EP2198449B1 - Hochauflösende weitwinkel-atomsonde - Google Patents

Hochauflösende weitwinkel-atomsonde Download PDF

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EP2198449B1
EP2198449B1 EP08838185.0A EP08838185A EP2198449B1 EP 2198449 B1 EP2198449 B1 EP 2198449B1 EP 08838185 A EP08838185 A EP 08838185A EP 2198449 B1 EP2198449 B1 EP 2198449B1
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detector
sample
electrode
probe according
atom probe
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EP2198449A1 (de
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Alain Bostel
Mikaïl YAVOR
Ludovic Renaud
Bernard Deconihout
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Centre National de la Recherche Scientifique CNRS
Cameca SAS
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Centre National de la Recherche Scientifique CNRS
Cameca SAS
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes
    • H01J49/34Dynamic spectrometers
    • H01J49/40Time-of-flight spectrometers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/0004Imaging particle spectrometry

Definitions

  • the present invention relates to improving the mass resolution of Large Angle Laser Tomographic Probes. It relates more particularly to the atomic probes called 3D atomic probes or "3D atom probe" according to the Anglo-Saxon name.
  • the atomic probe is an instrument well known to those skilled in the art which makes it possible to analyze samples on an atomic scale. Many instrumental configurations related to this analysis technique are described in the book " Atom probe field Ion microscopy, by Miller et al Published 1996by Clarendon Press / Oxford .
  • an essential parameter for obtaining a fine and precise measurement of the characteristics of the ions detected by an atomic probe is the measurement of the flight time of the ions detected, ie the time taken by the ion considered. to go through the space separating the sample from which they are torn from the detector. More specifically, the flight time is the time interval between an event triggering the pulling of the ion and its impact on the detector.
  • the triggering event may be an electrical pulse carried on the electrode next to the sample or a pulse of a laser beam directed on the sample.
  • the “Einzel” lens is, moreover, a device well known in the optics of charged particles and whose principle is not detailed here.
  • “Einzel” lenses please refer to volume 2 of the book “ Principles of electron optics, by PWHawkes and E. Kasper, published in 1989 by Academic Press .
  • tomographic atomic probes there are in particular the atomic probes known in the literature under the name of "3DAP” or " T ri D imensional A tom P gown” according to the Anglo-Saxon denomination or under the name of "PoSAP” or "Po sition ensitive S A P tom dress".
  • These probes are advantageously characterized by the fact that with such a detector both the moment of the impact, which measures the flight time of an ion, the position in a plane of this impact on the detector.
  • such a measure is only really possible if the position of the point of impact of a given ion is unequivocally linked to its position in the sample analyzed. This condition results in the fact that two distinct trajectories of ions must not lead to the same point of impact on the detector.
  • An object of the invention is to propose a solution for obtaining a tomographic probe, a pulsed 3D probe, a pulse probe laser in particular, simultaneously having a large angle of analysis (a large acceptance) and a large resolution in mass consecutive to a great length of flight.
  • the detector or a gate disposed near the detector is at a potential equal to that of the extractor.
  • the detector or a gate disposed near the detector, is placed at an intermediate potential between that of the sample and that of the extractor electrode.
  • the diameter d of the opening of the extractor is adapted to intercept the peripheral portion of the emitted ion beam so as to block the ions having the most peripheral trajectories.
  • the extractor comprises several diaphragms of different opening diameters, which can be alternately arranged at the central opening of the extractor.
  • the different diaphragms are made on a mobile bar slidable in front of the opening of the extractor so as to place the desired diaphragm in front of the opening; the slide movement of the bar being automated.
  • the three electrodes are configured and arranged in such a way as to leave a free space in the flight chamber sufficient to house a removable device for adjusting the probe.
  • a second electrostatic lens is placed between the first electrostatic lens and the detector.
  • the first electrostatic lens is configured to focus the least open paths near the median plane of the second electrostatic lens.
  • the invention has the advantage of making it possible, for a given opening angle of the emitted ion beam and a given detector surface, to produce a tomographic atom probe, in particular a "3D" probe, having a length of analysis. significantly higher than existing probes.
  • Figures 1 to 3 Figures which schematically show the basic structure of a tomographic atomic probe, including an atom probe called "3D" probe.
  • This type of probe is well known to those skilled in the art, so it is not a question in this document to describe in detail such a device.
  • the Figures 1 to 3 however, allow you to recall the following points.
  • a 3D tomographic atomic probe is intended to perform the analysis of a sample of material 11, atomic layer after atomic layer.
  • it basically comprises a sample holder on which is mounted the sample 11 of the material to be analyzed and a detector 12 located at a predetermined distance L of the sample. It also includes means (not shown on the figure 1 ) to evaporate (tear off), in ionic form, the atoms constituting the sample material analyzed and accelerate them so that the ions thus released follow a path that causes each ion 13 evaporated to strike the surface of the detector 12 in one given point 14 determined by the position of this ion on the surface of the sample before its tearing.
  • atom-by-atom erosion allowing a reconstruction of the composition of the atomic layer sample by atomic layer it is possible to determine the three-dimensional composition of the sample in question.
  • the probe also comprises a vacuum enclosure (not shown in FIG. figure 1 ), whose potential is, for example, that of the mass of the system in which the probe takes place.
  • a device comprising an ion source constituted by the sample 11, an analysis chamber, or flight chamber, of length L (analysis length) and a planar detector 12 whose dimensions cover a circular surface of diameter D.
  • the electric field prevailing in the flight chamber takes variable values and may for example be zero. In the latter case, the ions propagate at constant speed inside the flight chamber.
  • the detector At the arrival of an ion on the detector, it measures the position (x, y) on its surface of the point of incidence of the received ion. The detector also measures the "flight time", time counted from the moment corresponding to the tearing of the ion in question. A geometric correction is furthermore made to take into account the position of the point of impact in the calculation of the distance traveled between the tip and the detector. As a result, the position on the surface of the sample, occupied by the ion in question before it is torn off, is deduced in a known manner from the position of its point of impact on the surface of the detector, by application of a simple rule of projection.
  • the detector 12 also determines the instant of arrival of the considered ion, with respect to a known time reference, generally corresponding to the time at which the analysis began. of the sample 11.
  • a known time reference generally corresponding to the time at which the analysis began. of the sample 11.
  • the sample 11 is a piece of material having the shape of a substantially conical tip with an end forming a spherical cap of variable radius R over the analysis time.
  • the tomographic analysis consisting in tearing off, evaporating one after the other, the atoms forming the layers of atoms constituting the material, the radius of this spherical cap 21, initially of given value R 1 , a value R 2 corresponding to the spherical cap 22, existing at the end of the analysis; the erosion of the tip leading at the same time an equivalent variation in the distance between the sample 11 and the detector 12.
  • a tomographic atom probe can also be characterized, in known manner, by various parameters which are in particular its magnification G and by the potential difference V which must exist between the tip 11 constituting the sample and the input of the analysis chamber itself, potential difference responsible for the acceleration printed evaporated ions to cross the analysis chamber length L the electric field to be applied.
  • the coefficient b which depends on the geometry of the instrumentation, tip, detector and vacuum chamber is typically between 1 and 2.
  • the evaporated ions, by field effect, on the surface of the tip 11 are identified by time-of-flight mass spectrometry.
  • M represents the mass of the ion, v its velocity, n the number of elementary charges borne by the ion; e the elementary charge, ie the charge of the electron and V the acceleration voltage applied.
  • T The v
  • the mass resolution ⁇ M / M is proportional to the accuracy on the flight time ⁇ T / T, it is advantageous to have the greatest possible flight time T, and consequently the greatest distance L possible.
  • the measurement of the flight time is essential in the instrument to identify the ratio m / q of a detected ion, m being the mass of the ion and q its electric charge, it is advantageous to increase the distance L between the sample and the detector to also increase the flight time.
  • a device for focusing the ion beam emitted by the sample 11 on the detector 12 constituted.
  • This device can for example be constituted as illustrated by figure 4 by an electrostatic lens 41 such as an "Einzel" lens, a device well known in charged particle optics, placed between the sample 11 and the detector 12.
  • the "Einzel" lens consists of three electrodes 42, 43 and 44, placed in the path of the ions and configured to make a portion of the trajectory of these ions on an electric field which acts directly on this path. In this way the initially diverging beam 45 is modified into a convergent beam 46, the convergence obtained being a function of the intensity of the electric field produced.
  • the electrodes constituting the lens are placed at the appropriate potentials.
  • the "Einzel" lens may comprise a first electrode 42 placed in the vicinity of the sample 11, itself to ground, and then a second electrode 43 brought to a positive potential, then finally a third electrode 44 also grounded, so that at the exit of the lens, the ions continue their trajectories in a space without an electric field.
  • the first electrode 42 also plays the role of the extraction electrode, or counter electrode, or local electrode, which is generally implemented in the tomographic atomic probes to locate the electric field that produces the initial acceleration evaporated ions from the sample.
  • Such a focusing device advantageously makes it possible to limit the percentage of ions whose paths do not meet the detector. Nevertheless, its efficiency is generally limited by the fact that any electrostatic lens has what is called a spherical aberration which results in an overconversion of the outer region of the lens and a surfacing for the most eccentric trajectories which means that, as illustrated by Figures 5 and 6 (schematic sectional views) on two examples of lens configurations, the same point 51, 61, of the detector can intercept several distinct trajectories at once, resulting in a problem of indeterminacy of the original position of an ion having struck the detector at this point.
  • this corresponds for example to an atomic probe in which the sample 11 sees its tip brought to a voltage of 15kV, while the first electrode 42 of the "Einzel" lens (closest to the sample), which serves as an extractor electrode, is grounded, that the second electrode 43 is brought to a voltage of 14kV and that the third electrode 44 (closest to the detector) is also grounded, just like the detector 12.
  • the relative dimensions of the second and third electrodes are such that for the greater part of their path the ions remain under a focussing electric field.
  • this corresponds for example to an atomic probe in which the sample 11 sees its tip brought to a voltage of 15kV, while the first electrode 42 of the "Einzel" lens (closest to the sample), which serves as an extracting electrode, is grounded, that the second electrode 43 is brought to a voltage of 12.5kV and that the third electrode 44 (closest to the detector) is also grounded, just like the detector 12.
  • the relative dimensions of the second and third electrodes are such that for the greater part of their path the ions pass through. a space without a field, in which there is no focusing effect.
  • the probe according to the invention also comprises an accelerating electrode, or extractor, positioned near the sample and an electrostatic lens of the "Einzel" type for focusing the produced electron beam, consisting of three adjacent electrodes 71, 72 and 73, the first electrode of the "Einzel” lens being constituted by the accelerating electrode.
  • the electrodes of the electrostatic lens are polarized so that, taking into account the respective polarizations of the sample and the detector, the evaporated ions are initially accelerated towards the detector, to be then subjected for a part of their path, corresponding to the crossing of the lens, a focussing electric field.
  • the three electrodes are also preferably configured and arranged so as to provide the flight chamber with sufficient free space to house a removable device for adjusting the probe.
  • the adjustment device may be for example a field emission ion microscope or "Field ion microscope" according to the English name.
  • the zone of the detector may furthermore, according to the embodiment considered, be brought to an intermediate potential between that of the sample and that of the extracting electrode 71.
  • the setting of the potential considered is carried out directly or via a grid disposed near the detector. According to an alternative embodiment, this potential is that to which the extractor is carried.
  • the electrodes of the electrostatic lens consist of mechanical parts comprising a central opening and having a symmetry of revolution about a central axis, coinciding with the axis 74 joining the top of the tip forming the sample 11 of material to the detector 12 and perpendicular to the plane of the detector.
  • the first electrode 71, or extractor, located near the sample 11 and acting as an extracting electrode is preferably a thin piece having a hole 78 for passing ions, a circular hole for example.
  • the third electrode 73 of the electrostatic lens is any electrode, preferably of relatively small thickness and having a central opening 79 with a diameter greater than or at least approximately equal to the diameter D of the detector 12, so as to allow the propagation up to to the detector of evaporated ions, whatever the path taken by these ions in the lens.
  • Condition g) amounts to stating that all the points of the sectional profile 75 of the electrode situated between M 1 and M 3 must be situated outside the zone of the section plane delimited by the profile of a cone limited by the points M 2 and M 3 .
  • This resolution is advantageously obtained without undergoing at the detector the effects of confusion of the points of impact, or at least by undergoing these effects in a very weakened manner, effects consecutive to the spherical aberration of the electrostatic lens.
  • the opening angle remains otherwise unchanged, the resolution increase is done here without causing additional limitation of the analyzed surface.
  • the probe according to the invention makes it possible to increase very considerably the analysis length that can be used.
  • the intensity of the focus remains as for it defined by the value of the bias voltages applied to the different electrodes of the focussing lens produced.
  • the ion beam will be more or less focused, the objective being however that the focused beam covers the largest possible area on the detector.
  • the focused ion beam may then, for example, take the form of the beam 81 illustrated in FIG. figure 8 , or that of the beam 91 illustrated on the figure 9 .
  • the beam 81 is obtained by applying, for example, a voltage of 13.7 kV to the second electrode 72 and carrying the first and third electrode to ground, the detector itself being grounded and the sample being brought to a voltage of 15 kV.
  • the beam 91 is obtained by applying, for example, a voltage of 15.1 kV to the second electrode 72 and carrying the first and third electrode to ground, the detector and the sample being otherwise, as in the previous case, carried respectively to the ground and to a voltage of 15 kV.
  • the architecture of the atomic probe according to the invention corresponds to a basic common architecture, the probe according to the invention being able in practice to include certain variants corresponding to applications specific ones such as those presented in a nonlimiting manner in the following description.
  • the first electrode 71 constituting the focusing lens, the extracting electrode comprises a central opening 78 equipped with a multiple aperture device.
  • This device consists, as illustrated by figure 12 in a barrette of diaphragms 112 arranged to slide in front of the central opening 78 of the electrode 71.
  • the diameters of the various diaphragms 111 of the bar 112, smaller than that of the central opening 78, are defined so as to to decrease more or less strongly the diameter of the orifice of passage of ions emitted by the sample 11.
  • the diameter of the opening 78 so as to let the entire emitted ion beam 81 pass or to eliminate from the beam the ions presenting the most peripheral trajectories, in particular for limit the width of the analyzed sample surface and therefore the opening angle of the corresponding ion beam that will be detected by the sensor.
  • the diameter d of the opening of the extractor is thus adapted to intercept the peripheral portion of the emitted ion beam so as to block the ions having the most peripheral trajectories.
  • the different diaphragms are arranged on the bar so that the distance between two contiguous diaphragms is sufficient so that, with the exception of the diaphragm used, all the others are perfectly masked by the electrode.
  • the positioning in the two dimensions perpendicular to the axis of the beam can, moreover, be carried out by a suitable mechanism, possibly controlled by a computer and disposed outside the chamber of the probe.
  • the atomic probe according to the invention comprises a second focusing lens, of the "Einzel" lens type, for example, placed between the first lens and the detector.
  • This particular configuration makes it possible to compensate for the residual spherical aberration that the first focusing lens exhibits, despite its particular configuration, this spherical aberration of the first lens can not always be avoided.
  • the atomic probe according to the invention comprises, besides the three electrodes 71, 72 and 73 constituting the first lens, two complementary electrodes 132 and 133, the electrode 132 being placed adjacent to the electrode 73 and the electrode 133 being placed adjacent to the electrode 132, between this electrode and the detector 12.
  • the electrode 133 is brought to a potential substantially equal to that of the electrode 73, while the electrode 132 is brought to a potential allowing all three electrodes 73, 132 and 133 to constitute a second lens. electrostatic inside which reigns an electric field.
  • the electric field applied to the ion beam inside the second electrostatic lens may, depending on the case of use envisaged, be an accelerator or retarding field.
  • Such a device can for example be obtained from a structure such as that illustrated by FIG. figure 13 .
  • the detector 12 being brought to the ground potential and the sample 11 to a potential of 15 kV, the extraction electrode 71 is then grounded as well as the electrodes 73 and 133, while the central electrode 72 of the first
  • the lens is brought to a voltage of 15.3 kV and the central electrode 132 of the second lens is brought to a voltage of 14.5 kV.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Claims (15)

  1. Tomografische Atomsonde, die Folgendes umfasst:
    - eine Probentragvorrichtung zum Aufnehmen einer Probe (11) eines zu analysierenden Materials mit einer Extraktionszone mit einer im Wesentlichen spitzen Form,
    - einen positionsempfindlichen Detektor (12) mit einem nützlichen Durchmesser D, der von der Probe (11) um eine Distanz L beabstandet ist;
    - eine elektrostatische Linse bestehend aus drei Elektroden, einer ersten Elektrode (71) oder einem Extraktor, angeordnet in der Nähe der Probe (11), einer zweiten Elektrode (72), Zwischenelektrode genannt, und einer distalen dritten Elektrode (73), die zwischen der Zwischenelektrode (72) und dem Detektor (12) angeordnet sind, wobei die drei Elektroden eine Umdrehungssymmetrie um die Achse Oz aufweisen, die durch die Spitze der Probe und lotrecht zur Ebene P des Detektors verläuft;
    dadurch gekennzeichnet, dass, da die Distanz L größer ist als 2,75 D, die jeweiligen Potentiale der Probe (11), der ersten Elektrode (71) der Linse und des Detektors (12) so sind, dass die von der am Probenträger montierten Probe (11) ausgehenden Ionen zur ersten Elektrode (71) und zum Detektor (12) angezogen werden; wobei das Querschnittsprofil (74) der Zwischenelektrode (72), in einer durch die Achse Oz verlaufenden Querschnittsebene rOz, drei Punkte M1, M2 und M3 mit jeweiligen Koordinaten (r1, z1), (r2, z2) und (r3, z3) mit Bezug auf einen Ursprung z0 auf der Spitze der Probe definieren, die die folgenden Bedingungen erfüllen: z 1 < z 2 < z 3 ,
    Figure imgb0020
    | z 1 z 0 | < D / 3,
    Figure imgb0021
    | z 2 z 1 | < 0,65 D ,
    Figure imgb0022
    | z 3 z 1 | > 1,4 D ,
    Figure imgb0023
    r 2 = r 1 ,
    Figure imgb0024
    0,1 D < r 1 < 0,65 D ,
    Figure imgb0025
    D < r 3 < 1,6 D;
    Figure imgb0026
    wobei sich alle Punkte des Querschnittprofils der Elektrode außerhalb der Zone der durch das Profil (77) eines Kegels begrenzten Querschnittsebene befinden, am zylindrischen Ende durch die Punkte M1, M2 und M3 begrenzt.
  2. Tomografische Atomsonde nach Anspruch 1, dadurch gekennzeichnet, dass der Detektor (12) oder ein in der Nähe des Detektors angeordnetes Gitter auf einem Potential gleich dem des Extraktors (71) ist.
  3. Atomsonde nach Anspruch 1, dadurch gekennzeichnet, dass der Detektor oder ein in der Nähe des Detektors angeordnetes Gitter auf einem Zwischenpotential zwischen dem der Probe (11) und dem der Extraktorelektrode (71) ist.
  4. Tomografische Atomsonde nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass der Durchmesser d der Öffnung (77) des Extraktors (72) so bestimmt wird, dass der periphere Teil des emittierten Ionenstrahls abgefangen wird, um die Ionen mit den peripherischsten Flugbahnen zu sperren.
  5. Tomografische Atomsonde nach Anspruch 4, dadurch gekennzeichnet, dass der Extraktor mehrere Membranen (111) mit unterschiedlichen Öffnungsdurchmessern hat, die alternativ an der zentralen Öffnung (77) des Extraktors (72) angeordnet sein können.
  6. Tomografische Atomsonde nach Anspruch 5, dadurch gekennzeichnet, dass die unterschiedlichen Membranen (111) auf einem mobilen Steg (112) realisiert sind, der vor der Öffnung (77) des Extraktors (71) gleiten kann, um die gewünschte Membran vor der Öffnung zu platzieren; wobei die Gleitbewegung des Stegs automatisiert ist.
  7. Tomografische Atomsonde nach einem der vorherigen Ansprüche, dadurch gekennzeichnet, dass die drei Elektroden (71, 72 und 73) so konfiguriert und ausgelegt sind, dass in der Flugkammer ein freier Raum bereitgestellt wird, der zum Aufnehmen einer entfernbaren Vorrichtung zum Einstellen der Sonde ausreicht.
  8. Tomografische Atomsonde nach Anspruch 7, dadurch gekennzeichnet, dass der freie Raum zum Anordnen eines "Field Ion Microskope" in der Sonde ausreicht.
  9. Tomografische Atomsonde nach einem der vorherigen Ansprüche, dadurch gekennzeichnet, dass eine zweite elektrostatische Linse (73, 131 und 132) zwischen der ersten elektrostatischen Linse (71, 72 und 73) und dem Detektor (12) platziert ist.
  10. Tomografische Atomsonde nach Anspruch 9, dadurch gekennzeichnet, dass die erste elektrostatische Linse (71, 72 und 73) zum Fokussieren der am wenigsten offenen Flugbahnen in der Nähe der Medianebene der zweiten elektrostatischen Linse (73, 131 und 132) konfiguriert ist.
  11. Tomografische Atomsonde nach Anspruch 9, dadurch gekennzeichnet, dass die zweite elektrostatische Linse (73, 131 und 132) ein elektrisches Verzögerungsfeld erzeugt.
  12. Tomografische Atomsonde nach Anspruch 9, dadurch gekennzeichnet, dass die zweite elektrostatische Linse (73, 131 und 132) ein elektrisches Beschleunigungsfeld erzeugt.
  13. Tomografische Atomsonde nach Anspruch 1, dadurch gekennzeichnet, dass der Extraktor (71) einem Impulspotential ausgesetzt wird.
  14. Tomografische Atomsonde nach Anspruch 1, dadurch gekennzeichnet, dass die Ionen des Materials mit einem Impulslaser von der Probe (11) gelöst werden.
  15. Tomografische Atomsonde nach Anspruch 14, dadurch gekennzeichnet, dass der Extraktor (71) einem mit der Laseremission synchronisierten Impulspotential ausgesetzt wird.
EP08838185.0A 2007-10-12 2008-10-08 Hochauflösende weitwinkel-atomsonde Active EP2198449B1 (de)

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FR0707178A FR2922350B1 (fr) 2007-10-12 2007-10-12 Sonde tomographique grand angle a haute resolution.
PCT/EP2008/063462 WO2009047265A1 (fr) 2007-10-12 2008-10-08 Sonde tomographique grand angle a haute resolution

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FR2938963B1 (fr) * 2008-11-21 2010-11-12 Cameca Sonde atomique tomographique comportant un generateur electro-optique d'impulsions electriques haute tension.
JP6204367B2 (ja) * 2011-10-28 2017-09-27 レコ コーポレイションLeco Corporation 静電イオンミラー
DE112015006478T5 (de) * 2015-04-21 2018-01-04 Cameca Instruments, Inc. Atomsonde mit weitem Sichtfeld
US10614995B2 (en) 2016-06-27 2020-04-07 Cameca Instruments, Inc. Atom probe with vacuum differential
JP6788731B2 (ja) 2018-01-31 2020-11-25 カメカ インストゥルメンツ,インコーポレイテッド 複数の角度からの原子プローブ試料へのエネルギービーム入力
US11087956B2 (en) * 2018-06-29 2021-08-10 Taiwan Semiconductor Manufacturing Co., Ltd. Detection systems in semiconductor metrology tools

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WO2004111604A2 (en) * 2003-06-06 2004-12-23 Imago Scientific Instruments High resolution atom probe
JP4864501B2 (ja) * 2005-06-28 2012-02-01 富士通株式会社 3次元アトムレベル構造観察装置
US20070073364A1 (en) * 2005-09-29 2007-03-29 Siemens Aktiengesellschaft Combined OCT catheter device and method for combined optical coherence tomography (OCT) diagnosis and photodynamic therapy (PDT)

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FR2922350A1 (fr) 2009-04-17
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FR2922350B1 (fr) 2009-12-04
WO2009047265A1 (fr) 2009-04-16

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