US3798447A - Apparatus for directing an energizing beam on a sample to cause secondary ion emission - Google Patents

Apparatus for directing an energizing beam on a sample to cause secondary ion emission Download PDF

Info

Publication number
US3798447A
US3798447A US00144078A US3798447DA US3798447A US 3798447 A US3798447 A US 3798447A US 00144078 A US00144078 A US 00144078A US 3798447D A US3798447D A US 3798447DA US 3798447 A US3798447 A US 3798447A
Authority
US
United States
Prior art keywords
sample
analysis apparatus
primary
accordance
chamber
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.)
Expired - Lifetime
Application number
US00144078A
Other languages
English (en)
Inventor
P Lanusse
R Hernandez
G Slodzian
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.)
Office National dEtudes et de Recherches Aerospatiales ONERA
Original Assignee
Office National dEtudes et de Recherches Aerospatiales ONERA
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 Office National dEtudes et de Recherches Aerospatiales ONERA filed Critical Office National dEtudes et de Recherches Aerospatiales ONERA
Application granted granted Critical
Publication of US3798447A publication Critical patent/US3798447A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

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
    • 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
    • H01J49/142—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers using a solid target which is not previously vapourised

Definitions

  • the ion energisation should therefore enable the exploitation fully of the performances of mass analysers with high separating power called double focusing, and in particular mass spectrographs of the Mattauch and Herzog'type in which there is produced by an ion beam of small aperture emerging from an image projected on an input slot, a double focusing by the conjunction of an electrostatic analyser and of a magnetic analyser imposing respectively on the ion beam to be analysed deviations of opposite sense, the resulting focusing being thus of the first order for the whole of the ion species to-be separated.
  • ion energising chambers of known type are badly adapted to mass analysers with double focusing since they do not enable, either the obtaining ofvsecondary ion beams of small aperture, the focusing an ion image in the plane of the input slit, or the obtaining of a uniform ionic illumination of the region of the sample to be analysed.
  • the chamber of ion emission by ionic excitation comprises two vacuum enclosures of which the first contains emitting and focusing means for a beam of primary ions extracted from a flow of gas or of vapor and of which the second comprises means for deflection and projection of the said primary beam on to a solid sample to be excited, the two enclosures being provided with independent vacuum means and communicating through an orifice of such dimensions that it gives passage to the useful portion of the said primary beam whilst limiting the flow rate of the passage of gas from the first enclosure towards the second enclosure.
  • This arrangement enables the obtaining of an excellent vacuum in the second enclosure by means of a small delivery pump but without risking polluting the residual atmosphere, the said pump being advantageously an ion, pump whose action is possibly completed by a sublimator.
  • the second enclosure comprises an ion optic device forming an ion image carried by the beam of ions emit ted by the excited sample, or secondary ion beam, in the plane of an orifice formed in the said second enclosure and substantially coincidant with the input orifice of the analyser, the two enclosures being relatively arranged in such a way that the axis of the primary beam before passage into the deflection means of the second enclosure and the axis of the secondary beam are substantially at right-angles and the said deflecton means bend the primary beam on to the sample to be energised
  • This arrangement enables the ion optic device-to be housed in the second enclosure without impeding the passage of the primary beam.
  • Deflection means for the primary beam into the second enclosure comprise two pairs of electrodes acting respectively on the orientation of the-said beam in perpendicular directions and borne respectively to adjustable continuous potentials and/or adjustable alternating potentials of which the frequencies aredifferent,
  • these electrodes enabling a defined zone of the sample to be swept by the primary beam.
  • the face of the sample subjected to the impact of th primary ions is covered by a metal screen advantageously monoisotopic borne to the same potential as the sample and pierced by an orifice limiting the area of particle fall-back.
  • the combination of these features enables the obtaining of an excellent resulution of the analysis in area and in depth without pollution of the limitrophic zones.
  • the second enclosure contains a samplecarrier device which frees the face of the example nonexposed to the impact of the primary beam, and a retractable electronic gun projecting an electron beam on to the said non-exposed face, thus enabling, if necessary, rapid heating and without polluton of the said sample, in the course of examination if such is necessary.
  • the enclosure 1, vacuum-tight, of the ion emission chamber according to the invention communicates a. by a flange 2, with a sump and a valve not shown enabling the introduction of the borne object 3 without breaking the vacuum, I
  • the gas to be ionised by the gun 6 penetrates through the passage 11 under a pressure of 10' bars.
  • the gun of known type, delivers through the central orifice, of a diameter of 0.5 mm of the extraction electrode 6, brought to a potential of 29 kV, ions whose average energy is of the order of l 000 to l 500 electron-volts.
  • the chamber 5, called space-gun comprises means 12, shown by a rectangle in discontinuous lines, enabling acceleration of the ions to 30 kilovolts and focusing of them onto the central aperture, of diameter 0.5 mm, of the diaphragm 4 of monoisotopic metal for example of tantalum, which separates the space-gun from the space-object.
  • the characteristics of the ion beam are for example the following intensity 10.10 A; aperture 2.4.10 radians; brilliance 6.6 A/cm2/steradian.
  • An oil diffusion pump provided with a liquid nitrogen trap, and acting in the enclosure 5 through the orifice 13, ensures. a pumping flow rate of 100 litres per second for a pressure of 2.5.10 bars.
  • the vacuum necessary in the enclosure 1 is ensured firstly by an absorption pump then by anion pump of the triode type, the said pumps acting through the orifice 10.
  • the triode pump of which tthe total delivery rate is of the order of 100 litres per second, enables the obtaining in the enclosure 1 of a total pressure of the order of 10 bars.
  • the combination of the pumping means described with the diaphragm 4 separating the space-gun from the space-object is extremely advantageous. It enables the use, for the pumping of the space-gun of a high delivery pump and; for the pumping of the space-object of a triode pump with much lower delivery rate, but ensuring a high vacuum without risk of contaminating the space-object by hydrocarbon vapors, of flexible and positive usefulness and preserving a notable pumping delivery rate even for the rare gases (helium, argon etc. introduced into the gun to produce the primary ion beam.
  • the rare gases helium, argon etc.
  • the object-carrier 3 supports a metallic tube 14, open at both ends on which is fixed the object or target 15, for example by means of a metallic collar not shown supporting the target 15, by its periphery, against the tube 14.
  • the primary ion beam emerging from the central orifice of the diaphragm 4 is firstly guided by two pairs of deflection plates, the first pair 16 being shown in section and the second pair 17 in superposition, then passes through a tantalum diaphragm 18 having a central orifice of diameter 1.5 mm, and whose role is to avoid electrostatic charges of the insulating supports (not shown) of the plates 17 from disturbing the beam, finally it is directed to the center of the target by a spherical deflector 19 of known type.
  • spherical deflectors can be used, either for example, a deflector for bombarding the object 15 with positive ions, or again a 45 deflector followed by a neutralising chamber 20, such as a metallic tube filled with gas or vapor to bombard the object with neutral atoms of variable energy, obtained by exchange of charges.
  • the guide and deflection device described above comprises also a diaphragm 21 of metal advantageously monoisotopic, such as tantalum or gold, placed at a slight distance from the surface of the sample 15, held at the same potential as the said sample, for example by electrical contact and comprising a central orifice of diameter about 3mm.
  • the said diaphragm 21 protects the limitrophic zones of the object from the examination zone against the pollution by neutral particles torn of by the impact of the primary beam and by the secondary ions reflected by the adaptation optics which will be considered below.
  • the object-carrier 3 being provided with mechanical means (not shown) actuated from outside the enclosure 1 for translation of the object in the plane of the face examined whilst the diaphragm 20 is rigidly fixed to the enclosure 1, it is thus possible to proceed to the analysis of superficial layers of an extended region of the said examined face without risking closer and closer contamination.
  • pairs of electrodes 16 and 17 they are on one hand respectively polarised by continuous voltages of adjustable value enabling the obtaining of a precise guidance of the primary beam, on the other hand respectively polarised by alternating voltages of adjustable amplitude, the frequency supplying one pair being much greater than the frequency supplying the other pair.
  • the amplitudes of the alternating voltages are adjusted so that the primary beam sweeps through the orifice of the diaphragm l5 and without contact with the edges of the said orifice a zone of predetermined location and dimensions of the surface under examination, the said zone being thus uniformly illuminated by the primary beam and the eroded layers being of regular thickness. If the surface under examination is flat, the facet uncovered by erosion is also flat and lends itself to further examination.
  • the invention hence enables mass spectral analysis effected layer by layer with an excellent definition in depth.
  • the FIGURE shows also an electron gun 22 enabling in the course of operation, the local heating of the object 15 by its rear face.
  • the said gun can be retracted by means of its support 23 actuated from the outside to enable translation of the object-carrier 3.
  • the FIGURE shows also a cryogenic pumping device constituted by a toric reservoir 24 of metal, a good conductor of heat which can be filled from the outside, by
  • the enclosure 1 contains lastly an ionic optics device enabling the projection of the ionic image of the examined zone of the object 15 into the plane of the input slit 9 of the mass spectral analyser 8.
  • This device comprises an accelerating electrode 26 connected to the earth or to ground and followed by an electrostatic lens constituted by three electrodes 27, 28, 29, the electrodes 27 and 29 being grounded and the electrode 28 being brought to a high DC voltage.
  • the ion optics are calculated to give the observed zone of the object 15 an image with an amplification of two-thirds in the plane of the slit 9.
  • the deflection plates 16 and 17 can be arranged on both sides of the spherical deflector 19 or again upstream or downstream of the said deflector with respect to the direction of flow of the primary ions;
  • the excitation chamber according to the invention is usable both with a mass spectrometer and with a massspectrograph or with a mass spectral analyser effecting both functions.
  • Mass spectrometric analysis apparatus comprising 7 a chamber for ionic emission energization containing at least one solid sample for spectral mass analysis thereof, said chamber including means for directing a primary, energizing beam upon said sample so that said sample emits a secondary ion beam and a metallic diaphragm positioned parallel to and closely adjacent the face of the sample upon which said primary beam is directed, said metallic diaphragm having an orifice therein defining a passage for said primary beam substantially the size of the surface of said sample impinged by said beam and for said secondary ion beam emitted by said sample, said apparatus further comprising means for maintaining said metallic diaphragm at the same potential as the sample.
  • Mass spectrometric analysis apparatus comprising means for deflecting said primary beam, said deflecting means comprising first and second pairs of electrodes located so as to act on said primary beam in mutually perpendicular planes, means for applying a potential of variable amplitude and a first frequency to said first pair of electrodes, means for applying a potential of variable amplitude and a second, different frequency to said second pair of electrodes, and means for controlling the amplitude of said potentials so that the primary beam sweeps an area on the surface of the sample substantially the size of said orifice in said diaphragm.
  • Mass spectrometric analysis apparatus comprising a cryogenic container located adjacent the sample around said primary beam and said secondary ion beam emitted by said sample, said cyrogenic container being filled with liquified gas.
  • Mass spectrometric analysis apparatus comprising a chamber for ionic emission energization containing at least one solid sample for spectral mass analysis thereof, said chamber including means for directing a primary, energizing beam upon the sample so that said sample omits a secondary ion beam and a sample carrier for supporting the sample so that one face thereof is exposed to the primary beam and another surface of said sample opposed to said exposed surface is free, said chamber further containing an electron gun so located as to direct an electron beam against said another surface of the sample for providing localized heating of the sample.
  • Mass spectrometric analysis apparatus comprising a cryogenic container located adjacent the sample around said primary beam and said secondary ion beam emitted by said sample, said cryogenic container being filled with a liquified gas.
  • cryogenic container is of annular shape.
  • Mass spectrometric analysis apparatus comprising deflecting means for deflecting said primary, energizing beam and a neutralizing chamber positioned in the path of said primary beam between said deflecting means and said sample for producing an energizing beam containing neutral particles.
  • said neutralizing chamber comprises a metal tube filled with a fluid for bombarding the sample with neutral atoms of variable energy obtained by charge exchange.
  • Analysis apparatus in accordance with claim 7 further comprising a retractable support for mounting said electron gun.

Landscapes

  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
US00144078A 1970-05-27 1971-05-17 Apparatus for directing an energizing beam on a sample to cause secondary ion emission Expired - Lifetime US3798447A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR7019276A FR2087652A5 (fr) 1970-05-27 1970-05-27

Publications (1)

Publication Number Publication Date
US3798447A true US3798447A (en) 1974-03-19

Family

ID=9056188

Family Applications (1)

Application Number Title Priority Date Filing Date
US00144078A Expired - Lifetime US3798447A (en) 1970-05-27 1971-05-17 Apparatus for directing an energizing beam on a sample to cause secondary ion emission

Country Status (2)

Country Link
US (1) US3798447A (fr)
FR (1) FR2087652A5 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0155700A2 (fr) * 1984-03-22 1985-09-25 Nippon Telegraph And Telephone Corporation Appareil de spectrométrie quantitative de masse des ions secondaires
US4556794A (en) * 1985-01-30 1985-12-03 Hughes Aircraft Company Secondary ion collection and transport system for ion microprobe
EP0249424A3 (en) * 1986-06-11 1989-01-18 Vg Instruments Group Limited Glow discharge mass spectrometer
US20070045534A1 (en) * 2005-07-08 2007-03-01 Zani Michael J Apparatus and method for controlled particle beam manufacturing
US20100181473A1 (en) * 2007-07-21 2010-07-22 Paul William Miles Blenkinsopp Method and apparatus for the analysis of samples
US7993813B2 (en) 2006-11-22 2011-08-09 Nexgen Semi Holding, Inc. Apparatus and method for conformal mask manufacturing
US10566169B1 (en) 2008-06-30 2020-02-18 Nexgen Semi Holding, Inc. Method and device for spatial charged particle bunching
US11335537B2 (en) 2008-06-30 2022-05-17 Nexgen Semi Holding, Inc. Method and device for spatial charged particle bunching

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3005099A (en) * 1957-10-26 1961-10-17 Centre Nat Rech Scient X-ray diffractograph enabling diagrams to be taken at very high temperatures
US3124680A (en) * 1958-09-13 1964-03-10 Agent
CH464571A (de) * 1966-08-25 1968-10-31 Philips Nv Massenspektrometer
US3415985A (en) * 1962-11-28 1968-12-10 Centre Nat Rech Scient Ionic microanalyzer wherein secondary ions are emitted from a sample surface upon bombardment by neutral atoms
US3418465A (en) * 1965-08-17 1968-12-24 Zeiss Jena Veb Carl Radiation source for reducing specimen contamination in electron microscopes
US3517191A (en) * 1965-10-11 1970-06-23 Helmut J Liebl Scanning ion microscope with magnetic sector lens to purify the primary ion beam
US3585383A (en) * 1962-11-28 1971-06-15 Centre Nat Rech Scient Microanalyzer for producing a characteristic ionic image of a sample surface

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3005099A (en) * 1957-10-26 1961-10-17 Centre Nat Rech Scient X-ray diffractograph enabling diagrams to be taken at very high temperatures
US3124680A (en) * 1958-09-13 1964-03-10 Agent
US3415985A (en) * 1962-11-28 1968-12-10 Centre Nat Rech Scient Ionic microanalyzer wherein secondary ions are emitted from a sample surface upon bombardment by neutral atoms
US3585383A (en) * 1962-11-28 1971-06-15 Centre Nat Rech Scient Microanalyzer for producing a characteristic ionic image of a sample surface
US3418465A (en) * 1965-08-17 1968-12-24 Zeiss Jena Veb Carl Radiation source for reducing specimen contamination in electron microscopes
US3517191A (en) * 1965-10-11 1970-06-23 Helmut J Liebl Scanning ion microscope with magnetic sector lens to purify the primary ion beam
CH464571A (de) * 1966-08-25 1968-10-31 Philips Nv Massenspektrometer

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
A Theoretical Assessment of the Possibility of Selected Area Mass Spectrometric Analysis Using a Focused Ion Beam by J. V. P. Long from the British Journal of Applied Physics, Vol. 16, Sept., 1965, pages 1277 1284. *
Mass Spectrometric Micro Surface Analysis published by the Geophysics Corporation of America, Bedford, Mass. *

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0155700A2 (fr) * 1984-03-22 1985-09-25 Nippon Telegraph And Telephone Corporation Appareil de spectrométrie quantitative de masse des ions secondaires
EP0155700A3 (en) * 1984-03-22 1987-05-13 Nippon Telegraph And Telephone Corporation Apparatus for quantitive secondary ion mass spectrometry
US4766313A (en) * 1984-03-22 1988-08-23 Nippon Telegraph & Telephone Public Corporation Apparatus for quantitative secondary ion mass spectrometry
US4556794A (en) * 1985-01-30 1985-12-03 Hughes Aircraft Company Secondary ion collection and transport system for ion microprobe
EP0249424A3 (en) * 1986-06-11 1989-01-18 Vg Instruments Group Limited Glow discharge mass spectrometer
US4853539A (en) * 1986-06-11 1989-08-01 Vg Instruments Group Limited Glow discharge mass spectrometer
US7488960B2 (en) 2005-07-08 2009-02-10 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US7495242B2 (en) 2005-07-08 2009-02-24 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US20070278419A1 (en) * 2005-07-08 2007-12-06 Nexgensemi Holdings Corporation Apparatus and method for controlled particle beam manufacturing
US20070284538A1 (en) * 2005-07-08 2007-12-13 Nexgensemi Holdings Corporation Apparatus and method for controlled particle beam manufacturing
US20070284527A1 (en) * 2005-07-08 2007-12-13 Zani Michael J Apparatus and method for controlled particle beam manufacturing
US20070284537A1 (en) * 2005-07-08 2007-12-13 Nexgensemi Holdings Corporation Apparatus and method for controlled particle beam manufacturing
US20070045534A1 (en) * 2005-07-08 2007-03-01 Zani Michael J Apparatus and method for controlled particle beam manufacturing
US7495244B2 (en) 2005-07-08 2009-02-24 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US7495245B2 (en) 2005-07-08 2009-02-24 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US7259373B2 (en) 2005-07-08 2007-08-21 Nexgensemi Holdings Corporation Apparatus and method for controlled particle beam manufacturing
US7501644B2 (en) 2005-07-08 2009-03-10 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US7659526B2 (en) 2005-07-08 2010-02-09 Nexgen Semi Holding, Inc. Apparatus and method for controlled particle beam manufacturing
US7993813B2 (en) 2006-11-22 2011-08-09 Nexgen Semi Holding, Inc. Apparatus and method for conformal mask manufacturing
US8278027B2 (en) 2006-11-22 2012-10-02 Nexgen Semi Holding, Inc. Apparatus and method for conformal mask manufacturing
US20100181473A1 (en) * 2007-07-21 2010-07-22 Paul William Miles Blenkinsopp Method and apparatus for the analysis of samples
US10566169B1 (en) 2008-06-30 2020-02-18 Nexgen Semi Holding, Inc. Method and device for spatial charged particle bunching
US11335537B2 (en) 2008-06-30 2022-05-17 Nexgen Semi Holding, Inc. Method and device for spatial charged particle bunching
US11605522B1 (en) 2008-06-30 2023-03-14 Nexgen Semi Holding, Inc. Method and device for spatial charged particle bunching
US11699568B2 (en) 2008-06-30 2023-07-11 NextGen Semi Holding, Inc. Method and device for spatial charged particle bunching

Also Published As

Publication number Publication date
FR2087652A5 (fr) 1971-12-31

Similar Documents

Publication Publication Date Title
KR100232430B1 (ko) 성분 분석장치와 방법
US5654545A (en) Mass resolution in time-of-flight mass spectrometers with reflectors
Brutschy et al. A high-intensity beam of metastable helium atoms with good velocity resolution
US5742049A (en) Method of improving mass resolution in time-of-flight mass spectrometry
US5146088A (en) Method and apparatus for surface analysis
US4633084A (en) High efficiency direct detection of ions from resonance ionization of sputtered atoms
US3517191A (en) Scanning ion microscope with magnetic sector lens to purify the primary ion beam
US6974957B2 (en) Ionization device for aerosol mass spectrometer and method of ionization
US7230234B2 (en) Orthogonal acceleration time-of-flight mass spectrometer
EP3234978B1 (fr) Dispositif d'ionisation et spectromètre de masse en étant équipé
JP3556667B2 (ja) イオン銃及びこれを使用する質量分析計
US3619605A (en) Mass spectrometer method and apparatus employing high energy metastable ions to generate sample ions
US3798447A (en) Apparatus for directing an energizing beam on a sample to cause secondary ion emission
US3955091A (en) Method and apparatus for extracting well-formed, high current ion beams from a plasma source
Ninomiya et al. Development of a vacuum electrospray droplet ion gun for secondary ion mass spectrometry
US3937958A (en) Charged particle beam apparatus
US6236054B1 (en) Ion source for generating ions of a gas or vapor
US4166952A (en) Method and apparatus for the elemental analysis of solids
CN114068288A (zh) 具有掺杂气辅助的电离的解吸离子源
US3622782A (en) Blocking apparatus and method utilizing a low-energy ion beam
US4670651A (en) Apparatus for performing the SNMS method
GB2386747A (en) Fullerene ion gun
US11367587B2 (en) Gas field ionization source
US4447724A (en) Apparatus for the chemical analysis of samples
US3731089A (en) Mass spectrometer ion source having means for rapidly expelling ions from the source and method of operation