WO2013111453A1 - 電子顕微鏡用試料ホルダ - Google Patents

電子顕微鏡用試料ホルダ Download PDF

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Publication number
WO2013111453A1
WO2013111453A1 PCT/JP2012/081231 JP2012081231W WO2013111453A1 WO 2013111453 A1 WO2013111453 A1 WO 2013111453A1 JP 2012081231 W JP2012081231 W JP 2012081231W WO 2013111453 A1 WO2013111453 A1 WO 2013111453A1
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WIPO (PCT)
Prior art keywords
sample
holder
electron microscope
transmission electron
sample holder
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.)
Ceased
Application number
PCT/JP2012/081231
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English (en)
French (fr)
Japanese (ja)
Inventor
尚平 寺田
佳史 谷口
康平 長久保
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.)
Hitachi High Tech Corp
Original Assignee
Hitachi High Technologies Corp
Hitachi High Tech Corp
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 Hitachi High Technologies Corp, Hitachi High Tech Corp filed Critical Hitachi High Technologies Corp
Priority to US14/371,032 priority Critical patent/US9558910B2/en
Priority to DE112012005295.1T priority patent/DE112012005295T5/de
Priority to CN201280067960.9A priority patent/CN104067368B/zh
Publication of WO2013111453A1 publication Critical patent/WO2013111453A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/2007—Holding mechanisms
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/201—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated for mounting multiple objects
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
    • H01J2237/202—Movement
    • H01J2237/20214—Rotation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26—Electron or ion microscopes
    • H01J2237/28—Scanning microscopes
    • H01J2237/2802—Transmission microscopes

Definitions

  • the present invention provides a plurality of TEMs in a focused ion beam in a sample holder for a transmission electron microscope in which a plurality of sample stands on which a sample is placed can be arranged and at least one of the sample stands can move in three axial directions. Sample processing is possible.
  • the electron energy loss spectrum includes zero loss spectrum that does not lose energy when passing through the sample, plasmon loss spectrum obtained by losing energy by exciting electrons in the valence band, and energy by exciting core electrons. It can be roughly divided into inner-shell electron excitation loss spectra obtained by loss of. In the inner shell electron excitation loss (core loss) spectrum, a fine structure is observed near the absorption edge.
  • This structure is called an absorption edge microstructure (ELNES) and has information reflecting the electronic state and chemical bonding state of the sample. Moreover, since the energy loss value (absorption edge position) is unique to the element, qualitative analysis is possible. Further, since information related to the coordination around the element of interest can be obtained from the shift of the absorption edge position called chemical shift, simple state analysis is also possible.
  • ELNES absorption edge microstructure
  • the electron energy loss spectrum's aberration and origin position change due to the drift of the acceleration voltage of the electron beam and the change of magnetic field / electric field due to the disturbance change around the device. It is difficult to compare the shape of the absorption edge fine structure of the spectrum and the slight chemical shift.
  • Patent Document 1 discloses that a transmission electron microscope image in which the focal positions of both the x-axis and the y-axis are the same plane is obtained in a normal transmission electron microscope, whereas electron transmission spectroscopy is performed in the transmission electron microscope described above.
  • the image detector obtains a two-dimensional image with the x-axis focal position as the spectral plane and the one y-axis focal position as the image plane by differentiating the focal positions of the x-axis and y-axis. It is described.
  • the electron energy loss spectrum in the y-axis direction of the sample can be separated and observed. That is, as shown in FIG. 2B, the image obtained by the image detector can be observed as a spectral image having the amount of energy loss, that is, the energy dispersion axis, and the y axis indicating the position information of the sample, as shown in FIG. .
  • the spectrum image is observed in a band shape corresponding to each laminated film of the transmission electron microscope image shown in FIG. 2A, when the intensity profile of the spectrum image is extracted at each location corresponding to each laminated film, as shown in FIG. 2C, the electron energy loss spectra at different positions of the sample are simultaneously obtained. It can be observed, and the absorption edge fine structure and slight chemical shift of the electron energy loss spectrum at different positions can be compared in detail.
  • the spectral image in which the x-axis described in Patent Document 1 has an energy loss amount and the y-axis has the position information of the sample changes the lens action of an electron spectrometer or the like, and the focal positions of the x-axis and the y-axis differ, It is a two-dimensional image obtained by an image detector, that is, it is possible to simultaneously observe electron energy loss spectra at a plurality of points at different positions on the sample.
  • a technique for acquiring a spectrum image that is, an electron energy loss spectrum from a plurality of different points in one sample and discussing a chemical shift due to a difference in a chemical bonding state is disclosed.
  • Patent Document 2 discloses a transmission electron microscope sample holder capable of simultaneously acquiring spectrum images from a plurality of samples and measuring an electron energy loss spectrum and a chemical shift.
  • the sample holder for a transmission electron microscope disclosed in Patent Document 2 has a sample stage on which a plurality of sample stands can be arranged. Further, at least one sample stage can be moved by a driving mechanism, and a plurality of sample stages can be brought close to each other.
  • Spectra images can be simultaneously acquired from a plurality of samples by the transmission electron microscope sample holder disclosed in Patent Document 2 described above, and an electron energy loss spectrum and chemical shift can be measured.
  • the holder for the above-described technique is provided with an opening for allowing an electron beam to pass through at the tip of the sample
  • a focused ion beam device used in the preparation of a TEM sample is used.
  • An opening for irradiating the sample with the ion beam is not provided in the apparatus, and a thin sample for TEM cannot be produced in the FIB using the holder of the above-described technique. For this reason, it is necessary to prepare a TEM sample by FIB using another sample holder, and then place it again on the above-described sample holder.
  • Patent Document 3 discloses a sample holder capable of TEM sample preparation and TEM observation by FIB.
  • An object of the present invention is that a plurality of sample stands can be arranged in a sample holder for an electron microscope, at least one sample stand can be moved, and a plurality of TEM sample processing can be performed in a focused ion beam apparatus.
  • a sample holder and a sample stage that can acquire a transmission electron microscope image, an electron diffraction image, a spectrum image, a scanning transmission electron microscope image, and the like with high spatial resolution from all the samples arranged in the sample holder. is there.
  • the sample holder for an electron microscope can be provided with a plurality of sample stands, a sample driving unit that moves the sample stand, a rotation mechanism that rotates the sample stand, and the tip of the sample holder
  • the part is provided with an opening.
  • a plurality of sample stands are arranged, at least one sample stand is movable, and sample processing for a plurality of transmission electron microscopes is enabled in a focused ion beam apparatus. It is possible to realize a sample holder and a sample stage that can acquire a transmission electron microscope image, an electron diffraction image, a spectrum image, a scanning transmission electron microscope image, and the like with high spatial resolution from all the samples arranged in the holder.
  • the mechanism may be uniaxial only, the weight of the rear end of the sample holder can be reduced, and sample drift can be reduced.
  • sample holder which is an Example of this invention, and is a schematic top view (a) and side view (b) at the time of observing a sample with a transmission electron microscope. It is explanatory drawing of the transmission electron microscope image obtained by a transmission electron microscope, a spectrum image, and an electron energy loss spectrum. It is the sample holder which is an Example of this invention, and is a schematic top view (a) and side view (b) at the time of processing a sample with a focused ion beam apparatus. It is the schematic top view (b) along the AA 'line shown to the schematic top view (a) and (a) which expanded the front-end
  • FIG. 6 is an explanatory diagram illustrating an example when an observation sample for a transmission electron microscope is manufactured with a focused ion beam apparatus using the sample stage of FIG. 5 in the present invention.
  • FIG. 6 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 5 in the present invention.
  • FIG. 6 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 5 in the present invention.
  • FIG. 6 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG.
  • FIG. 6 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 5 in the present invention.
  • FIG. 6 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 5 in the present invention.
  • FIG. 7 is an explanatory view showing an example when an observation sample for a transmission electron microscope is manufactured by a focused ion beam apparatus using the sample stage of FIG. 6 in the present invention.
  • FIG. 7 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 6 in the present invention.
  • FIG. 7 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 6 in the present invention.
  • 1 is a schematic configuration diagram of a transmission electron microscope to which one embodiment of the present invention is applied. The scanning ion microscope image acquired after fixing a sample piece to the sample stand within the focused ion beam apparatus using the sample holder of the present invention. A transmission electron microscope image obtained after a plurality of measurement samples are brought close to each other. Electron energy loss spectra obtained from multiple samples.
  • FIG. 15 is a schematic configuration diagram schematically showing a configuration of a transmission electron microscope apparatus according to an embodiment of the present invention. Note that the transmission electron microscope apparatus 101 includes an electron spectrometer 108.
  • the transmission electron microscope apparatus 101 of this embodiment includes an electron source 102 that emits an electron beam 103, a converging lens 104, an objective lens 106, an imaging lens system 107 (imaging lens), a fluorescent plate 109, and an electron spectrometer. 108, an image display device 114, a data storage device 115, and a central control device 116. Between the converging lens 104 and the objective lens 106, a transmission electron microscope sample holder (hereinafter referred to as a sample holder) 1 having a plurality of sample stands 13 and 14 is disposed. Samples are fixed to the sample stands 13 and 14.
  • the electron spectrometer 108 includes a magnetic field sector 110, multipole lenses 111 and 112, and an image detector 113.
  • the configuration of the transmission electron microscope apparatus 101 and the configuration of the electron spectrometer 108 are not limited to this. Further, the position where the electron spectrometer 108 is arranged is not particularly limited. In the present embodiment, the electron spectrometer 108 is disposed between the fluorescent plate 109 and the image display device 114, but the electron spectrometer 108 may be disposed between the imaging lens system 107.
  • the electron beam 103 emitted from the electron source 102 passes through the converging lens 104 and is irradiated onto the sample fixed to the sample stage 13 or 14.
  • the electron beam 103 that has passed through the sample passes through the objective lens 106 and a plurality of imaging lens systems 107, and when the fluorescent screen 109 is opened, the electron beam 103 enters the electron spectrometer 108 as it is.
  • the electron beam 103 that has entered the electron spectrometer 108 is a magnetic field sector that can be dispersed by the amount of energy of the multipole lenses 111 and 112 and the electron beam 103 used for reducing the aberration of the electron energy loss spectrum in the electron spectrometer 108.
  • the image is taken by the image detector 113 as a transmission electron microscope image, a two-dimensional element distribution image, a spectrum image, etc., then displayed on the image display device 114 and stored in the data storage device 115.
  • the magnetic field sector 110 and the multipole lenses 111 and 112 are controlled by the central controller 116. Further, the central control device 116 can control switching of acquisition modes of a transmission electron microscope image, a two-dimensional element distribution image, and a spectrum image.
  • the image detector 113 can also be arranged immediately below the fluorescent screen 109, and can acquire a transmission electron microscope image and an electron diffraction image before entering the electron spectrometer 108. When it is desired to pass the electron beam 103 through the electron spectrometer 108, the image detector 113 can be removed from the path of the electron beam 103.
  • a long field limiting slit 117 is inserted in the x-axis direction, that is, the same direction as the energy dispersion axis, and in the y-axis direction, that is, the sample measurement position direction Sometimes it is done.
  • the entire sample holder 1 can be moved in the transmission electron microscope 101 by the sample holder moving device 118. Further, the sample holder 1 has a coarse motion drive 7 that can move the sample over a wide range and a fine movement mechanism 119 for adjusting the position in order to bring the sample table closer to a desired position. The mechanism 119 can move the sample stage by the sample moving device 120.
  • the coarse movement mechanism 7 of the sample holder 1 is described on the assumption that the driving sample stage is manually moved, but can be moved by the sample moving device 120 in the same manner as the fine movement mechanism 119.
  • At least one of the sample bases 13 and 14 can be moved in the major axis direction of the sample holder 1 by the coarse motion drive 7 or the fine motion mechanism 119, and the electron energy loss spectrum of the sample fixed to the sample bases 13 and 14 is simultaneously acquired. It is moved from time to time so that you can.
  • the arrangement of the samples fixed to the sample tables 13 and 14 can be performed while confirming with the fluorescent screen 9 or the image display device 14.
  • FIG. 1 is a schematic top view (a) and side view (b) when the sample holder 1 shown in FIG. 15 is observed with a transmission electron microscope.
  • a holder tip opening 9 is provided at the tip of the sample holder 1.
  • a guide pin 2, a guide cover 3, and a guide pin hole 4 are provided in the center of the sample holder 1.
  • the guide pin 2 can be varied depending on the size of the casing of the transmission electron microscope 101. For example, when the acceleration voltage is 200 kV, the current guide pin position, and when the acceleration voltage is 300 kV, the guide pin hole 4 can be changed to the guide pin 2. Further, when the position of the guide pin 2 is changed, the guide cover 3 is also slid at the same time to firmly fix the guide pin 2.
  • the rear end of the sample holder 1 has a knob 5, a rotation mechanism 6, a coarse movement mechanism 7, and a connector 8.
  • the sample holder 1 has a two-layer structure, and is connected to the coarse movement mechanism 7 and the tip of the sample holder, and is connected to the coarse movement mechanism 7 and the coarse movement mechanism 7 as the rotation mechanism 6 rotates.
  • the tip of the spins With this rotating mechanism, it is possible to rotate the arrangement of the sample when observing with a transmission electron microscope and when preparing a sample for a transmission electron microscope with a focused ion beam device.
  • the coarse movement mechanism 7 is installed at the end of the sample holder 1 and is movable in the long axis direction of the sample holder 1.
  • the method for moving the sample stage by the coarse movement mechanism 7 is not limited to this.
  • the fine movement mechanism 119 is disposed inside the sample holder 1, and the connector 8 is used to connect the electric cable for operating the fine movement mechanism 119 and the sample fine movement control device 120.
  • the wired connection method is selected for the operation of the fine movement mechanism 119, but it is also possible to operate the fine movement mechanism 119 in a wireless manner.
  • the connector 8 is preferably disposed on the lower side with respect to the incident direction of the electron beam 103. As the rotation mechanism 6 rotates, the fine movement mechanism 119 disposed between the coarse movement mechanism 7 and the tip of the sample holder also rotates.
  • FIG. 3 is a schematic top view (a) and a side view (b) when the sample for the transmission electron microscope is processed with the focused ion beam device, which is the sample holder 1 shown in FIG.
  • FIG. 3 when processing a sample for a transmission electron microscope with a focused ion beam apparatus, the position where the holder tip opening 9 is orthogonal as compared with the tip when observed with the transmission electron microscope 101 of FIG. Placed in.
  • the incident direction of the electron beam and the incident direction of the ion beam are orthogonal, but the rotation of the tip of the sample holder 1 is not limited to this.
  • FIG. 4 is a schematic top view (a) in which the tip of the sample holder according to the embodiment of the present invention is enlarged, and a schematic cross-sectional view (b) along the line AA ′ shown in (a).
  • the holder tip opening 9 is provided at the tip of the sample holder 1 as described above.
  • the sample stage 18 is a stage for installing the sample stage 13 and is disposed in the sample holder 1.
  • the sample stage 13 is fixed to the sample stage 18 by a holding screw 12 through the sample stage holding plate 11.
  • the sample stage 14 is fixed to the driving sample stage 15.
  • the fixing method is that the sample is fixed to the driving sample stage 15 by the holding screw 16 via the sample table holding plate 17.
  • the method for fixing each sample stage to the sample stage is not limited to this, and for example, fixing by a pressing spring or fixing with an adhesive tape is also conceivable.
  • the sample table 14 is independently moved in the three axis directions of X, Y, and Z by the coarse movement mechanism 7 and the fine movement mechanism 119. Can be moved.
  • the coarse movement mechanism 7 is only in the long axis direction of the sample holder 1, but the fine movement mechanism 119 is movable in three axis directions.
  • two sample stands are arranged in the sample holder 1, and the method of moving one of the sample stands has been described. However, there is no particular problem even if two or more sample stands are arranged on the sample holder 1 and moved. .
  • height adjusting screws 19 and 20 are provided in the sample stage 18 and the driving sample stage 15.
  • the height of the sample stands 13 and 14 is adjusted by the height adjusting screws 19 and 20.
  • the height adjusting screws 19 and 20 enable the coarse movement mechanism 7 to be driven only in the long axis direction, and it is possible to make a structure that is sufficient if the fine movement mechanism 119 is driven in the three axis directions. If the coarse motion mechanism 7 itself is driven in three axial directions, the drive mechanism itself becomes large, and the side entry type transmission electron microscope is susceptible to vibration. Further, since it is difficult to adjust the triaxial direction with the coarse movement mechanism 7 itself, the fine movement mechanism 119 can be moved in the triaxial direction only in the long axis direction of the sample holder 1 as in this embodiment. It is easier to adjust.
  • FIG. 5 is an explanatory view showing an example of a sample stage for setting a sample in the present invention.
  • a holding screw opening 31 is provided for allowing the holding screws 12 and 16 used for fixing to the sample stage 18 and the driving sample stage 15 to pass.
  • Sample fixing points 32, 33, and 34 are also provided to fix the sample pieces extracted in the focused ion beam apparatus. There is no problem even if the sample piece extracted in the focused ion beam apparatus is fixed at any position according to the method for measuring the electron energy loss spectrum described later. Moreover, it is also possible to fix a sample piece to all the places simultaneously.
  • FIG. 6 is an explanatory view showing another example of a sample stage for installing a sample in the present invention. Similar to the description in FIG. 5, a holding screw opening 31 is provided for allowing the holding screws 12 and 16 used when being fixed to the sample stages 12 and 18 to pass therethrough. Further, the sample piece extracted in the focused ion beam apparatus is fixed to the sample fixing portion 32.
  • the shape of the sample stage is not limited to this.
  • the sample stage when the sample stage is fixed to the sample stage, it is fixed without using a holding screw. In doing so, the holding screw opening 32 is not required.
  • the sample stage of this embodiment since the sample mounting position is near the center of the sample stage, there is an advantage that the sample position does not change even if the direction of the sample stage is changed.
  • FIG. 7 is an explanatory diagram showing an example when an observation sample for a transmission electron microscope is manufactured with a focused ion beam apparatus using the sample stage of FIG.
  • FIG. 7A is a diagram projected from the direction perpendicular to the incident direction of the ion beam
  • FIG. 7B is a diagram projected from the direction parallel to the incident direction of the ion beam. It is explanatory drawing at the time of fixing the sample pieces 48 and 49 to the sample fixing
  • the sample pieces 48 and 49 may be fixed to the sample bases 41 and 42 from either side, and after fixing the sample piece on one side, the other sample piece can be fixed.
  • the arrangement can be set with high accuracy in advance.
  • Sample pieces 48 and 49 fixed to the sample tables 41 and 42 are irradiated with an ion beam from the protective film side on which carbon, tungsten, aluminum, platinum, gold or the like is deposited, and are observed with a transmission electron microscope or an electron energy loss spectrum.
  • the sample is thinned to the thickness of the sample that can be measured.
  • the sample holder tip opening 9 provided at the tip of the sample holder 1 by the rotating mechanism 6 of the sample holder 1 is arranged on the incident direction side of the ion beam. That is, the ion beam image observed when the slice is formed is as shown in FIG. 7B, and the cross-sectional direction of the sample tables 41 and 42 is observed.
  • FIG. 8 is an explanatory view showing the arrangement of a sample when acquiring a spectral image by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. Is rotated by the rotating mechanism 6 and set for observation with a transmission electron microscope, and then inserted into the transmission electron microscope.
  • the rotation mechanism 6 can also rotate the transmission electron microscope.
  • the sample stage 41 is fixed to the sample stage 18, and the sample stage 42 is fixed to the driving sample stage 15.
  • the sample piece 42 is moved by the coarse movement mechanism 7 and the fine movement mechanism 119.
  • the distance between 48 and 49 can be approached.
  • the sample pieces 48 and 49 are constituted by the protective films 43 and 44 and the measurement samples 45 and 46 as described above.
  • FIG. 9 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. Shows the arrangement of the sample pieces 48 and 49 when projected onto the fluorescent screen 109 in parallel with the energy dispersion axis of the electron spectrometer 108.
  • an electron energy loss spectrum can be acquired by restricting the measurement region 47 of the spectrum by the restriction visual field slit 117.
  • FIG. 10 is another explanatory view showing the arrangement of the sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. The arrangement of the sample pieces 48 and 49 when the axial direction is projected onto the fluorescent screen 109 in parallel with the energy dispersion axis of the electron spectrometer 108 is shown.
  • the sample pieces 48 and 49 can be approached without removing the sample stage 41 or the sample stage 42, but the measurement sample 46 measures a place away from the protective film 44.
  • the sample thickness may not be thin enough to measure the electron energy loss spectrum.
  • FIG. 11 is another explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. The arrangement of the sample pieces 48 and 49 when the axial direction is projected onto the fluorescent screen 109 in parallel with the energy dispersion axis of the electron spectrometer 108 is shown.
  • the side surfaces of the sample pieces 48 and 49 are fixed to the sample bases 41 and 42, but when it is desired to fix the sample pieces firmly, the sample pieces are attached to the sample fixing points 33. After fixing and reversing one side of the sample stage, the sample pieces 48 and 49 may be brought close to each other.
  • FIG. 12 is an explanatory diagram showing an example when an observation sample for a transmission electron microscope is produced with a focused ion beam apparatus using the sample stage of FIG. 6 in the present invention.
  • 12A is a diagram projected from a direction perpendicular to the ion beam incident direction
  • FIG. 12B is a diagram projected from a direction parallel to the ion beam incident direction. It is explanatory drawing at the time of fixing the sample pieces 48 and 49 to the sample fixing
  • the sample pieces 48 and 49 may be fixed to the sample stages 41 and 42 from either side, and after the sample piece is fixed to one side, the other sample piece is fixed. Therefore, the arrangement between the two samples can be set with high accuracy in advance.
  • sample pieces 48 and 49 fixed to the sample tables 41 and 42 are irradiated with an ion beam from the protective film side on which carbon, tungsten, aluminum, platinum, gold, etc. are deposited, and are used in the transmission electron microscope.
  • the sample is thinned to a thickness that allows observation and measurement of an electron energy loss spectrum.
  • the sample holder tip opening 9 provided at the tip of the sample holder 1 by the rotating mechanism 6 of the sample holder 1 is arranged on the incident direction side of the ion beam. That is, the ion beam image observed when the slice is formed is as shown in FIG. 12B, and the cross-sectional direction of the sample tables 41 and 42 is observed.
  • FIG. 13 is an explanatory view showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. 6 in the present invention. After being rotated by the rotation mechanism 6 and set for observation with a transmission electron microscope, it is inserted into the transmission electron microscope.
  • the sample stage 41 is fixed to the sample stage 18, and the sample stage 42 is fixed to the driving sample stage 15.
  • the sample piece 42 is driven by the coarse movement mechanism 7 and the fine movement mechanism 119.
  • the distance between 48 and 49 can be approached.
  • the sample pieces 48 and 49 are constituted by the protective films 43 and 44 and the measurement samples 45 and 46 as described above.
  • FIG. 14 is another explanatory diagram showing the arrangement of a sample when a spectral image is acquired by a transmission electron microscope equipped with an electron spectrometer using the sample stage of FIG. The arrangement of the sample pieces 48 and 49 when the axial direction is projected onto the fluorescent screen 109 in parallel with the energy dispersion axis of the electron spectrometer 108 is shown.
  • an electron energy loss spectrum can be acquired by restricting the measurement region 47 of the spectrum by the restriction visual field slit 117.
  • the specific example which acquired the spectral image of the some sample simultaneously using the sample holder 1 mentioned above is shown.
  • the transmission electron microscope 101 was used, spectrum images were simultaneously obtained from two samples, and chemical shifts of electron energy loss spectra obtained from the spectrum images were measured.
  • the measurement samples were dimanganese trioxide (Mn 2 O 3 ) particles (measurement sample A) and manganese oxide (MnO) particles (measurement sample B).
  • the measurement sample was fixed on a sample stage in a focused ion beam apparatus after each powder particle was filled with resin.
  • the sample table 41 on which the sample piece 48 including the measurement sample A45 is fixed is placed on the tip side of the sample holder, that is, the sample stage 18, and the sample table 42 on which the sample piece 49 including the measurement sample B46 is fixed is sample driven. It was installed on the driving sample stage 15 connected to the working rod 21.
  • FIG. 16 is a scanning ion microscope image acquired after fixing the sample piece 49 to the sample stage 42 installed on the driving sample stage 15 in the focused ion beam apparatus using the sample holder 1 of the present invention. The sample was observed from the cross-sectional direction. From FIG. 16, it is meant that the sample piece can be fixed and thinned in the focused ion beam apparatus using the sample holder 1.
  • the tip of the sample holder 1 is set at the sample position for observation with a transmission electron microscope, pulled out from the focused ion beam device, and then transmitted. It was inserted into an electron microscope and a spectrum image was acquired.
  • the acceleration voltage of the transmission electron microscope 101 at the time of spectrum image acquisition was 200 kV
  • the take-in angle of the electron beam 3 was 6 mrad
  • the energy dispersion was 0.05 eV / pixel.
  • the image detector 113 used for acquiring the spectral image is a 1024 pixel ⁇ 1024 pixel two-dimensional detector.
  • the observation magnification of the transmission electron microscope 101 was set to 200 times, and the measurement sample B46 was moved using the coarse movement mechanism 7 so as to be as close to the measurement sample A45 as possible.
  • the positions of both were confirmed by using the image on the fluorescent screen 109 and moved so that the samples of both were placed in the central portion of the fluorescent screen 109 as much as possible.
  • the observation magnification on the display in the transmission electron microscope 1 was changed to 10,000 times, and the measurement sample B46 was moved so that the measurement sample A45 and the measurement sample B46 were orthogonal to the energy dispersion axis of the electron spectrometer 8. After that, the measurement sample B46 was further moved closer by the sample movement control device 120 so that the spectrum images of the measurement sample A45 and the measurement sample B46 can be acquired simultaneously. At this time, the positions of both were confirmed using a transmission electron microscope image obtained by the image detector 113.
  • FIG. 17 is a transmission electron microscope image acquired after the measurement sample A45 and the measurement sample B46 are brought close to each other.
  • the measurement sample A45 and the measurement sample B46 are approaching at an interval of about 20 nm. Further, it was found that both samples are located in the spectrum acquisition region 47, and a spectrum image can be acquired simultaneously from both samples. Moreover, since each sample is clear from the transmission electron microscope image in FIG. 17, it means that the sample drift is satisfactory for observing the transmission electron microscope image.
  • the observation magnification was set to 50000 times, and spectral images of the measurement sample A45 and the measurement sample B46 were simultaneously obtained.
  • the spectrum image was acquired in the L shell absorption edge region of manganese, and the electron energy loss spectrum was extracted from each sample in the spectrum image obtained from the L shell absorption edge region of manganese.
  • FIG. 18 shows electron energy loss spectra obtained from both samples. As a result of measuring the chemical shift between the two samples, it was found that dimanganese trioxide was shifted to about 1.6 eV higher loss energy side than manganese oxide.
  • this technology has made it possible to use a single sample holder from the preparation of a transmission electron microscope to the observation.
  • the present invention is not limited to the above-described embodiment.
  • electron diffraction, length measurement, and further It can be applied to aberration correction of a transmission electron microscope with spherical aberration correction (scanning).
  • the sample can be moved from the focused ion beam device to the transmission electron microscope without being exposed to the atmosphere.
  • voltage application measurement is also possible by placing a tungsten wire or the like with a sharpened tip without contacting a sample stage on the driving sample stage and contacting the sample placed on the sample stage.
  • the mechanical properties of the sample can be measured by adjusting the way in which the tungsten wire is pushed.
  • the arrangement of the sample stage and the tungsten wire is not limited to this.
  • a focused ion beam apparatus is combined with a transmission electron microscope or a scanning electron microscope
  • a plurality of ion beams are made incident from a holder tip opening 9 of a sample holder 1 on which a plurality of sample stands are installed.
  • a transmission image and an elemental analysis result can be obtained while thinning a sample fixed to each sample stage.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Sampling And Sample Adjustment (AREA)
PCT/JP2012/081231 2012-01-25 2012-12-03 電子顕微鏡用試料ホルダ Ceased WO2013111453A1 (ja)

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US14/371,032 US9558910B2 (en) 2012-01-25 2012-12-03 Sample holder for electron microscope
DE112012005295.1T DE112012005295T5 (de) 2012-01-25 2012-12-03 Probenhalter für Elektronenmikroskop
CN201280067960.9A CN104067368B (zh) 2012-01-25 2012-12-03 电子显微镜用试样支架

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CN114137010B (zh) * 2021-11-05 2024-02-13 上海交通大学 一种高温合金微量元素分布状态的测定方法

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CN104067368B (zh) 2016-08-24
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US9558910B2 (en) 2017-01-31
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