WO2016006375A1 - 電子顕微鏡、及び、試料の観察方法 - Google Patents
電子顕微鏡、及び、試料の観察方法 Download PDFInfo
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- WO2016006375A1 WO2016006375A1 PCT/JP2015/066424 JP2015066424W WO2016006375A1 WO 2016006375 A1 WO2016006375 A1 WO 2016006375A1 JP 2015066424 W JP2015066424 W JP 2015066424W WO 2016006375 A1 WO2016006375 A1 WO 2016006375A1
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000010894 electron beam technology Methods 0.000 claims description 75
- 230000000007 visual effect Effects 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims 3
- 238000002003 electron diffraction Methods 0.000 claims 2
- 239000013078 crystal Substances 0.000 abstract description 65
- 238000002524 electron diffraction data Methods 0.000 abstract description 24
- 230000007246 mechanism Effects 0.000 description 28
- 239000003550 marker Substances 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 11
- 239000000758 substrate Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 238000004364 calculation method Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000010191 image analysis Methods 0.000 description 3
- 238000012886 linear function Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000013079 quasicrystal Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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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
- H01J37/22—Optical or photographic arrangements associated with the tube
-
- 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 objects 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
- H01J37/02—Details
- H01J37/244—Detectors; Associated components or circuits therefor
-
- 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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/295—Electron or ion diffraction tubes
-
- 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
- H01J2237/20207—Tilt
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- 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 relates to an electron microscope, and more particularly to a transmission electron microscope capable of forming, observing, and recording a scanning and transmission electron image and an electron beam diffraction pattern.
- An electron diffraction pattern is used to align the crystal orientation of the sample with a transmission electron microscope.
- aligning the electron beam incident direction and the crystal axis direction it is possible to acquire atomic arrangement information and identify a crystal.
- the grain boundary width and the like can be accurately grasped by making the crystal grain boundary and the electron beam axis parallel.
- the crystal orientation of the Si substrate is aligned so that the electron beam is incident parallel to the substrate surface. The sample is tilted.
- Such crystal orientation adjustment is an indispensable technique when using a crystalline sample, but requires skill to accurately align the crystal orientation while observing an electron beam diffraction pattern.
- the crystalline sample is a sample in which part or all of the sample has a regular arrangement.
- a single crystal a polycrystal that is a composite of a plurality of microcrystals, and a quasicrystal.
- some of the crystalline sample also includes a compound consisting of a single element or a plurality of elements.
- Patent Document 1 with respect to crystal orientation alignment, electron diffraction pattern data acquired for each tilt angle of the sample is stored in advance, and spot distribution of the electron diffraction pattern is fitted with a circle based on the stored data.
- the sample is automatically tilted so that the radius of is minimized.
- the locus of the center coordinates of the approximate circle obtained is approximated by a linear function, and the intersection point on the linear function line where the linear function straight line and the direct spot central coordinate are the shortest distance.
- the sample inclination angle that can be taken is determined as the optimum inclination angle.
- Patent Document 1 it is necessary to store data of electron diffraction patterns corresponding to a plurality of different sample tilt angles in advance, and a crystallographic axis (a group of planes called crystallographic bands is formed). Since it takes a lot of time to obtain a single crystal axis to be shared, the throughput decreases.
- the present invention provides an apparatus and a method capable of observing a sample with a high throughput and a high-precision crystal orientation, regardless of the type of the sample and the crystal orientation, even if it is not an expert. Objective.
- the present invention in the alignment of the crystal orientation of the sample, superposition is performed so that the main spot is located on the circumference based on the luminance distribution of the diffraction spot in the electron diffraction pattern.
- the operation of the sample stage is controlled based on the direction and size of the displayed vector.
- FIG. 1 is a basic configuration diagram of an electron microscope according to the present embodiment.
- the flowchart which shows the procedure of the crystal orientation alignment which concerns on 1st Embodiment.
- the figure explaining the technique of the crystal orientation alignment which concerns on 3rd Embodiment The figure which shows an example of the transmission electron image before and behind crystal orientation alignment, and an electron beam diffraction pattern.
- the figure explaining the technique of the crystal orientation alignment which concerns on 4th Embodiment The figure explaining the main structures of the main-body control part relevant to the crystal orientation adjustment process which concerns on this Embodiment.
- FIG. 1 shows a basic configuration of an electron microscope 1 according to the present embodiment.
- the body of the electron microscope 1 is mainly composed of an electron gun 2, a condenser lens 3, an objective lens 4, an intermediate lens 5 and a projection lens 6.
- the sample 8 is mounted on the sample holder 7, and the sample holder 7 is introduced into the inside from a sample stage 32 provided on the side surface of the body of the electron microscope 1.
- the movement and inclination of the sample 8 are controlled by the sample fine movement drive mechanism 9 connected to the sample stage 32.
- a converging movable diaphragm 16 for converging the electron beam 15 irradiating the sample 8 is disposed above the objective lens 4.
- a diffraction pattern is formed on the rear focal plane of the objective lens 4, and an objective movable diaphragm 17 is provided on the same plane, and a limited field stop 18 is provided on the image plane.
- Each movable diaphragm is connected to the diaphragm drive control unit 19 and can move in the horizontal direction, and its operation is controlled by the diaphragm drive control unit 19 so as to be put in and out on the optical axis in accordance with the observation target.
- a fluorescent plate 10 is disposed below the projection lens 6, and a camera 11 is mounted under the fluorescent plate 10.
- the camera 11 is connected to the monitor 13 and the image analysis device 14 via the camera control unit 12.
- Each lens of the condenser lens 3, the objective lens 4, the intermediate lens 5, and the projection lens 6 is connected to a lens power source 20.
- the electron beam 15 emitted from the electron gun 2 is converged by the condenser lens 3 and the converging movable diaphragm 16 and irradiated onto the sample 8.
- the electron beam 15 transmitted through the sample 8 is imaged by the objective lens 4, and the image is magnified by the intermediate lens 5 and the projection lens 6 and projected onto the fluorescent plate 10.
- the image is projected on the camera 11, and a transmission image or an electron beam diffraction pattern 22 is displayed on the monitor 13 and recorded in the image analysis device 14.
- the main body control unit 21 is connected to the sample fine movement drive mechanism 9, the camera control unit 12, the aperture drive control unit 19, and the lens power source 20, and transmits / receives control signals for controlling the entire apparatus.
- the sample fine movement driving mechanism 9 includes a sample moving mechanism 9 a that moves the sample 8 and a sample tilt mechanism 9 b that tilts the sample 8.
- the configuration of the control system shown in FIG. 1 is merely an example, and modifications such as a control unit and wiring for communication are included in the category of the electron microscope of the present embodiment as long as the functions intended by the present embodiment are satisfied. It is.
- the main body control unit 21 is connected to each component unit to control the entire apparatus, but may be configured to include an independent control unit for each component unit.
- FIG. 11 is a diagram for explaining the components related to the crystal orientation alignment according to the present embodiment to be described later, among the components included in the main body control unit 21.
- Constituent units related to crystal orientation alignment are mainly a main spot setting unit 34, a pattern setting unit 35, a vector setting unit 36, a vector information acquisition unit, a calculation unit 38, a sample fine movement mechanism instruction unit 39, and an observation mode switching unit 40.
- the main body control unit 21 includes various components in addition to the above-described components.
- the main spot setting unit 34 sets the position of the main spot 23 in the electron diffraction pattern 22 projected on the fluorescent plate 10 or the camera 11 described later.
- a marker 25 is displayed at the set position of the main spot 23.
- the setting of the main spot 23 can be selected by an operator, or can be automatically determined by the apparatus as will be described later.
- the pattern setting unit 35 sets the circular pattern 26 or the arc-shaped pattern 33 so that the main spot 23 of the electron beam diffraction pattern 22b is located on the circumference.
- the pattern setting unit 35 can change the shape and size of the circular pattern 26 or the arc-shaped pattern 33 set based on the luminance distribution of the electron beam diffraction pattern 22b.
- the vector setting unit 36 uses a center point (or a virtual coordinate point of the center point), which will be described later, as a starting point and a vector having the position of the main spot 23 as the origin. Set V.
- the vector information acquisition unit 37 acquires information on the direction and size of the set vector V, and determines the tilt direction and tilt angle of the sample 8 based on this information.
- the sample fine movement drive mechanism instructing unit 39 controls the operation of the sample inclination mechanism 9b of the sample fine movement drive mechanism 9 based on the inclination direction and the inclination angle of the sample 8 obtained by the calculation unit 38.
- the observation mode switching unit 40 can change the observation mode of the electron microscope 1 between an image observation mode and an observation mode of the electron beam diffraction pattern 22.
- FIG. 2 shows an optical path diagram of the transmission electron microscope 1 during observation of the electron beam diffraction pattern 22 according to the present embodiment. Although this figure shows a state in which the fluorescent plate 10 is moved so as to deviate from the optical axis, the fluorescent plate 10 may be arranged on the upper part of the camera 11. The electron beam 15 is applied to the sample 8 in parallel.
- the electron beam 15 includes an electron beam 15a that travels straight without being diffracted by the crystal and an electron beam 15b that undergoes diffraction, and the electron beam 15b diffracted at the same angle is the objective lens. 4 gather at one point on the back focal plane, and form an electron beam diffraction pattern 22a on the back focal plane.
- the electron beam 15 on which these electron beam diffraction patterns 22a are formed further forms an image on the image plane of the objective lens 4.
- a limited field stop 18 is disposed on the image plane, and an area in which the image of the electron beam diffraction pattern 22 is observed is adjusted by the opening angle of the limited field stop 18.
- the focus of the intermediate lens 5 is focused on the electron beam diffraction pattern 22a formed at the back focal point of the objective lens 4, and enlarged by the intermediate lens 5 and the projection lens 6, and the fluorescent plate 10 Or it projects on the camera 11 and the electron beam diffraction pattern 22b after projection is obtained.
- the intermediate lens 5 is focused on the image formed on the image plane, magnified by the intermediate lens 5 and the projection lens 6, and projected onto the fluorescent screen 10 or the camera 11.
- the entire field of view is observed by extracting the limited field stop 18 from the mirror body. Further, by arranging the limited field stop 18 in the lens body and adjusting the opening angle, the electron beam diffraction pattern 22a formed in the field of view corresponding to the opening angle in the sample 8 is observed.
- FIG. 3 shows the relationship among the crystalline sample 8, the electron beam 15, and the electron diffraction pattern 22a according to the present embodiment.
- (A) is a state in which the electron beam 15 is incident in parallel to the crystal axis 8a of the crystal plane of the sample 8, and (b) is an angle ⁇ with respect to the crystal axis 8a of the crystal plane of the sample 8 from the crystal zone axis.
- the electron beam 15 is incident.
- the state in which the electron beam 15 is incident in parallel to the crystal axis 8a of the crystal plane of the sample 8 in (a) is referred to as a state in which the zone axis is incident. From FIG.
- FIG. 3B shows a case in which the sample 8 is inclined by an angle of ⁇ , and as shown in the figure, the electron beam 15 is incident in parallel to the crystal axis 8a, that is, the zone axis is incident. It can be seen that it is necessary to incline the sample 8 by the angle ⁇ in order to achieve this.
- FIG. 9 is a diagram showing an example of a transmission electron image before and after crystal orientation alignment and an electron beam diffraction pattern.
- (A), (c) shows the transmission electron image which expanded a part of structure of Si device, (b), (d) is the crystal orientation of Si substrate 29 of (a), (c), respectively.
- the corresponding electron beam diffraction pattern 22b is shown. From the result of the electron beam diffraction pattern 22b shown in (b), it can be seen that in (a), the electron beam 15 is incident with a deviation from the crystal axis of the Si substrate 29.
- the condition of the zone axis incidence capable of acquiring the transmission electron image shown in (c) can be easily obtained, so that the material structure can be measured quickly and accurately. .
- FIG. 4 is a diagram for explaining a method of crystal orientation alignment processing according to the first embodiment.
- the electron diffraction pattern 22 is displayed on the monitor 13.
- the marker 25 is displayed (a )
- This position is set to the origin 0 (0, 0)
- X, Y orthogonal coordinates in accordance with the inclination directions ⁇ , ⁇ of the sample 8 are acquired (b).
- X, Y orthogonal coordinates are displayed is shown, but actually, the acquired X, Y orthogonal coordinates can be stored and the processing can be advanced without being displayed on the monitor 13.
- the sample stage 32 is once moved to a place where the sample 8 does not exist, the position information of the shining spot is stored, and then the sample 8 after projection onto the fluorescent screen 10 or the camera 11 is stored.
- the sample stage 32 is moved so as to display the upper electron beam diffraction pattern 22b, and a position that coincides with the spot stored in advance can be determined as the main spot. In this way, the position of the main spot 23 can be correctly selected even when there are diffraction spots having similar intensities at adjacent positions.
- the position of the main spot 23 stored in advance by the above method is automatically selected according to an instruction from the main body control unit 21. You can also
- the circular pattern 26 is displayed so that the main spot 23 of the electron diffraction pattern 22b is positioned on the circumference (step 606).
- the operator can adjust the size of the circular pattern 26 according to the luminance distribution of the electron beam diffraction pattern 22b.
- the second marker 27 is displayed at the center of the circular pattern 26, and the coordinates P (x, y) of the position of the second marker 27 on the X, Y orthogonal coordinates are stored. Until the vector 28 is displayed (d).
- Information on the position of the coordinates on the X, Y orthogonal coordinates of 0 (0, 0) and P (x, y) and the size and direction information of the vector 28 are the vector information acquisition unit of the main body control unit 21. 37.
- the calculation unit 38 of the main body control unit 21 determines the inclination direction of the sample 8 from the direction of the vector 28, and the magnitude R of the vector 28, that is, the ⁇ coordinate difference x. , And the difference y of the ⁇ coordinates, the inclination angle of the sample 8 on the ⁇ and ⁇ axes can be obtained from the equation (1).
- the main body control unit 21 controls the sample tilt mechanism 9b of the sample fine movement drive mechanism 9 to tilt the sample 8.
- the electron beam 15 enters the zone axis. Further, by switching to the image observation mode when the sample 8 is tilted, the size of the field of view limited by the limited field stop 18 can be confirmed. Even when the visual field shift occurs due to the inclination of the sample 8, the operator manually adjusts the sample fine movement by operating the sample moving mechanism 9a of the sample fine movement driving mechanism 9 manually or by the main body control unit 21. It is possible to prevent the visual field from being lost when the sample 8 is tilted.
- the reproducibility and accuracy of the sample stage May not be adjusted to the actual position of the sample 8, but as described above, by correcting the visual field movement in real time at the time of image observation in the image observation mode, it is possible to reliably correct the positional deviation.
- FIG. 5 is a graph showing X, Y orthogonal coordinates used for obtaining the tilt direction and tilt angle of the sample 8 according to the present embodiment.
- the horizontal axis is the X axis corresponding to the ⁇ axis of the sample tilt axis
- the vertical axis is the Y axis corresponding to the ⁇ axis of the sample tilt axis
- the position of the main spot 23 of the electron beam diffraction pattern 22 is the origin 0 (0, 0).
- the center point of the circular pattern 26 superimposed and displayed in accordance with the luminance distribution of the electron beam diffraction pattern 22 is defined as P (x, y).
- the inclination angle and direction of the sample 8 are obtained.
- FIG. 6 is a flowchart showing an operation procedure for crystal orientation alignment according to the first embodiment.
- the magnification is set (step 601). At this time, it is desirable to set the magnification to an appropriate magnification or less in order to easily follow even if the visual field moves when the sample 8 is tilted.
- the visual field on the sample 8 for crystal orientation alignment is determined using the sample moving mechanism 9a and the sample tilting mechanism 9b of the sample fine movement driving mechanism 9 (step 602).
- the limited field stop 18 is inserted into the sample 8 to be crystal orientation aligned using the stop drive mechanism 19 (step 603).
- the observation mode of the electron diffraction pattern 22 is set to ON (step 604).
- the focus of the intermediate lens 5 is focused on the electron beam diffraction pattern 22a formed at the back focal point of the objective lens 4, the electron beam diffraction pattern 22 is enlarged by the intermediate lens 5 and the projection lens 6, and the fluorescent plate 10 or the camera 11 is enlarged.
- the lens power source 20 of the intermediate lens 5 and the projection lens 6 is controlled from the main body control unit 21 so as to project onto the lens.
- the electron beam diffraction pattern 22b after projection on the fluorescent screen 10 or the camera 11 is obtained.
- the electron beam diffraction pattern 22b projected on the fluorescent screen 10 or the camera 11 is displayed on the monitor 13 via the camera control unit 12 under the control of the main body control unit 21.
- the operator selects the main spot (direct beam) 23 of the electron diffraction pattern 22b displayed on the monitor 13 by a click operation or the like via an input device such as a mouse.
- the position of the main spot 23 is displayed by the setting unit 34 (step 605).
- the sample stage 32 is once moved to a place where the sample 8 does not exist, the position information of the shining spot is stored, and then the electron diffraction pattern 22 on the sample 8 is displayed.
- the sample stage 32 can be moved to a position that matches the previously stored position as the main spot 23. In this way, the main spot 23 can be correctly selected even when there is a diffraction spot having the same intensity at an adjacent position.
- the main spot can be automatically selected by an instruction from the main body control unit 21.
- the circular pattern 26 is superimposed and displayed so that the main spot 23 is positioned on the circumference via the pattern setting unit 35 of the main body control unit 21 (step). 606).
- the size of the circular pattern 26 can be adjusted in accordance with the luminance distribution of the electron diffraction pattern 22b.
- the pattern setting unit 35 of the main body control unit 21 can display so as to arrange the circular pattern 26 inside the luminance distribution of the diffraction spot of the electron beam diffraction pattern 22b.
- the circular pattern 26 and its center point (vector start point) P (x, y) are determined, and the center point P (x, y) of the circular pattern 26 and the origin (the position of the main spot 23)
- a vector V28 connecting the end point of the vector 0 (0, 0) is displayed.
- the sample 8 is tilted in accordance with the direction and size (length) of the vector 28 (step 607).
- the inclination of the sample 8 information on the position of coordinates on the X, Y orthogonal coordinates of 0 (0, 0) and P (x, y), and information on the size and direction of the vector 28, respectively.
- Is transmitted to the vector information acquisition unit 37 of the main body control unit 21, and the tilting direction and tilting angle of the sample 8 are obtained by the calculation unit 38. Therefore, the calculation is performed via the sample fine movement drive mechanism instructing unit 39 based on the obtained result. Is called.
- the electron microscope 1 is changed to the image observation mode by the observation mode switching unit 40 of the main body control unit 21, and an image when the sample 8 is tilted is displayed on the monitor 13.
- the operator adjusts the sample fine movement manually or by the main body control unit 21 automatically operating the sample moving mechanism 9a of the sample fine movement driving mechanism 9. For example, it is possible to prevent the visual field from being lost when the sample 8 is tilted.
- the reproducibility and accuracy of the sample stage May not be adjusted to the actual position of the sample 8, but as described above, by correcting the visual field movement in real time at the time of image observation in the image observation mode, it is possible to reliably correct the positional deviation.
- the visual field movement can be adjusted by changing the irradiation region of the electron beam 15 by controlling a deflector (not shown).
- the observation mode switching unit 40 of the main body control unit 21 changes the observation mode to the electron diffraction pattern 22b, and the electron diffraction pattern 22b is displayed on the monitor 13 (step 608).
- step 609 the crystal orientation alignment result of the displayed electron diffraction pattern 22 is confirmed (step 609).
- a further step is performed. The operation from step 608 to step 609 is repeated.
- step 607 described above when correction is made when the visual field shift occurs when the sample 8 is tilted, it is desirable to cope with the change to the image mode.
- the entire field of view is displayed by removing the limited field stop 18 in conjunction with switching to the image mode.
- the diaphragm driving mechanism 19 may be driven so that the limited field diaphragm 18 enters again when switching to the observation mode of the electron diffraction pattern 22b.
- switching to the image mode can be omitted.
- FIG. 7 is a diagram for explaining the operation of crystal orientation adjustment according to the present embodiment.
- Circular Pattern In the example of FIG. 4 described above in the first embodiment, the method of fitting the luminance distribution of the diffraction pattern 22 and the size of the circular pattern 26 has been described. However, when the observation of the diffraction pattern 22 is started, if the crystal orientation is greatly deviated from the zone axis incidence, fitting with the circular pattern 26 may be difficult with the above-described method.
- the main spot 23 is designated as the origin 0 (0, 0) by the cursor 25 (a), and then the diffraction spot of the electron diffraction pattern 22b, that is, the luminance distribution is large.
- the circle pattern 26 to be displayed is displayed so that the circumference of the circular pattern 26 always passes through the main spot 23, that is, the cursor 25 (b).
- the inclination angle of the sample 8 is obtained based on the marker 27 displayed as the center point P (x, y) of the circular pattern 26 and the vector 28 connecting the main spot 23, that is, the marker 25.
- FIG. 8 is a diagram showing a crystal orientation matching method according to the third embodiment. In the present embodiment, a method of performing fitting using an arc-shaped pattern (a part of the circumference) 33 instead of the circular pattern 26 described above will be described.
- the option marker 25 is displayed with the main spot 23 as the origin O (0, 0) (a).
- the arc-shaped pattern 33 is displayed (b) so as to pass through the origin 0 (0, 0), which is the main spot 23, that is, the marker 25 and fit to the luminance distribution of the electron beam diffraction pattern 22b.
- the coordinates (x1, y1) and (x2, y2) of any two points on the fitted arc-shaped pattern 33 are displayed and recorded (c).
- the fitted arc-shaped pattern 33 is a part of the circumference of the circular pattern 26, and the virtual coordinate point P (a, b) of the center point of the circular pattern 26 sets the virtual radius of the circular pattern 26 to r. Then, it can be obtained from the following simultaneous equations (2-1, 2-2, 2-3).
- FIG. 10 is a diagram for explaining the operation according to the fourth embodiment.
- (A) shows the electron diffraction pattern 22b in the case where the crystal orientation is deviated from the zone axis with respect to the incident axis of the electron beam 15, and (b) shows the crystal orientation with respect to the incident axis of the electron beam 15.
- the electron beam diffraction pattern 22b coincides with the zone axis, that is, in the state where the zone axis is incident.
- the circumference of the circular pattern 26 to be fitted to the diffraction spot is displayed not as a line but as a semi-transparent band-like marker having an arbitrary width.
- the position of the diffraction spot can be confirmed even if it is displayed superimposed on the diffraction spot. Therefore, compared with the embodiment described above, the fitting to the diffraction spot can be performed more easily.
- Electron diffraction pattern 22b ... Electron diffraction pattern 23 projected onto fluorescent screen or camera ... Main spot 24 ; Diffraction spot 25 ... Marker 26 ; Circular shape Pattern 27 ... Marker 28 Vector 29 ... Si substrate 30 ... gate electrode 31 ... gate electrode edge 32 ... sample stage 33 ... arcuate pattern (part of the circumference) 34 ... Main spot setting unit 35 ... Pattern setting unit 36 ... Vector setting unit 37 ... Vector information acquisition unit 38 ... Calculation unit 39 ... Sample fine movement drive mechanism instruction unit 40 ... Observation mode switching section
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Abstract
Description
以下、本発明の実施の形態について図面を用いて説明する。なお、全体を通して、各図における同一の各構成部分には同一の符号を付して説明を省略することがある。
≪装置構成≫
図1に本実施の形態に係る電子顕微鏡1の基本構成を示す。電子顕微鏡1の鏡体は、主として、電子銃2、コンデンサーレンズ3、対物レンズ4、中間レンズ5および投射レンズ6により構成される。
≪本体制御部の構成≫
図11は、本体制御部21に含まれる構成のうち、主に、後述する本実施の形態に係る結晶方位合わせに関係する構成部について説明する図である。結晶方位合わせに関係する構成部としては、主として、メインスポット設定部34、パターン設定部35、ベクトル設定部36、ベクトル情報取得部、演算部38、試料微動機構指示部39、観察モード切替え部40がある。なお、本体制御部21は上述の構成部以外にも種々の構成部を含むものとする。
≪光路図≫
図2に本実施の形態に係る電子線回折パターン22の観察時の透過電子顕微鏡1の光路図を示す。本図では、光軸から蛍光板10が外れるように移動したときの様子を示しているが、カメラ11の上部に蛍光板10を配置するようにすることもできる。電子線15は試料8に平行照射される。試料8が結晶性試料の場合、電子線15には結晶によって回折を受けずに直進する電子線15aと、回折を受ける電子線15bが存在し、同じ角度で回折された電子線15bは対物レンズ4の後焦点面で1点に集まり、後焦点面上に電子線回折パターン22aを形成する。
〔式1〕R=Ltanθ~Lθ
で表わされる。ここで、Lは予め既知の結晶性の試料8を用いて求められるので、電子線回折パターン22aが形成される面における距離Rと、試料8の結晶面の結晶軸8aに対して電子線15が入射する角度θは、回折パターン22上の距離Rを測定することによって式(1)により求めることができる。
わせ、円形状パターン26の大きさを調整することができる。ここで、本体制御部21のパターン設定部35は、電子線回折パターン22bの回折スポットの輝度分布の内側に円形状パターン26を配置するように表示することができる。
(第2の実施形態)
図7は、本実施の形態に係る結晶方位合わせの動作を説明する図である。円形状パターン
第1の実施形態において上述した図4の例では、回折パターン22の輝度分布と円形状パターン26の大きさをフィッティングさせる手法について説明した。しかしながら、回折パターン22の観察開始時に、結晶方位が晶帯軸入射から大きくずれている場合には、上述の手法では円形状パターン26によるフィッティングが困難となってしまうことがある。
(第3の実施形態)
図8は、第3の実施形態に係る結晶方位合わせの手法を示す図である。本実施の形態では、上述の円形状パターン26に代えて、円弧状パターン(円周の一部)33を利用してフィッティングを行う手法について説明する。
〔式2-1〕a2+b2=r2〔式2-2〕(x1-a)2+(y1-b)2=r2〔式2-3〕(x2-a)2+(y2-b)2=r2 上記の式から求めた結果より、中心点の仮想座標点P(a,b)から原点0(0,0)
すなわちマーカ25までのベクトル28が得られ、対応する試料8の傾斜の量および方向を求めて、試料微動駆動機構9の試料傾斜機構9bにより試料8を傾斜させ、結晶方位合わせを行って、晶帯軸入射(d)となるように調整することができる。
(第4の実施形態)
図10は、第4の実施の形態に係る動作を説明する図である。(a)は、電子線15の入射軸に対し、結晶方位が晶帯軸からずれている場合の電子線回折パターン22bを示し、(b)は電子線15の入射軸に対し、結晶方位が晶帯軸と一致している、すなわち晶帯軸入射の状態の電子線回折パターン22bを示す。本実施の形態では、回折スポットにフィッティングさせる円形状パターン26の円周は、線ではなく半透明の任意の幅の帯状のマーカとして表示する。これにより、回折スポットの上に重ね合わせて表示しても、回折スポットの位置を確認できる。よって、上述した実施の形態と比較して、回折スポットへのフィッティングをより容易に行うことができる。
2・・・電子銃
3・・・コンデンサーレンズ
4・・・対物レンズ
5・・・中間レンズ
6・・・投射レンズ
7・・・試料ホルダ
8・・・試料
8・・・結晶軸
9・・・試料微動駆動機構
9a・・・試料移動機構
9b・・・試料傾斜機構
10・・・蛍光板
11・・・カメラ
12・・・カメラ制御部
13・・・モニタ
14・・・画像解析部
15・・・電子線
16・・・収束可動絞り
17・・・対物可動絞り
18・・・制限視野可動絞り
19・・・可動絞り駆動制御機構
20・・・レンズ電源
21・・・本体制御部
22a・・・電子線回折パターン
22b・・・蛍光板またはカメラに投影後の電子線回折パターン
23・・・メインスポット
24・・・回折スポット
25・・・マーカ
26・・・円形状パターン
27・・・マーカ
28・・・ベクトル
29・・・Si基板
30・・・ゲート電極
31・・・ゲート電極エッジ
32・・・試料ステージ
33・・・円弧状パターン(円周の一部)
34・・・メインスポット設定部
35・・・パターン設定部
36・・・ベクトル設定部
37・・・ベクトル情報取得部
38・・・演算部
39・・・試料微動駆動機構指示部
40・・・観察モード切替え部
Claims (9)
- 電子線を試料に照射する電子源と、
前記試料を保持する試料ステージと、
前記試料ステージを駆動する駆動部と、
当該電子線の照射によって試料から得られる信号を取得し、試料像を検出する検出部と、
前記試料の電子線回折像を表示する表示部と、
制御部と、を備え、
前記制御部は、
前記表示部に表示された電子線回折パターンにおける回折スポットの輝度分布に基づいて、メインスポットが円周上に位置するように重ね合わせて表示されるフィッティング用の円形状パターンを設定するパターン設定部と、
当該表示された円形状パターンの中心位置を始点とし、前記円形状パターン形状パターンの円周上に位置するメインスポットの位置を終点として表示されるベクトルを設定するベクトル設定部と、を有し、
当該表示されたベクトルの向き、及び大きさに基づいて、前記試料を傾斜するように、前記駆動部を制御することを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記パターン設定部は、
前記フィッティング用の円形状パターンを、前記輝度分布が存在する領域の内側に表示されるように設定することを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記パターン設定部は、
前記円形状パターンの大きさを変更することを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記制御部は、
前記ベクトル設定部によって設定されたベクトルの向きに基づいて前記試料の傾斜方向を求め、前記ベクトルの大きさに基づいて前記試料の傾斜角度を求めることを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記制御部は、
前記試料を傾斜しているときに、
当該検出部に検出された試料像を前記表示部に表示するように観察モードを切り替えることを特徴とする荷電粒子線装置。 - 請求項1に記載された電子顕微鏡において、
前記電子線の照射領域を偏向する偏向器を備え、
前記制御部は、
前記試料を傾斜しているときに生じる視野ずれを補正するように、前記偏向器を制御することを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記パターン設定部は、
前記フィッティング用の円形状パターンに代えて、前記表示部に表示された電子線回折パターンにおける回折スポットの輝度分布に基づいて、メインスポットが円周上に位置するように重ね合わせて表示される前記円形状パターンの円周の一部を形成するフィッティング用の円弧状パターンを設定し、
前記ベクトル設定部は、
当該表示された円弧状パターンの円周上の任意の2点の座標に基づいて、前記円形状パターンの半径を求め、
当該求めた半径に基づいて、前記円形状パターンの中心位置を設定し、当該設定した中心位置を始点とし、前記円形状パターンの円周上に位置するメインスポットの位置を終点として表示されるベクトルを設定することを特徴とする電子顕微鏡。 - 請求項1に記載された電子顕微鏡において、
前記パターン設定部は、
前記フィッティング用の円形状パターンを、半透明の帯状に設定することを特徴とする電子顕微鏡。 - 電子線を試料に照射する電子源と、
前記試料を保持する試料ステージと、
前記試料ステージを駆動する駆動部と、
当該電子線の照射によって試料から得られる信号を取得し、試料像を検出する検出部と、
前記試料の電子線回折像を表示する表示部と、
制御部と、を備えた電子顕微鏡を用いた試料の観察方法であって、
前記表示部に表示された電子線回折パターンにおける回折スポットの輝度分布に基づいて、メインスポットが円周上に位置するように重ね合わせて表示されるフィッティング用の円形状パターンを設定するステップと、
当該表示された円形状パターンの中心位置を始点とし、前記円形状パターンの円周上に位置するメインスポットの位置を終点として表示されるベクトルを設定するステップと、
当該表示されたベクトルの向き、及び大きさに基づいて、前記試料を傾斜するステップと、を有することを特徴とする試料の観察方法。
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2019075286A (ja) * | 2017-10-17 | 2019-05-16 | 日本電子株式会社 | 電子顕微鏡および試料傾斜角の調整方法 |
KR20200012947A (ko) * | 2017-05-31 | 2020-02-05 | 닛폰세이테츠 가부시키가이샤 | 경사 각도량 산출 장치, 시료대, 하전 입자선 장치 및 프로그램 |
JP2020119667A (ja) * | 2019-01-21 | 2020-08-06 | 日本電子株式会社 | 電子顕微鏡 |
JPWO2020217297A1 (ja) * | 2019-04-23 | 2020-10-29 | ||
US11742172B2 (en) | 2019-01-11 | 2023-08-29 | Hitachi High-Tech Corporation | Charged particle beam device and control method thereof |
US11791131B2 (en) | 2019-05-23 | 2023-10-17 | Hitachi High-Tech Corporation | Charged particle beam apparatus and method for controlling charged particle beam apparatus |
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JP6823563B2 (ja) * | 2017-07-31 | 2021-02-03 | 株式会社日立製作所 | 走査電子顕微鏡および画像処理装置 |
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EP4401038A1 (en) * | 2021-10-18 | 2024-07-17 | Lightvision Inc. | System and method for generating tem sadp image with high distinguishability |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010212067A (ja) * | 2009-03-10 | 2010-09-24 | Jeol Ltd | 電子顕微鏡の自動試料傾斜装置 |
JP2011181393A (ja) * | 2010-03-02 | 2011-09-15 | Hitachi High-Technologies Corp | 荷電粒子線装置及び荷電粒子線を用いた測長方法 |
JP2013101791A (ja) * | 2011-11-08 | 2013-05-23 | Hitachi High-Technologies Corp | 走査透過電子顕微鏡、および試料観察方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5179280A (en) * | 1990-10-12 | 1993-01-12 | Chi & Associated Inc. | Computer control of the electron microscope sample stage |
US8203120B2 (en) * | 2008-10-09 | 2012-06-19 | California Institute Of Technology | 4D imaging in an ultrafast electron microscope |
US9103769B2 (en) * | 2009-12-15 | 2015-08-11 | The Regents Of The University Of California | Apparatus and methods for controlling electron microscope stages |
CN103149227B (zh) * | 2013-03-15 | 2015-04-15 | 中国工程物理研究院机械制造工艺研究所 | 一种用于高分辨中子粉末衍射谱仪的精密主体运动装置 |
-
2015
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010212067A (ja) * | 2009-03-10 | 2010-09-24 | Jeol Ltd | 電子顕微鏡の自動試料傾斜装置 |
JP2011181393A (ja) * | 2010-03-02 | 2011-09-15 | Hitachi High-Technologies Corp | 荷電粒子線装置及び荷電粒子線を用いた測長方法 |
JP2013101791A (ja) * | 2011-11-08 | 2013-05-23 | Hitachi High-Technologies Corp | 走査透過電子顕微鏡、および試料観察方法 |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20200012947A (ko) * | 2017-05-31 | 2020-02-05 | 닛폰세이테츠 가부시키가이샤 | 경사 각도량 산출 장치, 시료대, 하전 입자선 장치 및 프로그램 |
KR102408912B1 (ko) | 2017-05-31 | 2022-06-14 | 닛폰세이테츠 가부시키가이샤 | 경사 각도량 산출 장치, 시료대, 주사 전자 현미경 및 컴퓨터 판독 가능 저장 매체에 저장된 컴퓨터 프로그램 |
JP2019075286A (ja) * | 2017-10-17 | 2019-05-16 | 日本電子株式会社 | 電子顕微鏡および試料傾斜角の調整方法 |
JP6994897B2 (ja) | 2017-10-17 | 2022-01-14 | 日本電子株式会社 | 電子顕微鏡および試料傾斜角の調整方法 |
US11742172B2 (en) | 2019-01-11 | 2023-08-29 | Hitachi High-Tech Corporation | Charged particle beam device and control method thereof |
JP2020119667A (ja) * | 2019-01-21 | 2020-08-06 | 日本電子株式会社 | 電子顕微鏡 |
JP7126960B2 (ja) | 2019-01-21 | 2022-08-29 | 日本電子株式会社 | 電子顕微鏡 |
JPWO2020217297A1 (ja) * | 2019-04-23 | 2020-10-29 | ||
WO2020217297A1 (ja) * | 2019-04-23 | 2020-10-29 | 株式会社日立ハイテク | 荷電粒子線装置及び荷電粒子線装置の制御方法 |
JP7187685B2 (ja) | 2019-04-23 | 2022-12-12 | 株式会社日立ハイテク | 荷電粒子線装置及び荷電粒子線装置の制御方法 |
US11756764B2 (en) | 2019-04-23 | 2023-09-12 | Hitachi High-Tech Corporation | Charged particle beam apparatus and method of controlling charged particle beam apparatus |
US11791131B2 (en) | 2019-05-23 | 2023-10-17 | Hitachi High-Tech Corporation | Charged particle beam apparatus and method for controlling charged particle beam apparatus |
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