US3585383A - Microanalyzer for producing a characteristic ionic image of a sample surface - Google Patents

Microanalyzer for producing a characteristic ionic image of a sample surface Download PDF

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Publication number
US3585383A
US3585383A US518453A US3585383DA US3585383A US 3585383 A US3585383 A US 3585383A US 518453 A US518453 A US 518453A US 3585383D A US3585383D A US 3585383DA US 3585383 A US3585383 A US 3585383A
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United States
Prior art keywords
ions
arrangement
sample
energy
magnetic
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Expired - Lifetime
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US518453A
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English (en)
Inventor
Raymond Castaing
Georges Slodzian
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Centre National de la Recherche Scientifique CNRS
Thales SA
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Centre National de la Recherche Scientifique CNRS
CSF Compagnie Generale de Telegraphie sans Fil SA
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/44Energy spectrometers, e.g. alpha-, beta-spectrometers
    • H01J49/46Static spectrometers
    • H01J49/48Static spectrometers using electrostatic analysers, e.g. cylindrical sector, Wien filter
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02Details
    • H01J37/04Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/05Electron or ion-optical arrangements for separating electrons or ions according to their energy or mass
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/252Tubes for spot-analysing by electron or ion beams; Microanalysers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/10Ion sources; Ion guns
    • H01J49/14Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/142Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes
    • H01J49/28Static spectrometers
    • H01J49/284Static spectrometers using electrostatic and magnetic sectors with simple focusing, e.g. with parallel fields such as Aston spectrometer
    • H01J49/286Static spectrometers using electrostatic and magnetic sectors with simple focusing, e.g. with parallel fields such as Aston spectrometer with energy analysis, e.g. Castaing filter
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/44Energy spectrometers, e.g. alpha-, beta-spectrometers
    • H01J49/46Static spectrometers
    • H01J49/466Static spectrometers using crossed electric and magnetic fields perpendicular to the beam, e.g. Wien filter

Definitions

  • the present invention relates to microanalysers and more particularly to microanalysers making use of the secondary ion emission for producing, by means of a corpuscular optical system which combines ion optics and mass spectrography, characteristic images of the surface of the sample which indicate the map of distribution of its various elements or isotopes.
  • Microanalysers wherein the analysis of a sample takes place by collecting and focusing into an image of the sample the secondary ions emitted by the sample under the impact of a beam of primary positive ions, are known in the art.
  • a suitable optical system was described in the French Pat. No. 1,240,658 and in a scientific paper by the applicants R. CASTAING and G. SLODZIAN PREMIERS ESSAIS DE MICROSANALYSE PAR EMISSION IONIQUE SECON- DAIRE Comptes Rendus Academic des Sciences de Paris 255, 1893-1895 (15th Oct. 1962 Its operation is generally satisfactory. It has, however, the drawback of not allowing an easy separation of the secondary ions of high and nearly equal mass on account of the fact that all the secondary ions do not leave the sample at the same initial velocity.
  • the arrangement formicroanalysis by bombardment with primary positive ions or neutral atoms comprises an optical system for focusing secondary ions, including means for eliminating by filtering those secondary ions whose initial energy is higher than a predetermined value.
  • the said electron optical system includes a spherical capacitor which, by means of a slit, ensures the elimination of ions whose initial energy is higher than or different from a predetermined value.
  • the electron optical system includes means for deflecting the secondary ion beam onto an electrostatic mirror in order to eliminate the excessively fast ions while reflecting the others.
  • FIG. 1 shows very schematically a first embodiment of the invention
  • FIG. 2 shows in more detail a possible arrangement of the different parts according to this first embodiment
  • FIG. 3 shows another embodiment of the invention.
  • FIG. 4 shows in more detail a possible arrangement of the different parts according to this second embodiment.
  • a sample 1 emits, under the impact of a beam of positive primary ions or fast neutral atoms 2, characteristic secondary ions which are taken up by the acceleration optical system 3, comprising electrodes 31 to 33 and an aperture 34.
  • a spherical capacitor 4 is placed in the path of the beam oft secondary ions. It comprises two plates 41 and 42, held at different potentials by means of a source 5; it gives of the crossover of the acceleration optical system 3, which is located in the aperture 34, a real image crossover located in a symmetrical position, at a distance of the outlet of the spherical capacitor, equal to the radius of curvature of the mean ion trajectory.
  • a wall provided with a slit g, stops some of the ions which have gone through the capacitor 4, and the remaining ions are focused by a lens 10.
  • the optical system includes, in addition, the magnetic sector 6, which deflects ions which propagate through it and is adjustable by a suitable control device, and lastly an ion optical system 8 which comprises a selection slit 81, a stigmator and other electrodes (not shown) which are parts of an image converter, as disclosed in the above-mentioned French Patent.
  • the ions accelerated by electrodes 31 to 33 are deflected by capacitor 4 towards magnetic sector 6.
  • the angle of deflection of each ion trajectory depends on the energy of the corresponding ion. For the purpose of simplification, it is assumed that the ions considered are positive and of the single charge type.
  • ions whose initial energy is too low may be stopped by the lower edge of slit 9 and eliminated from the beam entering the magnetic sector 6 if that is considered necessary for the analytical procedure.
  • the electrostatic lens 10 is positioned and excited in such a way that the ion beam, after passing it, enters the magnetic sector under suitable conditions, as is known in the art and described in the French Patent No. 1,240,658, for ensuring focusing in both transverse directions and production of an exit crossover at the level of slit 81.
  • the radius of curvature of the trajectories in the magnetic sector depends only on the momentum of the emitted particle, for a given induction, that is to say on the value EM, where E is the energy of the particle and M is its mass number.
  • Diaphragm 34 does actually ensure some elimination of ions emitted at a certain initial velocity, but such filtering is insufiicient since it acts on the component of the initial velocity of the secondary ions perpendicular to the axis of the system only.
  • the spherical capacitor which deflects the ions as a function of their energy and not of their momentum, ensures a perfect filtering.
  • the optical system which comprises the first emission lens 3, the spherical capacitor 4, the intermediate lens 10 and the magnetic sector 6 gives, when properly adjusted, a characteristic image of the sample surface produced by ions of any desired mass, which is achromatic, that is to say insensitive to the slight heterogeneity of the ion energies which is allowed by the width of slit 9.
  • FIG. 2 shows in more detail a possible arrangement of the different parts.
  • the sample 1 is bombarded by the ion beam produced by the focusing gun 2 which comprises an ion source 21, excited by high frequency generator 211 and fed by gas inlet 212, and a condenser lens 22. Means for neutralizing the primary ions have not been represented here.
  • the secondary ions are accelerated and focused into an image of the sample surface by the emission lens 3 which comprises accelerating electrode 31, focusing electrodes 32 and 33 and aperture 34.
  • the crossover at the aperture34 acts as a source for the energy selecting spherical capacitor 4 comprising two plates 41 and 42.
  • the stigmator 82 corrects for astigmatism the characteristic image of the sample surface which is produced by the whole optical system. This image is then taken up by the image converter 1 I, known in the art, for convenient observation and recording through a window 111.
  • the system is evacuated through openings 01, 02, 03 and 04.
  • FIG. 3 shown another embodiment of a system according to the invention. shows for simplification, it is assumed that the secondary ions are positive, but negative secondary ions could be used as well in the embodiment of FIGS. 1 and 2 as in the embodiment of FIGS. 3 and 4.
  • FIG. 3 the same reference numerals designate the same parts as in FIG. I.
  • the shape of the magnetic sector 6 is as shown.
  • Electrode 103 is at a slightly higher positive potential than target 1.
  • This electrode may be provided with an aperture 105; in this case excessively fast ions pass through this aperture and do not return, while slower ions are decelerated and returned by electrode 103 towards the upper part 62 of sector 6 which deflects them towards selection slit 81, stigmator 82 and the image converter.
  • electrode 103 may be solid (devoid of the aperture 105) to capture excessively fast ions, while reflecting slower ions.
  • FIG. 3 provides, over that shown in FIG. 1, the additional advantage of making it possible to place the sample coaxially with the display screen (not shown).
  • the arrangement of FIG. 1 provides the advantage of making it possible to pick up for obtaining the image the secondary ions which are emitted by the sample with a given initial energy and rejecting those of the secondary ions which are emitted with a lower or higher initial energy.
  • FIG. 4 shows in more detail the arrangement of the various parts of the system; the mirror electrode 103 is in this figure devoid of the aperture 105 and it stops the ions whose energy is too high.
  • lens means for concentrating said secondary ions to form a beam providing an ionic image of the sample surface
  • magnetic field means positioned in the path of said filtered beam for rejecting therefrom the ions having a momentum different from a predetermined value, said magnetic means having an outlet and means located at said outlet for displaying said lOlllC image,
  • said magnetic field means comprise a magnetic sector and means for controlling the magnetic field in said sector
  • said eliminating means comprise a spherical capacitor, having two plates facing each other and an outlet, means for creating between said plates a direct current electric field, and a wall having a slit, being positioned near said outlet.
  • a primary ion source for bombarding said sample;
  • lens means for concentrating said secondary ions to form a beam providing an ionic image of the sample surface;
  • magnetic field means positioned in the path of said filtered beam for rejecting therefrom the ions having a momentum difi'erent from a predetermined value, said magnetic means having an outlet;
  • said magnetic filed means comprise a magnetic sector and means for controlling the magnetic field in said sector
  • said eliminating means comprise an ion mirror, said ion mirror comprising means for reflecting ions whose energy is lower than a predetermined level and for eliminating the other ions.
  • said mirror comprises an electrode which collects the ions having an energy higher than said predetermined level.
  • said mirror comprises an apertured electrode, having a center hole for allowing the ions, whose energy is higher than said predetermined level, to propagate beyond said mirror.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Electron Tubes For Measurement (AREA)
US518453A 1962-11-28 1966-01-03 Microanalyzer for producing a characteristic ionic image of a sample surface Expired - Lifetime US3585383A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR916836A FR1352167A (fr) 1962-11-28 1962-11-28 Nouveau dispositif de microanalyse par émission ionique secondaire

Publications (1)

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US3585383A true US3585383A (en) 1971-06-15

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US (1) US3585383A (enrdf_load_stackoverflow)
JP (2) JPS5211599B1 (enrdf_load_stackoverflow)
DE (1) DE1498646B2 (enrdf_load_stackoverflow)
FR (1) FR1352167A (enrdf_load_stackoverflow)
GB (1) GB1078823A (enrdf_load_stackoverflow)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3798447A (en) * 1970-05-27 1974-03-19 Onera (Off Nat Aerospatiale) Apparatus for directing an energizing beam on a sample to cause secondary ion emission
US3986025A (en) * 1973-06-08 1976-10-12 Hitachi, Ltd. Ion microanalyzer
US4296323A (en) * 1980-03-10 1981-10-20 The Perkin-Elmer Corporation Secondary emission mass spectrometer mechanism to be used with other instrumentation
US4694170A (en) * 1984-12-28 1987-09-15 Office National D'etudes Et De Recherches Aerospatiales Instrument for very high resolution ionic micro-analysis of a solid sample
US5721428A (en) * 1994-12-28 1998-02-24 Ebara Corporation Magnetic field type mass spectrometer
US20100072363A1 (en) * 2006-12-11 2010-03-25 Roger Giles Co-axial time-of-flight mass spectrometer
US20120261571A1 (en) * 2009-09-24 2012-10-18 Dietmar Funnemann Imaging energy filter for electrically charged particles and spectroscope having same
US9741525B1 (en) * 2016-02-02 2017-08-22 Fei Company Charged-particle microscope with astigmatism compensation and energy-selection

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1439064A (fr) * 1965-02-09 1966-05-20 Centre Nat Rech Scient Perfectionnements aux analyseurs ioniques
US3517191A (en) * 1965-10-11 1970-06-23 Helmut J Liebl Scanning ion microscope with magnetic sector lens to purify the primary ion beam
GB1171700A (en) * 1967-10-31 1969-11-26 Atomic Energy Authority Uk Improvements in or relating to Ion Beam Intensity Measuring Apparatus and Methods
US3558879A (en) * 1968-03-12 1971-01-26 Atomic Energy Commission Electrostatic deflector for selectively and adjustably bending a charged particle beam
JPS5531771U (enrdf_load_stackoverflow) * 1978-08-21 1980-02-29
JPS58116270A (ja) * 1981-12-30 1983-07-11 Nissan Motor Co Ltd 車体シ−ル構造
JPS59110473U (ja) * 1983-01-18 1984-07-25 トヨタ自動車株式会社 鋼板合わせ面の水入り防止構造
GB8725459D0 (en) * 1987-10-30 1987-12-02 Nat Research Dev Corpn Generating particle beams

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2947868A (en) * 1959-07-27 1960-08-02 Geophysics Corp Of America Mass spectrometer
US2976413A (en) * 1956-06-25 1961-03-21 Cons Electrodynamics Corp Mass spectrometer
US3061720A (en) * 1960-02-29 1962-10-30 Ewald Heinz Spectrograph
US3126477A (en) * 1964-03-24 Multiple dispersion mass spectrometer
US3174034A (en) * 1961-07-03 1965-03-16 Max Planck Gesellschaft Mass spectrometer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3126477A (en) * 1964-03-24 Multiple dispersion mass spectrometer
US2976413A (en) * 1956-06-25 1961-03-21 Cons Electrodynamics Corp Mass spectrometer
US2947868A (en) * 1959-07-27 1960-08-02 Geophysics Corp Of America Mass spectrometer
US3061720A (en) * 1960-02-29 1962-10-30 Ewald Heinz Spectrograph
US3174034A (en) * 1961-07-03 1965-03-16 Max Planck Gesellschaft Mass spectrometer

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Mass Spectrometer Image Displacements Due To Second-Order Aberrations by C. F. Robinson from THE REVIEW OF SCIENTIFIC INSTRUMENTS, Vol. 29, No. 7, July, 1958, Pgs. 622 624. Q184.R5 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3798447A (en) * 1970-05-27 1974-03-19 Onera (Off Nat Aerospatiale) Apparatus for directing an energizing beam on a sample to cause secondary ion emission
US3986025A (en) * 1973-06-08 1976-10-12 Hitachi, Ltd. Ion microanalyzer
US4296323A (en) * 1980-03-10 1981-10-20 The Perkin-Elmer Corporation Secondary emission mass spectrometer mechanism to be used with other instrumentation
US4694170A (en) * 1984-12-28 1987-09-15 Office National D'etudes Et De Recherches Aerospatiales Instrument for very high resolution ionic micro-analysis of a solid sample
US5721428A (en) * 1994-12-28 1998-02-24 Ebara Corporation Magnetic field type mass spectrometer
US20100072363A1 (en) * 2006-12-11 2010-03-25 Roger Giles Co-axial time-of-flight mass spectrometer
US8952325B2 (en) * 2006-12-11 2015-02-10 Shimadzu Corporation Co-axial time-of-flight mass spectrometer
US20120261571A1 (en) * 2009-09-24 2012-10-18 Dietmar Funnemann Imaging energy filter for electrically charged particles and spectroscope having same
US8530835B2 (en) * 2009-09-24 2013-09-10 Dietmar Funnemann Imaging energy filter for electrically charged particles and spectroscope having same
US9741525B1 (en) * 2016-02-02 2017-08-22 Fei Company Charged-particle microscope with astigmatism compensation and energy-selection

Also Published As

Publication number Publication date
GB1078823A (en) 1967-08-09
JPS4821314B1 (enrdf_load_stackoverflow) 1973-06-27
DE1498646A1 (de) 1968-12-12
JPS5211599B1 (enrdf_load_stackoverflow) 1977-03-31
DE1498646B2 (de) 1971-12-16
FR1352167A (fr) 1964-02-14

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