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EP2394290B1 - Magnetisches achromatisches massenspektrometer mit doppelfokussierung - Google Patents

Magnetisches achromatisches massenspektrometer mit doppelfokussierung Download PDF

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Publication number
EP2394290B1
EP2394290B1 EP20100701685 EP10701685A EP2394290B1 EP 2394290 B1 EP2394290 B1 EP 2394290B1 EP 20100701685 EP20100701685 EP 20100701685 EP 10701685 A EP10701685 A EP 10701685A EP 2394290 B1 EP2394290 B1 EP 2394290B1
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Prior art keywords
electrostatic
axis
aberrations
mass
mass spectrometer
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French (fr)
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EP2394290A1 (de
Inventor
Emmanuel De Chambost
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Cameca SAS
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Cameca SAS
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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
    • H01J49/32—Static spectrometers using double focusing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/06—Electron- or ion-optical arrangements

Definitions

  • the present invention relates to a dual focus achromatic magnetic mass spectrometer.
  • Mass spectrometers are devices that allow the characterization of the chemical structure of molecules constituting a sample or analyte. Mass spectrometry is thus a micro-analysis technique typically requiring only a few picomoles of the sample, to extract characteristic information as to its molecular weight or even its molecular structure.
  • mass spectrometers There are different types of mass spectrometers, among which are mainly time-of-flight mass spectrometers, quadrupole mass spectrometers and magnetic mass spectrometers.
  • mass spectrometers among which are mainly time-of-flight mass spectrometers, quadrupole mass spectrometers and magnetic mass spectrometers.
  • optical is for the future to be considered in its broadest sense, here applied to ion optics.
  • SIMS mass spectrometry
  • Secondary Ion Mass Spectrometry that is, “Secondary Emission Mass Spectrometry”.
  • One of the problems specific to this analysis technique is that accelerated ions in the mass spectrometer have a high energy dispersion.
  • chromatic properties of mass spectrometers and in particular the devices treating ions with a wide dispersion of energy, reference will be made to the A. Benninghoven et al., Secondary Ion Mass Spectrometry, edited by John Wiley, 1987 . This book deals in particular with the SIMS technique.
  • the present invention is particularly in the field of mass spectrometers of the SIMS type.
  • mass spectrometers of this type it is known that the principle of secondary ion extraction results in a large energy dispersion of the emitted ions.
  • electrostatic sector between the sample and the magnetic sector, this electrostatic sector being intended to make the mass spectrometer achromatic for at least one mass.
  • the condition of achromatism is not attached to a given mass, but to a particular trajectory. If this trajectory is considered as the main axis of the spectrometer, it is said that the spectrometer is achromatic on the axis, and that it is not off the axis or "off axis”.
  • the present invention may relate as well to a so-called “mono-collection” spectrometer, that is to say capable of measuring a mass in the axis, that to a mass spectrometer said to " multi-collection ", that is to say able to simultaneously measure several masses.
  • a mass spectrometer said to “ multi-collection ", that is to say able to simultaneously measure several masses.
  • it is possible to measure several masses simultaneously by arranging a plurality of collectors on the focusing plane of the mass spectrometer.
  • the blur observed at the point of focus of a given mass different from the mass on the axis, when the energy distribution of the ions is relatively wide, is called off-axis chromatic aberration.
  • H the blur observed at the point of focus of a given mass different from the mass on the axis, when the energy distribution of the ions is relatively wide.
  • M0 is the mass on the main axis for which the chromatic focusing is well done
  • ⁇ E the energy dispersion of the beam
  • ⁇ x1 the blur formed at the point where the trajectories of the mass M1 are focused in opening.
  • the Mattauch-Herzog spectrometer also known from the state of the art, is characterized in particular by the fact that the output face of the magnet is aligned with the entry point. This particular configuration allows a certain number of remarkable properties, and in particular makes it possible to offer an achromatism for different masses. However, it is sometimes very advantageous for a mass spectrometer to have a large mass dispersion, and in this case, the Mattauch-Herzog spectrometer is not appropriate.
  • second-order aberrations are produced in mass spectrometers comprising a magnetic sector and an electrostatic sector, these second order aberrations are noted in accordance with the use in the field of optics or ion optics: a first aberration noted x / aa proportional to square of the angle of aperture in the radial plane, a second aberration x / bb proportional to the square of the opening angle in the transverse plane, a third aberration x / ae proportional to the opening angle in the radial plane and away in relative energy, and a fourth aberration x / ee proportional to the square of the difference in relative energy.
  • this type of spectrometer is not stigmatic, that is to say that it is impossible to have at the output of the spectrometer the ionic microscope function which makes it possible to visualize an image of the sample, filtered mass. .
  • hexapoles can correct second-order aberrations.
  • a hexapole is a set of six poles arranged around the main axis, and alternately set to an electric potential + V or -V.
  • Spectrometers known from the state of the art are equipped with corrective electrostatic hexapoles: a single focus mass spectrometer as described in the European patent application EP 0124440 or a dual-focus mass spectrometer as described in US Pat. US 4,638,160 .
  • the advantage of introducing electrostatic hexapoles to reduce aberrations is that it is then possible to adjust the aberration correction as finely as possible by adjusting the excitation voltage of the hexapole while observing a signal characteristic of the fineness of the spot, as for example, the signal resulting from the scanning of the beam on the edge of the exit slot of the spectrometer, arranged upstream of a counting member or the projection on an ion-photon conversion device such as a micro-channel slab, from the image of the ion beam to the plane of the exit slit.
  • An object of the present invention is to overcome at least the aforementioned drawbacks, by proposing a solution for significantly reducing the four second-order aberrations, as well as the out-of-axis chromatic aberrations, while allowing modulation of the mass dispersion, for example a reduction of the mass dispersion to concentrate the masses in the focal plane in order to reduce the travel of mobile collectors or an increase in dispersion mass to be able to measure closer masses with a multi-collection system.
  • the magnetic mass spectrometer may be characterized in that the second electrostatic device comprises an electrostatic lens and / or a quadrupole and / or an octopole centered on the main axis of the mass spectrometer and whose north and south poles located in the transverse plane and on an axis perpendicular to the radial axis are brought to an electrical potential V, and the east and west poles located on an axis located in the radial plane, perpendicular to the axis defined by the North and South poles, are brought to an electric potential -V.
  • the magnetic mass spectrometer may be characterized in that the first electrostatic device comprises a lens and / or a quadrupole and / or a multiplex activated as a stigmator.
  • the figure 1 presents, by a synoptic diagram, an example of an achromatic magnetic mass spectrometer on the axis known from the state of the art.
  • a magnetic mass spectrometer 100 is shown in a section in the radial plane.
  • the mass spectrometer 100 includes an inlet slot 101 and an exit slot 102.
  • a diaphragm 103 is located downstream of the inlet slot 101.
  • An electrostatic sector 104 is located downstream of the diaphragm 103.
  • a magnetic sector 105 is disposed downstream of the electrostatic sector 104.
  • An optical device 106 is located between the electrostatic sector 104 and the magnetic sector 105.
  • the radial plane is defined as the plane of symmetry of the mass spectrometer containing the main axis of the mass spectrometer 100, perpendicular to the large dimension of the entrance slot 101 and containing the main axis
  • the transverse plane is defined as the plane perpendicular to the radial plane, and which also contains the main axis of the mass spectrometer 100.
  • the mass spectrometer itself is located downstream of the inlet slit 101, and the ionization device, and the ion beam shaping devices up to at the entrance slot 101 are not shown in the figure. In the same way, the collection and measurement devices located downstream of the exit slot 102 are not shown.
  • the opening angle ⁇ of the ion beam is designated a.
  • the mass spectrometer shown in the figure is a Nier-Johnson spectrometer. This type of spectrometer is an example of an achromatic mass spectrometer on the axis. A particular configuration of the physical and geometrical characteristics of the mass spectrometer 100 allows the measurement in the axis of a given mass with a given mass resolution.
  • the figure 2 presents an overall diagram of an example of a magnetic mass spectrometer according to the present invention.
  • the magnetic mass spectrometer 200 includes an input slot 101, a plurality of output slots 102 for filtering the ion beams to a plurality of collectors not shown in the figure for the sake of clarity.
  • the mass spectrometer 200 also comprises a first diaphragm 103, an electrostatic sector 104, a magnetic sector 105.
  • the mass spectrometer 200 further comprises, upstream of the electrostatic sector 104, a first electrostatic device 201 located downstream of the electrostatic gap. 101, a first hexapole 202 downstream of the first electrostatic device 201 and upstream of the diaphragm 103.
  • the mass spectrometer 200 Downstream of the electrostatic sector 104 and upstream of the magnetic sector 105, the mass spectrometer 200 comprises, in series, a first optical device 211, a second hexapole 212, a second diaphragm 213, a second optical device 214, a third hexapole 215 and a third optical device 216.
  • the mass spectrometer 200 Downstream of the magnetic sector 105 and upstream of the output slots 102, the mass spectrometer 200 comprises in series a fourth hexapole 221 and a second electrostatic device 222.
  • optical and electrostatic devices to be considered in a broad sense as optical ion systems electrostatic, which may include lenses with symmetry of revolution, anisotropic lenses more or less effective respectively in the radial plane and in the transverse plane or multipoles for achieving achromatism on the axis, such as commonly used devices in dual mass spectrometers focusing or multipoles also to treat trajectories differently in the transverse plane, as is described for example in the book by E. de Chambost et al. supra.
  • first electrostatic device 201 and the second electrostatic device 222 located respectively between the input slot 101 and the output of the electrostatic sector 104, and between the magnetic sector 105 and the output slots 102, which solves the problem. both the problem of the modulation of mass dispersion and the problem of suppressing off-axis chromatic aberration. In both cases, it is the second electrostatic device 222 which is active, but as it creates a defocusing of the image of the entrance slot 101 to the detection plane, it is necessary to compensate this effect with the first electrostatic device 201 It is necessary that the first electrostatic device 201 be located neither in the region where the trajectories are dispersed in mass, nor in those where they are dispersed in energy.
  • the present invention proposes to arrange in the part where the trajectories are dispersed in mass, that is to say between the magnetic sector 105 and the exit slots 102, a focusing device - the second electrostatic device 222.
  • the second electrostatic device 222 is necessarily more efficient peripherally than in the center, and its convergence is necessarily inversely proportional to the energy of the particle.
  • This adjustment can for example be done using a suitable calculation program or by using appropriate measures that can characterize the fineness of the beam or the displacement of the beam resulting from an energy shift.
  • suitable calculation programs ISIOS described by MIYavor, ASBerdnikov in "ISIOS: a program to calculate imperfect particle optical systems" (Nucl.Instr and Meth in Phys Res, Vol 363, No.
  • This same electrostatic device 222 may be used, excited otherwise, that is to say polarized with different voltages, when the problem is not to reduce out-of-axis aberrations, but to modulate the mass dispersion.
  • the parasitic side effect is the displacement of the plane of the image of the entrance slot. This parasitic side effect is compensated by the first electrostatic device 201 which has the same effect on the trajectories, whatever the mass of the ion in question.
  • the second electrostatic device 222 downstream of the magnetic sector 105, produces in a plane normal to the axis, an electric field all the more important that the point is considered distant from the axis. This electric field is of opposite sign according to whether one is on the side of the weak masses or the side of the strong masses.
  • These electrostatic means may be an electrostatic lens centered on the axis, that is to say a series of revolution symmetry electrodes polarized by applied voltages.
  • These electrostatic means may also be a quadrupole device such that the plane containing one of the pairs of opposite poles contains the radial plane of the spectrometer.
  • These electrostatic means can also be an octopole where the poles located on the Ox and Oy axes are excited as quadrupoles, and the diagonal poles are set to zero.
  • the electrostatic means located between the input slot 101 and the output of the electrostatic sector 104 are intended to reconstruct the opening focus which is broken by the activation of the devices located between the magnet and the detection.
  • the first hexapole 202 arranged in the example of the figure between the input slot 101 and the electrostatic sector 104, is particularly dedicated to the cancellation of the second aberration of the second order x / bb.
  • the fourth hexapole 221, disposed between the magnetic sector 105 and the detection plane on which the output slots 102 are located, is particularly dedicated to the cancellation of the first second order aberration x / aa.
  • the second hexapole 212 disposed near the second diaphragm 213 forming an energy slot, is particularly dedicated to the cancellation of the fourth second order aberration x / ee.
  • the third hexapole 215, disposed between the second diaphragm 213 and the magnetic sector 105, is particularly dedicated to the cancellation of the third aberration of the second order x / ae.
  • the system for varying the magnitudes in the radial plane and in the transverse plane, comprising in particular the optical devices 211, 214 and 216, can be for example that described in the European patent application. EP0473488 supra.
  • the figure 3a presents a preferred embodiment for the magnetic sector 105 of the magnetic mass spectrometer 200 according to the invention.
  • the structure of the mass spectrometer is for example of the Nier-Johnson type.
  • the magnetic sector 105 produces on the main axis a deflection of the trajectory of the ions by an angle of 90 °.
  • the trajectory of the ions on the main axis has a radius of curvature equal to 585 mm.
  • the input and output faces 301 and 302 of the magnetic sector 105 have, relative to the plane normal to the axis, an angle of 27 °, in order to give the magnetic sector 105 stigmatic properties, according to a configuration in itself known from the state of the art.
  • Point of focusing of the mass on the main axis is located at a distance of 1220 mm from the output of the magnetic sector 105.
  • the figure 3b presents a preferred embodiment for the second electrostatic device 222.
  • Three different trajectories for three different masses M0, M1 and M2 are represented.
  • M0 is the mass on the main axis.
  • a tangent plane P is also represented; this plane P is an approximation of the surface on which the different masses M0, M1 and M2 focus.
  • the figure 3c presents a perspective view of a preferred embodiment of an example octopole forming the second electrostatic device 222.
  • the octopole 222 comprises eight poles North, Northeast, East, Southeast, South, Southwest , West and Northwest formed by eight cylindrical bars arranged around the main axis.
  • the North-South axis is perpendicular to the radial plane, and located in the transverse plane.
  • the East-West axis is perpendicular to the North-South axis, and located in the radial plane.
  • the octopole 222 100 mm deep may be disposed 460 mm upstream of the focal point of the mass M0.
  • the eight poles of the octopole can be located on a circle with a radius of 75 mm.
  • the diameters of the cylindrical poles may be about 30 mm. If we wish to compress the positive ion trajectories and reduce the mass dispersion, then the North-West, North-East, South-East and South-West poles of the octopole can be excited at 0 Volt, the poles East and West at a positive potential + V, and the North and South poles at potential -V.
  • the typical value of the voltage V which cancels out-of-axis chromatic aberrations is 300 volts, for a kinetic energy of the ions of 10 keV.
  • the application of a voltage on the poles has the effect of tightening the dispersed paths in mass, thus reducing the mass dispersion, typically by a factor of 2/3.
  • an electrostatic lens rather than an octopole, that is to say for example a so-called Einzel lens
  • an active electrode of the same internal diameter as the octopole
  • the additional convergence introduced by the second electrostatic device 222 disrupts the focusing in opening of the entrance slot 101 to the plane of the exit slot 102.
  • a device must be activated. focalisant located in a region where the beam is neither dispersed in mass nor dispersed in energy.
  • a stigmator function may be integrated in the electrostatic sector 104, as illustrated by FIG. figure 3d .
  • the figure 3d shows an exemplary embodiment of an electrostatic sector 104, in sectional view in a plane perpendicular to the main axis of the mass spectrometer.
  • the electrostatic sector 104 comprises, for example, a pair of additional external parallel plates 341 and a second pair of internal parallel plates 342, called Matsuda plates or, according to the English terminology, "flat Matsuda", arranged on a truncated spherical electrostatic sector. consisting of an outer electrode 343 where is applied, in the case of positively charged ions, a + Ve voltage, and an inner electrode 344 where is applied, always in the case of positively charged ions, a voltage -Ve .
  • the two outer plates 341, symmetrical with respect to the radial plane are interconnected, and the inner two plates 342 are also interconnected.
  • the additional plates 341 and 342, give the truncated sector a full spherical symmetry if they are applied respective voltages V ext and V int determined by the calculation or by experience.
  • V ext and V int from V hex and V stig voltages that can of course be controlled by computer.
  • the application on the plates 341 and 342 of a common V stig component creates a stigmatory effect which can be judiciously used to compensate for the defocusing created by the second electrostatic device 222 disposed downstream of the magnetic sector. 105, but without any effect on the bulk dispersion. In this embodiment, it is therefore possible to substitute the Matsuda plates 341 and 342 for the first electrostatic device 201.
  • An advantage of the invention is that this method should be performed once and only once during the life of the mass spectrometer 200.

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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
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Claims (3)

  1. Magnetisches Massenspektrometer mit Doppelfokussierung (200), das eine Ionenquelle, einen Eintrittsschlitz (101), einen elektrostatischen Sektor (104), einen magnetischen Sektor (105) und Mittel (102) zum gleichzeitigen Erkennen von wenigstens einer Ionenmasse und Folgendes umfasst:
    - eine erste elektrostatische Vorrichtung (201), die sich zwischen der Ionenquelle und dem Ausgang des elektrostatischen Sektors (104) befindet und den Ionenstrahl auf die Hauptachse des Massenspektrometers (200) fokussiert;
    - eine zweite elektrostatische Vorrichtung (222), die unterhalb des magnetischen Sektors (104) angeordnet ist und in der Längssymmetrieebene ein radiales elektrisches Feld erzeugt, das umso stärker ist, je weiter der betrachtete Punkt von der Achse entfernt ist, und dessen jeweilige Vorzeichen auf der Seite von schwachen Massen und auf der Seite von starken Massen entgegengesetzt sind;
    dadurch gekennzeichnet, dass:
    - der elektrostatische Sektor (104) ein abgeflachter sphärischer elektrostatischer Sektor ist, umfassend eine äußere Elektrode (343), an der eine Spannung +Ve anliegt, eine innere Elektrode (344), an der eine Spannung -Ve anliegt, wobei die äußere Elektrode (343) und die innere Elektrode (344) darüber hinaus ein Paar äußere parallele Platten (341), die auf beiden Seiten der äußeren Elektroden (343) angeordnet sind und an denen eine Spannung Vext anliegt, und ein Paar innere parallele Platten (342), die auf beiden Seiten der inneren Elektrode (344) angeordnet sind und an denen eine Spannung Vint anliegt, umfassen, wobei die Paare von inneren und äußeren parallelen Platten (341, 342) die erste elektrostatische Vorrichtung (201) bilden;
    wobei die jeweils an die äußere und innere (341, 342) parallele Platte angelegten Spannungen Vext, Vint jedesmal auf eine selbe Spannungsdifferenz ΔV eingestellt werden, wenn die zweite elektrostatische Vorrichtung (222) aktiviert wird, um die Massendispersion zu modulieren oder um den achsversetzten Chromatismus zu annulieren, so dass der Ionenstrahl entsprechend der Masse auf der Achse immer auf der Hauptachse fokussiert bleibt.
  2. Magnetisches Massenspektrometer (200) nach Anspruch 1, dadurch gekennzeichnet, dass die zweite elektrostatische Vorrichtung (222) eine elektrostatische Linse und/oder ein Quadrupol und/ein Oktopol umfasst, die/das auf der Hauptachse des Massenspektrometers (200) zentriert ist und an dessen Nord- und Südpolen, die sich in der Transversalebene und auf einer Achse lotrecht zur radialen Achse befinden, ein elektrisches Potential V anliegt, und an dessen Ost- und Westpolen, die sich auf einer Achse befinden, die in der radialen Ebene lotrecht zu der durch die Nord- und Südpole definierten Achse liegt, ein elektrisches Potential -V anliegt.
  3. Magnetisches Massenspektrometer (200) nach einem der vorherigen Ansprüche, dadurch gekennzeichnet, dass es darüber hinaus Mittel zum Annulieren von Aberrationen der zweiten Ordnung umfasst, wobei die Mittel Folgendes umfassen:
    - ein erstes Hexapol (202), das die Aberrationen der zweiten Ordnung proportional zum Quadrat des Öffnungswinkels in der Transversalebene annuliert, Aberrationen in x/bb genannt,
    - ein zweites Hexapol (212), das die Aberrationen der zweiten Ordnung proportional zum Quadrat der relativen Energieabweichung annuliert, Aberrationen in x/ee genannt,
    - ein drittes Hexapol (215), das die Aberrationen der zweiten Ordnung proportional zum Öffnungswinkel in der radialen Ebene und zur relativen Energieabweichung annuliert, Aberrationen in x/ae genannt,
    - ein viertes Hexapol (221), das die Aberrationen der zweiten Ordnung proportional zum Quadrat des Öffnungswinkels in der radialen Ebene annuliert, Aberrationen in x/aa genannt.
EP20100701685 2009-02-06 2010-01-29 Magnetisches achromatisches massenspektrometer mit doppelfokussierung Active EP2394290B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0950764A FR2942072B1 (fr) 2009-02-06 2009-02-06 Spectrometre de masse magnetique achromatique a double focalisation.
PCT/EP2010/051101 WO2010089260A1 (fr) 2009-02-06 2010-01-29 Spectrometre de masse magnetique achromatique a double focalisation

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EP2394290A1 EP2394290A1 (de) 2011-12-14
EP2394290B1 true EP2394290B1 (de) 2015-04-29

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EP (1) EP2394290B1 (de)
JP (1) JP5521255B2 (de)
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WO (1) WO2010089260A1 (de)

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US9594879B2 (en) 2011-10-21 2017-03-14 California Instutute Of Technology System and method for determining the isotopic anatomy of organic and volatile molecules
GB2561998A (en) * 2012-10-10 2018-10-31 California Inst Of Techn Mass spectrometer, system comprising the same, and methods for determining isotopic anatomy of compounds
LU92981B1 (en) * 2016-02-19 2017-09-08 Luxembourg Inst Science & Tech List Extraction system for charged secondary particles for use in a mass spectrometer or other charged particle device
CA3097198A1 (en) * 2018-04-30 2019-11-07 Leidos, Inc. A low-power mass interrogation system and assay for determining vitamin d levels _______________________________________________

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FR1576381A (de) * 1968-02-16 1969-08-01
JPS59117055U (ja) * 1983-01-28 1984-08-07 日本電子株式会社 質量分析装置
US4507555A (en) * 1983-03-04 1985-03-26 Cherng Chang Parallel mass spectrometer
FR2544914B1 (fr) * 1983-04-19 1986-02-21 Cameca Perfectionnements apportes aux spectrometres de masse
FR2545651B1 (fr) 1983-05-03 1986-02-07 Cameca Spectrometre de masse a grande luminosite
FR2558988B1 (fr) * 1984-01-27 1987-08-28 Onera (Off Nat Aerospatiale) Spectrometre de masse, a grande clarte, et capable de detection multiple simultanee
JPH03269944A (ja) * 1990-03-20 1991-12-02 Jeol Ltd 同時検出型質量分析装置
FR2666171B1 (fr) * 1990-08-24 1992-10-16 Cameca Spectrometre de masse stigmatique a haute transmission.
US6614026B1 (en) * 1999-04-15 2003-09-02 Applied Materials, Inc. Charged particle beam column
US6979818B2 (en) * 2003-07-03 2005-12-27 Oi Corporation Mass spectrometer for both positive and negative particle detection

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FR2942072A1 (fr) 2010-08-13
US8373121B2 (en) 2013-02-12
FR2942072B1 (fr) 2011-11-25
JP5521255B2 (ja) 2014-06-11
US20120032075A1 (en) 2012-02-09
EP2394290A1 (de) 2011-12-14
JP2012517083A (ja) 2012-07-26
WO2010089260A1 (fr) 2010-08-12

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