WO2014034277A1 - Microscope électronique et procédé d'acquisition d'images de microscope électronique - Google Patents

Microscope électronique et procédé d'acquisition d'images de microscope électronique Download PDF

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Publication number
WO2014034277A1
WO2014034277A1 PCT/JP2013/068590 JP2013068590W WO2014034277A1 WO 2014034277 A1 WO2014034277 A1 WO 2014034277A1 JP 2013068590 W JP2013068590 W JP 2013068590W WO 2014034277 A1 WO2014034277 A1 WO 2014034277A1
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WIPO (PCT)
Prior art keywords
electron microscope
image
scanning transmission
microscope image
sample
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PCT/JP2013/068590
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English (en)
Japanese (ja)
Inventor
悠香 腰越
尚平 寺田
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株式会社 日立製作所
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Publication of WO2014034277A1 publication Critical patent/WO2014034277A1/fr

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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
    • H01J37/26—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
    • 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
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/05—Electron or ion-optical arrangements for separating electrons or ions according to their energy or mass
    • 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
    • H01J2237/244—Detection characterized by the detecting means
    • H01J2237/2449—Detector devices with moving charges in electric or magnetic fields

Definitions

  • the present invention relates to an electron microscope that obtains an enlarged image by irradiating a sample with an electron beam to detect electrons transmitted or scattered in the sample.
  • an electron microscope image acquisition condition calculation system and an electron microscope image acquisition condition adjustment method capable of adjusting an electron microscope image acquisition condition with high efficiency and high accuracy, and an electron microscope image acquisition condition adjustment method about.
  • the scanning transmission electron microscope converges and scans an electron beam accelerated at a high voltage on the sample, thereby detecting electrons transmitted or scattered from the sample by a detector and acquiring an electron microscope image.
  • enlargement, reduction, focus, astigmatism correction, and the like of the image are adjusted by a lens and a diaphragm in the microscope.
  • Cited Document 1 discloses a method of adjusting a multipole lens of an electron spectrometer having a plurality of multipole lenses attached to a transmission electron microscope, and parameter design using the excitation current of the multipole lens as a parameter.
  • a lens adjustment method for obtaining an optimum condition by simulation using a technique is disclosed.
  • Patent Document 1 discloses a lens adjustment method and a lens adjustment system for an electron spectrometer capable of adjusting an optimum condition of an electron spectrometer attached to a (scanning) transmission electron microscope with high efficiency and high accuracy.
  • a lens adjustment method and a lens adjustment system for an electron spectrometer capable of adjusting an optimum condition of an electron spectrometer attached to a (scanning) transmission electron microscope with high efficiency and high accuracy.
  • no consideration is given to the sample to be measured. Therefore, it is necessary to study to obtain optimum electron microscope image acquisition conditions with high efficiency and high accuracy according to the sample. Furthermore, it is desirable to improve the operability for determining the above acquisition conditions.
  • the present invention can search for the conditions at the time of acquiring an electron microscope image of the above-described conventional scanning transmission electron microscope with high efficiency and high accuracy, and adjust a lens, a diaphragm, etc. arranged in the scanning transmission electron microscope.
  • An electron microscope image acquisition condition adjustment method, an electron microscope image acquisition condition calculation system, and a sample film thickness condition calculation system are provided.
  • the present invention has the following configuration.
  • a scanning transmission electron microscope having a plurality of lenses, a diaphragm for limiting an electron beam, a detector, and acquiring an electron microscope image, an acquisition condition calculation system for calculating an acquisition condition of the electron microscope image, and the electron
  • a scanning transmission electron microscope comprising: a sample film thickness condition calculation system for calculating a sample film thickness in a line transmission direction.
  • the electron microscope image acquisition conditions ie, electron beam acceleration voltage, convergence angle, capture angle, probe current, detector, number of image capture pixels, image capture time or sample film thickness
  • the electron microscope image acquisition conditions ie, electron beam acceleration voltage, convergence angle, capture angle, probe current, detector, number of image capture pixels, image capture time or sample film thickness
  • FIG. 1 is a schematic view of a scanning transmission electron microscope according to one embodiment of the present invention.
  • the flowchart which showed the use procedure of the acquisition condition calculation system in this invention. Schematic which showed an example of the display content of the image display apparatus 12 in this invention.
  • Fig. 6 is a schematic diagram of the sample used for examining the optimum conditions.
  • the factor effect figure obtained by embodiment of this invention.
  • the electron microscope image obtained after optimizing the acquisition conditions of an electron microscope image by embodiment of this invention.
  • FIG. 3 is another schematic diagram of a scanning transmission electron microscope according to an embodiment of the present invention.
  • FIG. 3 is another schematic diagram of a scanning transmission electron microscope according to an embodiment of the present invention.
  • Scanning transmission electron microscopy is a technique for obtaining an enlarged image by converging an accelerated electron beam on a sample, scanning the sample two-dimensionally, and detecting electrons transmitted or scattered in the sample. Electrons that have passed through the sample are broadly divided into transmitted electrons that have lost energy and lost, elastically scattered electrons that are scattered without losing energy, and inelastically scattered electrons that are scattered with some energy lost. Depending on the method, there are differences in the scattering angle and scattering amount of electrons. In particular, the difference in the scattering angle of elastically scattered electrons depends on the atomic number. A sample with a large atomic number has a large scattering angle, and a sample with a small atomic number has a small scattering angle.
  • the amount of elastically scattered electrons depends on the sample density, and a sample with a high sample density has a large amount of scattered electrons and a sample with a low sample density has a small amount of scattered electrons.
  • image contrast is important in addition to spatial resolution.
  • the image contrast can be evaluated by the ratio of image intensity at each part of the sample. When there is no image contrast, it means that the image intensity ratio of each sample is 1. In addition, when the difference between the image intensity ratio and 1 is large, it is expressed as an optimum electron microscope image acquisition condition.
  • FIG. 1 is a schematic diagram of this embodiment.
  • the scanning transmission electron microscope with an electron spectrometer of the present embodiment includes a scanning transmission electron microscope 1, an electron beam spectrometer 11, an image display device 12, an electron microscope control device 15, an acquisition condition calculation system 13, and a sample film thickness calculation system 14. Etc.
  • the scanning transmission electron microscope 1 is provided with an electron source 2 that emits an electron beam 2, a converging lens 4, a spherical aberration corrector 5, a converging aperture 6, an objective lens 7, a projection lens 9, a detector 10, and the like.
  • a sample 8 is arranged between the projection lens 7 and the projection lens 9.
  • the configuration of the scanning transmission electron microscope 1 and the configuration of the electron spectrometer 8 are not limited to this.
  • the electron beam 3 emitted from the electron source 2 passes through the converging lens 4, the spherical aberration corrector 5, the converging diaphragm 6, and the objective lens 7 in the scanning transmission electron microscope, and irradiates the sample 8.
  • the electron beam 3 that has passed through the sample 8 passes through the projection lens 9 and is detected by the detector 10.
  • the detector 10 includes a bright field detector 51 that captures electrons having a small scattering angle and a dark field detector 52 that captures electrons having a large scattering angle.
  • the electron beam source 2, the converging lens 4, the converging diaphragm 6, the objective lens 7, the projection lens 9, and the detector 10 are controlled by the electron microscope control device 15.
  • the control content can be confirmed by the image display device. Further, the control content is appropriately stored in the electron microscope control device 15.
  • the electron beam 3 is caused to enter the electron spectrometer 11 attached immediately below the scanning transmission electron microscope.
  • an acquisition condition calculation system 13 and a sample film thickness calculation system 14 are used to acquire an electron microscope image acquisition condition of an electron beam acceleration voltage, convergence angle, capture angle, probe current, and detector.
  • a factorial effect diagram is created by simulation using a parameter design method with the number of image capture pixels, image capture time, or sample film thickness as parameters, and the electron microscope image acquisition conditions that optimize the image contrast using the factorial effect diagram Ask for.
  • the electron beam source 2, the focusing lens 4, the focusing diaphragm 6, the objective lens 7, the projection lens 9, and the detector 10 in the electron microscope 1 are adjusted according to the obtained acquisition conditions. Since the control contents are stored as appropriate, the previous control conditions can be used to adjust the conditions, and the simulation can be made more efficient and the results optimized.
  • FIG. 2 is a flowchart showing an example of the procedure for adjusting the electron microscope image acquisition condition, and shows the adjustment contents in the acquisition condition calculation system 13 and the sample film thickness calculation system 14 that optimize the image contrast.
  • FIG. 2 shows the contents of S103 to S112 implemented by the acquisition condition calculation system 13.
  • a sample is prepared by adjusting the sample film thickness in the electron beam transmission direction at an arbitrary position of the sample (S100).
  • at least three parameters for each condition in electron microscope image acquisition are input (S101).
  • the input parameter level may be the maximum value, the intermediate value, and the minimum value in the fluctuation region with respect to the electron microscope image acquisition conditions, or may be within a predetermined vertical range with respect to the set value at the time of installation of the apparatus good.
  • a lens or the like that has little influence on the adjustment of the electron beam acquisition conditions may be set with a fixed level at the time of device installation or device manufacture. In such a case, a plurality of parameters are fixed when the apparatus is installed, and parameters that are not fixed are adjusted during measurement.
  • the fixed parameter may be used for the simulation of the adjustment of the electron microscope image acquisition condition, the simulation is facilitated by deleting the fixed value from the parameter.
  • the number of simulations is one or more, and there is no limit on the number of simulations.
  • the number of simulations is large, it takes time to obtain the optimum conditions for the electron microscope image acquisition conditions. Therefore, it is desirable to confirm the current image contrast once before adjusting the parameters. By checking the image contrast before adjustment, the setting of the number of simulations can be changed according to the result, and the time until completion of necessary adjustment can be shortened.
  • the parameters of each electron microscope image acquisition condition are assigned to the orthogonal table in Taguchi method (S103, 104).
  • an L18 orthogonal table may be used, and when four or less parameters are used, an L9 orthogonal table may be used.
  • An electron microscope image is acquired under experimental conditions based on an orthogonal table. When acquiring the electron microscope image, the image may be acquired anywhere as long as the sample at the desired observation position is included.
  • the electron microscope image acquisition condition parameters are reset and the above procedure is performed again (S108 to 111).
  • the accuracy is improved if the range of the upper and lower limit values of the parameters is limited as compared with the previous simulation.
  • an optimal solution was obtained using only the acquisition conditions related to the electron microscope as a parameter, using a sample whose thickness was adjusted in advance.
  • the sample film thickness may also be set as a parameter as one of the acquisition conditions of the electron microscope image.
  • the sample film thickness for optimizing the image contrast can be calculated from the amount of transmitted electrons, the density of the sample, and the like measured in advance by the sample film thickness calculation system 14. Actual measurements are made with optimized sample thickness.
  • the sample 10 may have a wedge-shaped sample shape with a different film thickness in the transmission direction.
  • the sample film thickness is taken as a parameter by taking an electron microscope image at any time at a location with a different film thickness.
  • the calculation system 14 can be used to optimize electron microscope image acquisition conditions. In this case as well, actual measurement is performed at a position where an optimized sample film thickness is obtained.
  • FIG. 3 is a diagram showing an example of display contents in the image display device 12.
  • the selection button group 16 includes an electron microscope image acquisition condition calculation button 17 for starting adjustment of an electron microscope image acquisition condition, a position input button for inputting a location for reading the image intensity of the acquired electron microscope image of the sample, and image contrast.
  • a formula input button for inputting a formula (for example, a relative ratio of image intensities between two predetermined points) is included.
  • an electron microscope image display that displays the electron microscope image acquired by the detector 10 is displayed.
  • a plurality of image intensity reading points 19 indicating positions for reading the image intensity are displayed on the screen 18.
  • each electron microscope image acquisition condition is input as a parameter.
  • the input value can be selected as either a fixed value or a set value.
  • the parameters are assigned to the orthogonal table 23 in the Taguchi method.
  • the parameter input diagram 22 for the electron microscope image acquisition condition and the orthogonal table 23 are displayed every time the electron microscope image acquisition condition calculation button 17 for starting the adjustment of the electron microscope image acquisition condition is selected. do not have to.
  • the orthogonal table L9, L18 orthogonal table, or the like can be used depending on the number of conditions that need to be adjusted.
  • an electron microscope image display screen 18, an electron microscope image intensity reading point 19, an image contrast calculation expression input term 20, and a calculation result display function 21 are added.
  • An example of the procedure for calculating and displaying the image contrast of the electron microscope image is as follows. (1) An electron microscope image is displayed. (2) The position where the image intensity of the electron microscope image is acquired is determined, and the image intensity at each position is obtained. (3) An expression for calculating the image contrast is input. If registered in advance, select one from the registered expressions. (4) The image contrast is calculated from the image intensity at each position. This procedure is an example showing a method for calculating and displaying an image contrast, and the calculation method is not particularly limited to this. As for the image contrast, a position is determined in a vacuum portion other than on the sample, and the image contrast at each sample position can be calculated based on that point.
  • FIG. 4 is a diagram for explaining a parameter input diagram of electron microscope image acquisition conditions.
  • the leftmost column shows each electron beam acquisition condition (acceleration voltage, convergence angle, capture angle, probe current, detector, observation position, number of image capture pixels, and image capture time), and is necessary for adjustment. It is possible to increase or decrease according to various electron microscope image acquisition conditions.
  • the level number level 1 to 3 of each acquisition condition is written, and 2 or 3 levels are set for each condition. As described above, this level may be fixed at the time of installation of the apparatus or set for each adjustment before measurement.
  • FIG. 5 is a diagram for explaining a diagram showing an L18 orthogonal table in the present invention.
  • the numbers in FIG. 5 mean that the levels (levels 1 to 3) in FIG. 4 are input.
  • the L9 orthogonal table is used.
  • an electron microscope image acquisition condition calculation system and a sample film thickness condition calculation system are used to adjust eight electron beam acquisition conditions in the electron microscope, and based on the image intensity of a point in a vacuum. The image contrast at the two points on the sample was maximized.
  • Figure 6 shows a schematic diagram of the sample used for the examination of the optimum conditions.
  • amorphous carbon 32 and protective film 31 are deposited on highly oriented graphite 33. Both of the elements constituting the highly oriented graphite 33 and the amorphous carbon 32 are carbon.
  • the protective film 31 was deposited to protect the highly oriented graphite 33 and the amorphous carbon 32 from the ion beam when the focused ion beam apparatus was used to prepare a sample for a scanning transmission electron microscope.
  • the sample film thickness at the location where the electron microscope image was acquired was set to 50 to 150 nm, and the examination was made within the range where EELS was measurable.
  • FIG. 7 is an electron microscope image before adjustment.
  • This electron microscope image was observed by the bright field detector 52.
  • This time we use the L18 orthogonal table to adjust the 8 acquisition conditions (acceleration voltage, convergence angle, capture angle, probe current, detector, number of image capture pixels, image capture time, observation position) in the electron microscope 1 It was. The number of simulations was two.
  • Parameter Input for Electron Microscope Image Acquisition Conditions In FIG. 22, the levels of each acquisition condition are input so that the set values change from small to medium to large.
  • Fig. 8 shows the factor effect diagram obtained after the first simulation.
  • a second simulation was performed by allocating again to the L18 orthogonal table with ⁇ 10% of the set value of the level at which the S / N ratio was maximum for each parameter as the level.
  • FIG. 9 shows an electron microscope image after adjusting the acquisition conditions based on the electron microscope image acquisition conditions obtained from the optimum level of each output acquisition condition after the second simulation.
  • condition calculation button for operating the acquisition condition calculation system 13 is provided on the electron microscope image display screen, but it may be provided in another location.
  • control of the electron microscope image acquisition conditions for each measurement does not change the set value of the level, and when using a preset value, it is not necessary to input the set value of the level every time. There is little inconvenience even if no start button is provided on the apparatus.
  • the adjustment of the electron microscope image acquisition condition by the electron microscope can be performed with high efficiency and high accuracy. I can do it.
  • FIG. 10 is a schematic diagram showing another example of the scanning transmission electron microscope for optimizing the acquisition conditions of the scanning transmission electron microscope while processing the sample 8 as a thin piece.
  • the scanning transmission electron microscope 1 and the focused ion beam device 80 are connected in the vicinity of the sample chamber, and the sample 8 can freely move between both devices by a sample transfer system not shown in FIG. I can do it.
  • the focused ion beam device 80 includes an ion source 71, a focusing lens 72, a beam deflector 73, an objective lens 74, a probe 78, a secondary electron detector 77, a tungsten source 76, a focused ion beam device controller 79, and the like. Yes.
  • an ion beam 75 is generated from the ion source 71.
  • the irradiation position of the ion beam 75 on the sample 10 is designated by the beam deflector 73 and can be processed into a desired film thickness.
  • the ion beam 75 is irradiated from a direction perpendicular to the observation direction of the electron microscope image by the scanning transmission electron microscope 1, and the observation sample is thinned.
  • the electron microscope image can be observed while adjusting the sample film thickness as needed, so that the acquisition conditions can be optimized using the sample film thickness as a parameter.
  • FIG. 11 is a schematic view showing another example of the scanning transmission electron microscope for optimizing the acquisition conditions of the scanning transmission electron microscope while processing the sample 8 as a thin piece.
  • the scanning transmission electron microscope 1 and the focused ion beam device 80 are connected as in FIG.
  • acquisition conditions can be optimized using the sample film thickness as a parameter. For example, the sample is first processed into a wedge shape, and the optimum sample film thickness is obtained by the above-described method. Thereafter, processing is performed to obtain an optimum film pressure, and observation is performed after an observation sample is prepared.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

La présente invention vise à ajuster à un haut niveau d'efficacité et de précision des conditions optimales d'acquisition par un microscope électronique lors de l'acquisition, au moyen d'un microscope électronique à transmission par balayage, d'une image de microscope électronique d'un échantillon présentant un contraste élevé, configuré pour comporter des éléments d'éclairage. Le microscope électronique à transmission par balayage (1) qui acquiert une image de microscope électronique comprend : une pluralité de lentilles (4, 7, 9), un diaphragme (6) qui restreint un faisceau électronique ; un détecteur (10) ; un système de calcul des conditions d'acquisition (13) qui calcule les conditions d'acquisition de l'image de microscope électronique ; et un système de calcul des conditions d'épaisseur du film échantillon (14) qui calcule une épaisseur du film échantillon dans la direction de transmission du faisceau d'électrons.
PCT/JP2013/068590 2012-08-30 2013-07-08 Microscope électronique et procédé d'acquisition d'images de microscope électronique WO2014034277A1 (fr)

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JP2012189417A JP2014049214A (ja) 2012-08-30 2012-08-30 電子顕微鏡および電子顕微鏡像の取得方法
JP2012-189417 2012-08-30

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005108567A (ja) * 2003-09-29 2005-04-21 Hitachi High-Technologies Corp 電子顕微鏡による試料観察方法
JP2006127850A (ja) * 2004-10-27 2006-05-18 Hitachi High-Technologies Corp 荷電粒子ビーム装置及び試料作製方法
JP2006190567A (ja) * 2005-01-06 2006-07-20 Hitachi High-Technologies Corp 電子線装置
JP2007173132A (ja) * 2005-12-26 2007-07-05 Hitachi High-Technologies Corp 走査透過電子顕微鏡、および走査透過電子顕微鏡の調整方法
JP2009037738A (ja) * 2007-07-31 2009-02-19 Hitachi High-Technologies Corp 電子分光器を備えた電子顕微鏡

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005108567A (ja) * 2003-09-29 2005-04-21 Hitachi High-Technologies Corp 電子顕微鏡による試料観察方法
JP2006127850A (ja) * 2004-10-27 2006-05-18 Hitachi High-Technologies Corp 荷電粒子ビーム装置及び試料作製方法
JP2006190567A (ja) * 2005-01-06 2006-07-20 Hitachi High-Technologies Corp 電子線装置
JP2007173132A (ja) * 2005-12-26 2007-07-05 Hitachi High-Technologies Corp 走査透過電子顕微鏡、および走査透過電子顕微鏡の調整方法
JP2009037738A (ja) * 2007-07-31 2009-02-19 Hitachi High-Technologies Corp 電子分光器を備えた電子顕微鏡

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