the left of the representation of FIG. 3, is used for the mass spectrometer itself, while the other branch 31 is intended for a viewing device combined with the spectrometer massive.
  • the envelope 21 preferably has a shape similar to that of the magnetic sector 12a and comprises two branches in an arc 30a, 31a, connecting to the common end 32a. Only the branch 30a involved in the part of the spectrometer used for the ionic analyzer comprises the steps 29. The presence of the branch 31a makes it possible to avoid parasitic phenomena, in particular distortions on the image observed in this part of the apparatus. .
  • the focusing effects which may be introduced by electrostatic means 18, 19, the plates 24 and 25 on the one hand and 26, 27 on the other hand, are given a shape allowing avoid or reduce these parasitic focusing effects.
  • the optical properties of the acceleration and braking spaces can be taken into account as well as their deleterious effects on the double focusing.
  • Small "muultipotes" and in particular "quadruooles” 33, 34 suitably placed at the input and / or at the output of the magnetic sector make it possible to correct these parasitic effects. Voltages of a few volts are sufficient so that there is no difficulty in programming the quasi-simultaneous application of the voltage on the envelope 21 and of the voltages on the quadrupoles 33, 34.
  • the quadrupole 33 is formed by four rectangular metal plates arranged along the faces of a rectangular parallelepiped (see FIG. 5); the plates opposite two by two are brought to the medium; the neighboring plates located in orthogonal planes are therefore at different potentials.
  • the fixed value of the magnetic field does not have to be exactly set for a particular isotope to pass through the slots 14; this adjustment can be made directly by means of the voltage "v" applied to the metal casing 21.
  • the precision of the pointing of a line greatly exceeds the resolution in mass; indeed, an ⁇ M / M of 10 -5 is detectable. This precision can be used to determine exactly the nature of a polyatomic ion; it can also be used to address the lines in the middle of the selection slot 14; we can then give the latter the optimal width compatible with the elimination of the interfering ion and with a precise measurement of the intensity of the line because the risks of cutting by the lips of the slot are then minimized.
  • FIG. 2 shows an alternative embodiment according to which the magnetic sector 12 is located upstream of the electrostatic sector 6.
  • the same reference numerals as those in FIG. 1 are used, in FIG. 2, to designate identical or similar elements.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Electron Tubes For Measurement (AREA)
EP84400707A 1983-04-19 1984-04-10 Massenspektrometer Expired EP0125950B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8306375 1983-04-19
FR8306375A FR2544914B1 (fr) 1983-04-19 1983-04-19 Perfectionnements apportes aux spectrometres de masse

Publications (3)

Publication Number Publication Date
EP0125950A2 true EP0125950A2 (de) 1984-11-21
EP0125950A3 EP0125950A3 (en) 1986-04-23
EP0125950B1 EP0125950B1 (de) 1989-11-02

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ID=9287995

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84400707A Expired EP0125950B1 (de) 1983-04-19 1984-04-10 Massenspektrometer

Country Status (5)

Country Link
US (1) US4672204A (de)
EP (1) EP0125950B1 (de)
JP (1) JPS59205142A (de)
DE (1) DE3480366D1 (de)
FR (1) FR2544914B1 (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2620858A1 (fr) * 1987-09-18 1989-03-24 Jeol Ltd Instrument de spectrometrie de masse d'ions secondaires avec formation directe de l'image
EP0490626A2 (de) * 1990-12-10 1992-06-17 FISONS plc Massenspektrometer mit elektrostatischem Energiefilter
WO1992016008A1 (en) * 1991-03-11 1992-09-17 Fisons Plc Isotopic-ratio plasma source mass spectrometer
GB2270416A (en) * 1992-08-25 1994-03-09 Specs Ges Fuer Oberflaechenana Charged particles analyser
WO2003004892A1 (en) 2001-07-07 2003-01-16 Eaton Corporation Synchronizer

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8912580D0 (en) * 1989-06-01 1989-07-19 Vg Instr Group Charged particle energy analyzer and mass spectrometer incorporating it
US5128543A (en) * 1989-10-23 1992-07-07 Charles Evans & Associates Particle analyzer apparatus and method
FR2666171B1 (fr) * 1990-08-24 1992-10-16 Cameca Spectrometre de masse stigmatique a haute transmission.
GB9019560D0 (en) * 1990-09-07 1990-10-24 Vg Instr Group Method and apparatus for mass spectrometry
US7427752B2 (en) * 2002-11-15 2008-09-23 Micromass Uk Limited Mass spectrometer
EP1517353B1 (de) * 2003-09-11 2008-06-25 ICT Integrated Circuit Testing Gesellschaft für Halbleiterprüftechnik mbH System zur Verschmälerung der Energieverteilung eines Teilchenstrahls für ein Teichenstrahlsystem
EP1721330A2 (de) * 2004-03-05 2006-11-15 Oi Corporation Fokalebenen-detektorbaugruppe eines massenspektrometers
FR2942072B1 (fr) * 2009-02-06 2011-11-25 Cameca Spectrometre de masse magnetique achromatique a double focalisation.
GB2570954B (en) * 2012-10-10 2019-09-18 California Inst Of Techn Mass spectrometer, system comprising the same, and methods for determining isotopic anatomy of compounds
EP2988118A1 (de) * 2014-08-22 2016-02-24 MB Scientific AB Detektor von neutralem Atom oder Molekül
WO2017075470A1 (en) * 2015-10-28 2017-05-04 Duke University Mass spectrometers having segmented electrodes and associated methods

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3231735A (en) * 1959-06-11 1966-01-25 John L Peters Mass spectrometer leak detector with an accelerator section between plural analyzersand the method for using same
FR2015813A1 (de) * 1968-08-16 1970-04-30 Atomic Energy Authority Uk
US3866042A (en) * 1972-07-21 1975-02-11 Cameca Microanalyser convertible into a mass spectrometer

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3231735A (en) * 1959-06-11 1966-01-25 John L Peters Mass spectrometer leak detector with an accelerator section between plural analyzersand the method for using same
FR2015813A1 (de) * 1968-08-16 1970-04-30 Atomic Energy Authority Uk
US3866042A (en) * 1972-07-21 1975-02-11 Cameca Microanalyser convertible into a mass spectrometer

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
INSTRUMENTS AND EXPERIMENTAL TECHNIQUES, no. 1, janvier-février 1968, pages 155 et 156, New York, US; V.I. KARATAEV: "Chromatic aberration in a mass spectrometer with a two-stage homogeneous magnetic field" *
INSTRUMENTS AND EXPERIMENTAL TECHNIQUES, no. 3, mai/juin 1962, pages 529-533, New York, US; N.I. IONOV et al.: "Double magnetic mass spectrometer for analyzing small amounts of impurities" *
INTERNATIONAL JOURNAL OF MASS SPECTROSCOPY AND ION PHYSICS, vol. 8, no. 1, janvier 1972, pages 475-492, Elsevier Publishing Cy., Amsterdam, NL; A.J.H. BOERBOOM: "Ion optics of the electric hexapole" *
SPACE SCIENCE INSTRUMENTATION, vol. 2, no. 4, septembre 1976, pages 499-521, Ball Brothers, Research Corporation, Boulder, US; H. BALSIGER et al.: "A satellite-borne ion mass spectrometer for the energy range 0 to 16 keV" *
THE REVIEW OF SCIENTIFIC INSTRUMENTS, vol. 42, no. 4, avril 1971, pages 475 et 476, New York, US; H. BALSIGER et al.: "A mass spectrometer for the simultaneous measurement of the neutral and the ion composition of the upper atmosphere" *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2620858A1 (fr) * 1987-09-18 1989-03-24 Jeol Ltd Instrument de spectrometrie de masse d'ions secondaires avec formation directe de l'image
EP0490626A2 (de) * 1990-12-10 1992-06-17 FISONS plc Massenspektrometer mit elektrostatischem Energiefilter
EP0490626A3 (en) * 1990-12-10 1992-09-02 Fisons Plc Mass spectrometer with electrostatic energy filter
WO1992016008A1 (en) * 1991-03-11 1992-09-17 Fisons Plc Isotopic-ratio plasma source mass spectrometer
US5352893A (en) * 1991-03-11 1994-10-04 Fisons Plc Isotopic-ratio plasma source mass spectrometer
GB2270416A (en) * 1992-08-25 1994-03-09 Specs Ges Fuer Oberflaechenana Charged particles analyser
WO2003004892A1 (en) 2001-07-07 2003-01-16 Eaton Corporation Synchronizer

Also Published As

Publication number Publication date
DE3480366D1 (en) 1989-12-07
FR2544914A1 (fr) 1984-10-26
JPH0378742B2 (de) 1991-12-16
EP0125950B1 (de) 1989-11-02
EP0125950A3 (en) 1986-04-23
FR2544914B1 (fr) 1986-02-21
JPS59205142A (ja) 1984-11-20
US4672204A (en) 1987-06-09

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