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WO2019008699A1 - Dispositif à faisceau de particules chargées - Google Patents

Dispositif à faisceau de particules chargées Download PDF

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Publication number
WO2019008699A1
WO2019008699A1 PCT/JP2017/024650 JP2017024650W WO2019008699A1 WO 2019008699 A1 WO2019008699 A1 WO 2019008699A1 JP 2017024650 W JP2017024650 W JP 2017024650W WO 2019008699 A1 WO2019008699 A1 WO 2019008699A1
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WIPO (PCT)
Prior art keywords
image
charged particle
sample
particle beam
irradiating
Prior art date
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Ceased
Application number
PCT/JP2017/024650
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English (en)
Japanese (ja)
Inventor
宗史 設楽
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Hitachi High Tech Corp
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Hitachi High Technologies Corp
Hitachi High Tech Corp
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Priority to JP2019528259A priority Critical patent/JP6811324B2/ja
Priority to PCT/JP2017/024650 priority patent/WO2019008699A1/fr
Publication of WO2019008699A1 publication Critical patent/WO2019008699A1/fr
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
    • H01J37/02—Details
    • H01J37/22—Optical, image processing or photographic arrangements associated with the tube

Definitions

  • the present invention relates to a charged particle beam device.
  • the grain size and shape of the crystal grains in the crystalline sample are closely related to the material properties. For example, it is known that when the crystal grain is miniaturized in the metal wiring, the wiring resistance increases due to the increase of the grain boundary, and the strength changes depending on the shape of the crystal grain. Therefore, accurate understanding of the state of crystal grains is important in understanding material characteristics.
  • ECC electron channeling contrast
  • EBSD backscattered electron diffraction
  • Patent Document 1 discloses a method of accurately specifying the three-dimensional positional relationship and density distribution of the internal structure of a sample by using a signal generated from the sample. At this time, the sample or the electron beam is tilted to obtain a signal.
  • Patent Document 2 discloses a method capable of optimizing the ECC and optimizing the domain with high versatility by optimizing the deposition thickness of the conductive film and the observation conditions in the domain observation of a ferroelectric or the like. There is.
  • the grain size and shape of the crystal grains can be grasped by the ECC observation, depending on the crystal orientation, the ECC of the adjacent crystal grains may be low and the crystal grains may be overlooked. Therefore, in order to accurately grasp the crystal grains, it is necessary to change the electron diffraction conditions by changing the SEM conditions such as the acceleration voltage and the sample inclination angle to obtain a plurality of different ECC images. Specifically, a plurality of ECC images are acquired in the same field of view, and the acquired ECC images are compared.
  • the SEM conditions for example, the acceleration voltage is changed
  • the incident depth of the electron beam to the sample changes, so the generation depth of the reflected electrons changes and the particle size obtained from the ECC image changes.
  • the optical conditions are also changed, deviation of the observation position or the like occurs.
  • the sample tilt angle is changed, it is necessary to correct the magnification change due to the shift of the observation position or the tilt, and there is a concern that the accuracy may be reduced.
  • the throughput also decreases because it is necessary to move the stage.
  • Patent Document 1 describes the method of specifying the internal structure of a sample, it does not describe specifying the structure of the crystal grain in the sample surface.
  • the method described in Patent Document 2 may have low image contrast in adjacent domains and it may be difficult to accurately grasp crystal grains.
  • the present invention has been made in view of the above problems, and in a charged particle beam apparatus for observing a sample by irradiating the sample with a charged particle beam, crystal grains of a crystalline sample can be accurately measured. It provides technology that can be grasped.
  • a first image obtained by irradiating the sample with the charged particle beam in a first direction, and the charged particle beam with respect to the sample in the first direction A crystal grain is grasped
  • crystal grains can be accurately grasped in a crystalline sample.
  • FIG. 1 is a configuration diagram of a scanning electron microscope 100 according to Embodiment 1. It is a schematic diagram which shows the example of an ECC image. It is an example of the synthetic
  • FIG. 7 is a flowchart illustrating a procedure of analyzing the configuration of a sample 11 by a computer 27. FIG. It is an observation example in the similar part of the schematic diagram shown in FIG. It is an observation example in the similar part of the schematic diagram shown in FIG.
  • FIG. 1 is a block diagram of a scanning electron microscope 100 according to a first embodiment of the present invention.
  • the scanning electron microscope 100 is an apparatus for acquiring an observation image of the sample 11 by irradiating the sample 11 with the electron beam 2.
  • the scanning electron microscope 100 includes an electron microscope main body 70, a control unit 80, and an input / output unit 90.
  • the high voltage power supply control circuit 19 applies a high voltage to the electron gun 1.
  • the electron gun 1 emits an electron beam 2 when a high voltage is applied.
  • the electron beam 2 generated from the electron gun 1 is irradiated by the focusing lens 3 and the objective lens 6 so as to be focused on the sample 11 as a minute spot.
  • the focusing lens control circuit 20 controls the focusing lens 3, and the objective lens control circuit 23 controls the objective lens 6.
  • the electron beam 2 is two-dimensionally scanned on the sample 11 by the upper and lower scanning coils 4.
  • the scanning coil control circuit 21 controls the scanning coil 4.
  • the scanning coil control circuit 21 repeats line scanning. That is, after scanning in the + X direction from a certain position, the scanning in the + X direction is repeated shifting from the certain position in the 1-pixel Y direction. Furthermore, by using the gradient coil 5 and the focusing coil 7 in combination, the electron beam 2 can be tilted to be incident on the sample 11 from the first direction 9 or the second direction 10.
  • the gradient coil control circuit 22 controls the gradient coil 5.
  • the focusing coil control circuit 24 controls the focusing coil 7.
  • the first direction 9 and the second direction 10 referred to here are directions on the plane on which the sample 11 is placed.
  • the tilt angle of the electron beam 2 with respect to the same plane (or the tilt angle of the electron beam 2 with respect to the optical axis) is the same in both the first direction 9 and the second direction 10.
  • the computer 27 controls the scanning timing of the electron beam 2. By sequentially irradiating the non-tilt / first direction 9 / second direction 10 for each line, it is possible to obtain observation images corresponding to the respective incident directions.
  • Each control circuit can switch between the three types of beams at such a time interval that there is no sense of incongruity even when a human looks at three types of observation images generated from these three types of beams. All three of these beams can be illuminated for the same scan position within a time interval of, for example, about one second or less.
  • the sample 11 is fixed to the sample stage 12.
  • the upper surface (sample mounting surface) of the sample stage 12 can be configured to be parallel to the installation surface of the scanning electron microscope 100.
  • the sample stage 12 can move the sample 11 in the XYZ directions to rotate and tilt the sample mounting surface.
  • the sample stage control circuit 26 controls the sample stage 12.
  • the computer 27 includes a high voltage power supply control circuit 19, a focusing lens control circuit 20, a scanning coil control circuit 21, a gradient coil control circuit 22, an objective lens control circuit 23, a focusing coil control circuit 24, a signal input circuit 25, and a sample stage control circuit. It is connected to 26 etc. and controls these in an integrated manner.
  • the computer 27 is connected with an input device 30 such as a keyboard, a mouse, a trackball, and a control panel for changing the focus magnification. The user can set the acquisition condition of the observation image through the input device 30.
  • the signal detected by the X-ray detector 18 is sent to the computer 31 for elemental analysis.
  • the elemental analysis computer 31 specifies the constituent elements of the sample 11 using the signal.
  • the computer 31 for elemental analysis is connected to the computer 27 and can control the high voltage power control circuit 19 and the like in the same manner as the computer 27.
  • the elemental analysis computer 31 can further capture an observation image of the sample 11 and carry out elemental analysis and image analysis of the same field of view.
  • FIG. 2 is a schematic view showing an example of the ECC image.
  • a nickel alloy which is a crystalline sample was used as the sample 11.
  • the ECC image 201 is an observation image obtained by irradiating the electron beam 2 in the first direction 9.
  • the ECC image 202 is an observation image obtained by irradiating the electron beam 2 in the second direction 10.
  • the grain boundaries in the dotted line are blurred. This is because the angle at which the electron beam 2 is incident on the sample 11 differs in the first direction 9 and the second direction 10, so that the electron diffraction conditions change, and as a result, the amount of reflected electrons generated per ECC image Attributable to different things.
  • the computer 27 generates a composite image 203 by combining the ECC images 201 and 202.
  • a clear grain boundary image is obtained over the entire image by compensating the grain boundary portion which is unclear on any one of the ECC images by the other clear grain boundary portion. Therefore, crystal grains can be grasped with a single composite image 203 without comparing ECC images.
  • FIG. 3 shows an example of a composite image 203 synthesized after color arrangement.
  • the computer 27 can generate, for example, an image having only a red component for the ECC image 201 and generate an image having only a blue component for the ECC image 202. By combining these ECC images, it is possible to obtain a combined image 203 in which the red color arrangement and the blue color arrangement are mixed. Other color schemes may be used. The user can recognize crystal grain boundaries more clearly by synthesizing a plurality of color arrangements.
  • FIG. 4 is an example of a grain boundary extraction image.
  • the computer 27 extracts crystal grain boundaries from each of the ECC images 201 and 202, and superimposes the extracted crystal grain boundaries by, for example, a method such as pattern matching to generate a grain boundary extracted image as illustrated in FIG. can do.
  • the computer 27 may generate the composite image 203 and the grain boundary extraction image at the same time when the ECC images 201 and 202 are stored in the image memory 29, or after the ECC images 201 and 202 are once generated, they are off-line. These images may be created by processing.
  • the electron beam 2 irradiated in the first direction 9 and the electron beam 2 irradiated in the second direction 10 may be irradiated to different portions of the sample 11, respectively. In this case, the irradiation direction may be corrected by the gradient coil 5, or the corresponding areas may be superimposed by pattern matching or the like after the ECC image is once acquired.
  • FIG. 5 is the analysis result by EBSD.
  • the same composite image as FIG. 3 is shown at the top of FIG. 5 for comparison.
  • the lower part of FIG. 5 is an EBSD analysis result in the same visual field region. It can be seen that the composite image has obtained grain boundaries equivalent to the analysis result by EBSD.
  • the scanning electron microscope 100 generates the ECC image 201 by irradiating the electron beam 2 in the first direction 9, and generates the ECC image 202 by irradiating the electron beam 2 in the second direction 10. By combining these, a composite image 203 is obtained. Thereby, since the difference in electron channeling contrast caused by the incident direction of the electron beam 2 can be compensated by each ECC image, the crystal grain boundary of the crystalline sample 11 can be identified accurately.
  • the scanning electron microscope 100 switches the first direction 9 and the second direction 10 within a very short time interval.
  • the composite image 203 can be obtained in substantially real time, the user can efficiently search for the optimal observation conditions that can best identify the grain boundaries.
  • the scanning coil control circuit 21 (and the scanning coil 4) can also change the scanning direction by rotating the scanning direction of the electron beam 2 by an arbitrary angle (for example, 90 °). This function is called raster rotation.
  • an operation example using an ECC image acquired in the changed scanning direction will be described.
  • the configuration of the scanning electron microscope 100 is the same as that of the first embodiment.
  • FIG. 6 shows an example of the ECC images 204 and 205 acquired after changing the scanning direction of the electron beam 2 by 90 degrees.
  • the image is rotated by -90 degrees in order to align with FIG. 9 described later.
  • FIG. 6 it can be seen that an ECC image different from that of FIG. 9 is obtained. This is because the direction in which the electron beam 2 is incident on the sample 11 is rotated by 90 degrees from the first direction 9 and the second direction 10 by rotating the scanning direction.
  • the crystal grains can be analyzed more accurately and in detail.
  • the scanning direction may be rotated at an angle other than 90 degrees.
  • images similar to the ECC images 204 and 205 may be acquired after being acquired respectively in a plurality of scanning directions.
  • Embodiment 3 Since ECC is generated according to the crystal structure of the sample 11, it changes depending on the incident direction of the electron beam 2. On the other hand, the luminance value of the observation image may be different from that of the other portions due to the difference in the composition in each portion of the sample 11. Since all of these appear as differences in luminance values of pixels on the observation image, it is generally difficult to distinguish whether the differences in luminance values are caused by crystal structure or due to differences in composition. In the third embodiment of the present invention, a method of distinguishing these differences will be described. The configuration of the scanning electron microscope 100 is the same as that of the first embodiment.
  • FIG. 7 is a schematic view showing an example of an ECC image acquired for a portion where a carbon foreign matter 703 is present on a nickel alloy.
  • the ECC image 701 is acquired in the first direction 9, and the ECC image 702 is acquired in the second direction 10.
  • the luminance value of the grain boundary is lowered and blurred as shown by the dotted line, but the luminance value of the foreign matter 703 hardly changes in the ECC images 701 and 702. This is because the ECC relies on the incident direction of the electron beam 2 while the luminance value due to the composition has a small dependence on the incident direction.
  • this fact is used to distinguish whether the change in luminance value is caused by the composition or the crystal structure.
  • the generation rate of the backscattered electrons is about 0.3 when the incident angle of the electron beam is 0 degree (the electron beam is incident perpendicularly to the sample 11) Even if the electron beam 2 is inclined 50 degrees with respect to the optical axis, it is about 0.4. Even when the incident direction is changed instead of the incident angle, the same tendency is obtained. This indicates that the luminance value due to the difference in composition is less affected by the incident direction and the incident angle of the electron beam 2.
  • the computer 27 in the area where the luminance value differs by a predetermined threshold (for example, a relative ratio of 5%) or more between the ECC images 701 and 702, the computer 27 generates the luminance difference due to the ECC, and the luminance difference is a predetermined threshold. It is determined that the luminance difference is caused due to the composition for the area less than. Thereby, ECC and composition contrast can be distinguished. That is, it can be determined whether the cause of the luminance difference is due to the crystal orientation or the composition.
  • a predetermined threshold for example, a relative ratio of 5%
  • FIG. 8 is a flow chart for explaining the procedure of analyzing the configuration of the sample 11 by the computer 27. Each step of FIG. 8 will be described below.
  • Step S801 The operator inputs analysis conditions such as an analysis range and acceleration voltage via the input device 30.
  • the computer 27 receives the analysis condition specification.
  • Step S802 The operator specifies through the input device 30 whether the sample 11 is a crystalline sample.
  • the computer 27 receives the designation. If the sample 11 is a crystalline sample, the process proceeds to step S803. If the sample 11 is not a crystalline sample, the process proceeds to step S806. This step is provided to omit steps S803 to S805 when the sample 11 is an amorphous sample. Therefore, if it is not necessary to omit these steps, this step is not necessary either.
  • Step S803 The computer 27 acquires observation images in each of the first direction 9 and the second direction 10, and extracts crystal particles from the observation image.
  • Step S804 The operator selects, via the input device 30, whether the purpose of analysis is to extract the compositional contrast of the sample 11 or whether to aim at extracting others (that is, extracting crystal grains). If the purpose is to extract the composition contrast, the process advances to step S805; otherwise, the process advances to step S807.
  • Step S805 The computer 27 extracts a portion where the difference in luminance value is less than a predetermined threshold between the two observation images acquired in step S803. It can be estimated that the place where the luminance value does not change even if the incident direction of the electron beam 2 is changed is the place representing the composition of the sample 11.
  • Step S806 The computer 27 obtains an observation image by vertically impinging the electron beam 2 on the sample 11. Alternatively, observation images may be acquired in each of the first direction 9 and the second direction 10, and these may be combined. After this step, the process skips to step S808.
  • Step S 807 The computer 27 extracts a portion where the difference in luminance value is equal to or greater than a predetermined threshold (the same as the threshold in step S805) between the two observation images acquired in step S803.
  • a predetermined threshold the same as the threshold in step S805
  • ECC the luminance value change due to the crystal orientation
  • Step S808 The computer 27 performs particle identification such as shape recognition of particles and elemental analysis of the particles using the images acquired in steps S805 to S807. Since only the composition contrast or only the ECC is extracted in steps S805 and S807, particles and crystals can be accurately analyzed in this step.
  • Steps S809 to S810 The operator selects, via the input device 30, whether or not to end the particle analysis (S809). If it does not end, the process moves to the next view and returns to step S802 (S810). When the analysis is ended, this flowchart is ended.
  • ECC electrospray analysis
  • compositional contrast is particularly important in particle analysis.
  • Particle analysis is an analysis method of extracting particles such as inclusions and impurities from an image and specifying the shape, number, and composition thereof.
  • particle analysis is performed on a crystalline sample, crystal grains by ECC may be extracted as particles such as inclusions.
  • particle analysis is performed automatically by a computer, so it is not possible to determine composition contrast and ECC empirically by visual confirmation in the process of particle analysis.
  • the method of changing the diffraction condition of the electron beam 2 by inclining the sample 11 during particle analysis or EBSD analysis has disadvantages in terms of accuracy and throughput.
  • elemental analysis although the element type can be specified, it can not be determined whether the place where the element is specified is a crystal grain or a particle of the same composition.
  • the scanning electron microscope 100 distinguishes the composition contrast from the ECC by deflecting the incident direction of the electron beam 2 and acquiring a plurality of observation images, the sample 11 can be analyzed efficiently.
  • a portion where the luminance value changes by a threshold or more between the first direction 9 and the second direction 10 can be excluded from the analysis target.
  • the crystal grain distribution can be grasped by extracting only a portion where the luminance value has changed by a predetermined threshold or more and performing particle analysis on the portion.
  • FIG. 9 is an observation example at a similar part of the schematic view shown in FIG.
  • the ECC image 206 is an observation image acquired by irradiating the electron beam 2 from the first direction 9.
  • the ECC image 207 is an observation image obtained by irradiating the electron beam 2 in the second direction 10.
  • crystal grains in the arrow portion can be grasped, but in the ECC image 207, crystal grains in the arrow portion can not be grasped.
  • the crystal grain of the arrow head can not be grasped, but in the ECC image 207, the crystal grain of the arrow head can be grasped.
  • the generation amount of the backscattered electrons differs for each ECC image.
  • FIG. 10 is an observation example at a similar part of the schematic view shown in FIG.
  • the ECC image was acquired about the location where the foreign material 706 of carbon exists on a nickel alloy similarly to FIG.
  • the ECC image 704 is an observation image acquired by irradiating the electron beam 2 from the first direction 9.
  • the ECC image 705 is an observation image obtained by irradiating the electron beam 2 in the second direction 10.
  • the brightness value of the grain boundary is lowered as shown by the arrow portion, but the brightness value of the foreign material 706 hardly changes between the ECC images 704 and 705.
  • the change in the luminance value is different depending on which of the composition and the crystal structure results.
  • the present invention is not limited to the above embodiment, but includes various modifications.
  • the above-described embodiment is described in detail to explain the present invention in an easy-to-understand manner, and is not necessarily limited to one having all the described configurations.
  • part of the configuration of one embodiment can be replaced with the configuration of another embodiment, and the configuration of another embodiment can be added to the configuration of one embodiment.
  • another configuration can be added to, deleted from, or replaced with a part of the configuration of each embodiment.
  • An anaglyph image is generated using the optical path difference of the electron beam 2 generated by the unevenness of the sample 11 while switching the observation image acquired in the first direction 9 and the observation image acquired in the second direction 10, and the surface of the sample 11
  • the ability to view 3D images is called the live stereo feature. Since this function is to observe the surface shape of the sample 11 using the secondary electrons 14, it can be used in combination with the method according to the present invention.
  • the method according to the present invention can be used to observe the crystal grains in the flat portion of the sample 11, and the live stereo function can be used to observe the three-dimensional shape of the uneven portion.
  • the method according to the present invention can also be used to detect minute crystal orientation changes such as crystal distortion and crystal defect observation.
  • minute crystal orientation changes such as crystal distortion and crystal defect observation.
  • semiconductors such as metals and InGaN
  • the number of fine orientation changes and the number of crystal defects are largely attributed to sample characteristics.
  • the contrast of crystal distortion and crystal defects can not be observed depending on the electron diffraction conditions. Therefore, it is considered that the method of the present invention which can easily grasp the change in orientation is useful.
  • the method of the present invention can also be used for a sample having poor conductivity and a charge-up phenomenon is likely to occur, or a sample whose sample shape is changed by an electron beam (for example, biological samples such as pearls and snail shells) .
  • EBSD analysis has the disadvantage of being susceptible to charge-up phenomena and sample damage, as it needs to be irradiated with a large amount of electron beams of high acceleration voltage in addition to low throughput and the need for expensive equipment.
  • the phenomenon is remarkable particularly in biological samples such as metal and snail shells molded into a blank.
  • the approach of the present invention can be used under conditions in which an ECC image is generally observed, so there is no need to use high acceleration large current conditions like EBSD analysis. Therefore, it is easy to suppress the charge up phenomenon and the electron beam damage.
  • the computer 27 has been described to display the analysis result as an image on the display device 28.
  • other output formats can be used.
  • data describing the position of grain boundaries can be output to an appropriate medium such as a storage device or a communication network, or can be output or printed on a medium such as paper by a printer or a camera.
  • data describing which one of the composition contrast and the ECC has been determined can be output together with the coordinates of the determined portion.
  • Other suitable output formats may be used.
  • the scanning electron microscope 100 has been described as an example of a charged particle beam device, but in other types of charged particle beam devices, crystals of a crystalline sample can be obtained by applying the same method as the present invention. Grain boundaries can be identified accurately.
  • Electron gun 2 Electron beam 3: Focusing lens 4: Scanning coil 5: Tilting coil 6: Objective lens 7: Focusing coil 8: Reflected electron detector 9: First direction 10: Second direction 11: Sample 12: Sample stage 13: reflection electron 14: secondary electron 15: X-ray 16: reflection electron detector 17: secondary electron detector 18: X-ray detector 19: high voltage power supply control circuit 20: Focusing lens control circuit 21: Scanning coil control circuit 22: gradient coil control circuit 23: objective lens control circuit 24: focus adjustment coil control circuit 25: signal input circuit 26: sample stage control circuit 27: computer 28: display device 29: image memory 30: input device 31: for elemental analysis Computer 70: electron microscope main body 80: control unit 90: input / output unit 100: scanning electron microscope

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Abstract

La présente invention concerne une technologie grâce à laquelle un dispositif à faisceau de particules chargées qui analyse un échantillon par irradiation d'un faisceau de particules chargées sur l'échantillon est capable de déterminer avec précision des grains cristallins dans un échantillon cristallin. Ce dispositif à faisceau de particules chargées utilise une première image et une seconde image et détermine des grains cristallins, ladite première image étant obtenue par irradiation d'un faisceau de particules chargées sur l'échantillon à partir d'une première direction et ladite seconde image étant obtenue par irradiation du faisceau de particules chargées sur l'échantillon à partir d'une seconde direction différente de la première direction.
PCT/JP2017/024650 2017-07-05 2017-07-05 Dispositif à faisceau de particules chargées Ceased WO2019008699A1 (fr)

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PCT/JP2017/024650 WO2019008699A1 (fr) 2017-07-05 2017-07-05 Dispositif à faisceau de particules chargées

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JP2022155554A (ja) * 2021-03-30 2022-10-13 エフ イー アイ カンパニ 三次元電子回折データを取得するための方法およびシステム

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