WO2014069325A1 - 電子ビーム顕微装置 - Google Patents

電子ビーム顕微装置 Download PDF

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Publication number
WO2014069325A1
WO2014069325A1 PCT/JP2013/078807 JP2013078807W WO2014069325A1 WO 2014069325 A1 WO2014069325 A1 WO 2014069325A1 JP 2013078807 W JP2013078807 W JP 2013078807W WO 2014069325 A1 WO2014069325 A1 WO 2014069325A1
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WIPO (PCT)
Prior art keywords
sample
electron beam
microscope according
sample holder
beam microscope
Prior art date
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Ceased
Application number
PCT/JP2013/078807
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English (en)
French (fr)
Japanese (ja)
Inventor
秀樹 菊池
圭司 田村
浩大 上田
浩一郎 齋藤
亮史 滑川
博実 稲田
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Hitachi High Tech Corp
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Hitachi High Technologies Corp
Hitachi High Tech Corp
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Publication of WO2014069325A1 publication Critical patent/WO2014069325A1/ja
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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
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement or ion-optical arrangement
    • H01J37/09—Diaphragms; Shields associated with electron or ion-optical arrangements; Compensation of disturbing fields
    • 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
    • H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
    • 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
    • H01J37/16—Vessels; Containers
    • 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

Definitions

  • the present invention relates to an electron beam microscope.
  • a sample is irradiated with an electron beam, and at that time, as an electron beam microscope that detects and analyzes characteristic X-rays generated from the sample, a transmission electron microscope (TEM), a scanning electron microscope (SEM), an electron probe micro analyzer (EPMA) etc. are widely used.
  • TEM transmission electron microscope
  • SEM scanning electron microscope
  • EPMA electron probe micro analyzer
  • the observation sample in the electron beam microscope is thinned to the order of several tens of nm by a focused ion beam apparatus or the like.
  • the observation sample is attached to the sample holder and introduced to the irradiation position of the electron beam in the evacuated sample chamber.
  • sample drift may occur due to a temperature difference between the sample holder and the inner wall of the sample, and the observed image may be distorted. Therefore, in order to reduce this sample drift, it is necessary to wait for a certain time after introducing the sample into the sample chamber.
  • a certain waiting time is required, and therefore, when it is desired to observe a plurality of samples, the time taken to introduce the sample is further increased.
  • Patent Document 1 discloses a sample exchange mechanism capable of detaching a sample at the tip of the sample holder in a sample chamber of an electron beam microscope.
  • FIG. 14 is a cross-sectional view of the sample surface of the conventional electron beam microscope, and illustrates the arrangement of the components of the conventional electron beam microscope.
  • a mirror 141 of the electron beam microscope comprises a sample stage 144, and the sample stage 144 has a sample holder 142 for mounting a sample 143.
  • the mirror body 141 is provided with an EDX detector 145, an exhaust port 146, an aperture mechanism 147, and a cold block 148.
  • the EDX detector 145, the aperture mechanism 147, and the cold block 148 are fixed to the port (opening) of the mirror 141. Therefore, when replacing or maintaining these components (EDX detector 145, diaphragm mechanism 147, cold block 148, etc.), it is necessary to release the electron beam microscope to the atmosphere, which greatly affects the throughput of sample observation. .
  • the present invention has been made in view of such a situation, and does not open the sample chamber of the electron beam microscope, but the various components used for the sample and the observation and analysis in a state where the sample chamber is evacuated. Provide technology that can be introduced.
  • the present application includes a plurality of means for solving the above-mentioned problems, one example thereof is a mirror capable of vacuum evacuation, an electron gun for generating an electron beam, an electromagnetic lens for focusing the electron beam, A first stage having a first sample holder on which the first sample is mounted, and a first air lock mechanism capable of introducing the first sample holder into the mirror without releasing the mirror into the atmosphere; A detector for detecting a signal generated as a result of interaction between the electron beam and the first sample, wherein the mirror is mounted on the first sample holder An opening portion provided with a second air lock mechanism is provided substantially in the same plane as the first sample, and the second air lock mechanism allows a predetermined member to be contained in the mirror body without releasing the mirror to the atmosphere. To be able to introduce Have been made electron beam microscopy device is provided.
  • the present invention it is possible to introduce components used for observation and analysis in a state where the sample chamber is evacuated, without releasing the sample chamber of the electron beam microscope into the atmosphere. This reduces the exchange time of the components, thereby improving the throughput of sample observation.
  • FIG. 1 is an entire configuration view of a transmission electron microscope (TEM) according to the present invention. It is sectional drawing of a sample stage. It is sectional drawing in the sample surface of the transmission electron microscope which concerns on 1st Example. It is a figure explaining the evacuation system of the transmission electron microscope concerning a 1st example. It is a figure explaining the stage control system of the transmission electron microscope concerning a 1st example. It is a top view of the outer cylinder of the sample stage of the transmission electron microscope which concerns on 1st Example. It is sectional drawing in the sample surface of the transmission electron microscope which concerns on 1st Example. It is a figure explaining the transmission electron microscope concerning a 2nd example. It is a figure explaining the transmission electron microscope concerning a 3rd example.
  • TEM transmission electron microscope
  • FIG. 1 is an entire configuration diagram of a transmission electron microscope (TEM) according to the present invention.
  • TEM transmission electron microscope
  • the configuration of a transmission electron microscope will be described as an example of an electron beam microscope, but the same configuration, operation, and effects can be applied to other electron beam microscopes that irradiate electron beams in vacuum. It is obvious that it can be obtained.
  • the transmission electron microscope 100 includes a vacuum-evacuable mirror 1, an electron gun 51, an electron lens 54, a mount 50, a sample stage 6, a stage controller 53, a detector 55, and a main control unit 57. Equipped with The mirror 1 is fastened to the vibration-removing mount 50.
  • the electron gun 51 is provided on the top of the mirror 1, and the electron lens 54 is disposed below the electron gun 51.
  • the sample stage 6 is provided at a port (opening) on the side of the mirror 1.
  • the sample stage 6 is controlled by a stage controller 53 which has received a command from the main control unit 57.
  • the detector 55 is disposed below the sample stage 6 and detects a signal resulting from the interaction between the electron beam from the electron gun 51 and the sample.
  • the electron beam generated by the electron gun 51 is converged by the electron lens 54 and irradiated to the sample mounted on the sample stage 6. Electrons transmitted through the sample on the sample stage 6 are detected by the detector 55. Then, the detected signal is captured by the main control unit 57 and imaged to observe the sample.
  • FIG. 2 is a cross-sectional view of the sample stage 6.
  • a spherical receiver 36 is fixed to the side surface of the mirror 1, and the spherical receiver 36 is in contact with the spherical fulcrum 37.
  • the sample stage 6 includes an air lock chamber (air lock mechanism) 600.
  • the air lock chamber 600 is constituted by a space surrounded by the air lock valve 34 and the outer cylinder 38.
  • the air lock chamber 600 can introduce the sample holder 2 into the mirror 1 while the mirror 1 is evacuated without releasing the mirror 1 to the atmosphere.
  • the air lock chamber 600 swings around the center of the spherical fulcrum 37, and as a result, the sample 3 mounted on the tip of the sample holder 2 in the Z direction (vertical direction) and the Y direction Direction) can be moved.
  • An inner cylinder 33 is disposed inside the outer cylinder 38. Further, the slider cylinder 30 is disposed inside the inner cylinder 33. Furthermore, the sample holder 2 is disposed inside the slider cylinder 30, and the sample holder 2 is attached to the slider cylinder 30 via the holder O-ring 4. The slider cylinder 30 is connected to the inner cylinder 33 by a bellows 32.
  • a base 24 is fixed to the mirror 1, and the rotary cylinder 20 is fastened to the base 24 via a bearing 23.
  • the Z drive linear mechanism 21 is fixed to the rotary cylinder 20 and configured to push the outer cylinder 38 in the Z direction.
  • a Z spring 22 is fixed at a position facing the Z drive linear mechanism 21 in the rotary cylinder 20, and the Z spring 22 is in contact with the outer cylinder 38.
  • An X drive linear mechanism 29 is attached to the rotary cylinder 20. Further, a lever mechanism 25 is attached to the rotary cylinder 20, and the lever mechanism 25 is in contact with the X drive linear mechanism 29 and the slider cylinder 30 with a fulcrum provided on the rotary cylinder 20. With this configuration, the driving force of the X drive linear mechanism 29 is transmitted to the slider cylinder 30 by the lever mechanism 25 so that the sample holder 2 can be driven in the X direction.
  • the contact portion between the lever mechanism 25 and the slider cylinder 30 includes a sliding mechanism (not shown) for the driving of the sample holder 2 in the Z-axis and Y-axis directions.
  • the X drive linear mechanism 29 is installed on the rotary cylinder 20 as the X fine movement mechanism in FIG. 2, a similar mechanism may be installed on the outer cylinder 38. In that case, since the X fine movement mechanism moves integrally with the driving in the Z-axis and Y-axis directions, the sliding mechanism is unnecessary. Although not described here, another linear mechanism capable of driving in the Y direction (direction perpendicular to the sheet of the drawing) is provided on the rotary cylinder 20 or the outer cylinder 38 to drive the sample holder 2 in the Y direction. can do.
  • the sample holder 2 is moved to the negative side in the X direction until the holder step portion 2 a of the sample holder 2 and the holder abutting portion 40 contact with each other.
  • this position is the origin of the sample moving mechanism.
  • FIG. 3 is a cross-sectional view of the transmission electron microscope (TEM) according to the first embodiment on the sample surface.
  • the mirror 1 includes a plurality of ports (openings) 11a, ..., 11e.
  • a sample stage 6, a second sample stage 7, a sample chamber evacuation port 9, a preliminary evacuation path 8, an EDX detector 10, and a cold block are provided at ports 11a to 11e of the mirror 1.
  • And 12 are provided.
  • a port 11a is provided at a position facing the sample stage 6 and on substantially the same plane as the sample 3 mounted on the sample stage 6, and the second sample stage 7 is a port 11a.
  • the EDX detector 10 is provided at a port 11 c located in the direction perpendicular to the sample holder 2 of the sample stage 6.
  • the second sample stage 7 has the same configuration as the sample stage 6 described in FIG.
  • the second sample stage 7 includes an air lock chamber (air lock mechanism) 700.
  • the air lock chamber 700 has the same configuration as the air lock chamber 600 described above, and can introduce the sample holder 701 into the mirror 1 while the mirror 1 is evacuated without releasing the mirror 1 to the atmosphere. It is.
  • the second sample stage 7 is provided in the port 11 a substantially on the same plane as the sample 3 mounted on the sample stage 6, the second sample stage 7 is a sample holder 701, which is a sample 702. Can be introduced on substantially the same plane as the sample 3 of the sample stage 6.
  • the observation sample is thinned to several tens of nm order by a focused ion beam apparatus or the like, and mounted on a sample table (not shown).
  • the sample 3 mounted on the sample table is mounted on the sample holder 2 and introduced into the mirror 1 through the air lock chamber 600 built in the sample stage 6.
  • the mirror 1 is evacuated to about 10 ⁇ 5 Pa via the sample chamber evacuation port 9.
  • the EDX detector 10 detects the characteristic X-ray and performs elemental analysis.
  • the sample 702 after observing the sample 3 of the sample stage 6, the sample 702 can be introduced into the mirror 1 by the second sample stage 7 and observation of the sample 702 can be performed following observation of the sample 3 Become. Moreover, since the second sample stage 7 includes the air lock chamber 700, and the sample 702 can be introduced through the air lock chamber 700, the sample 702 can be introduced without releasing the mirror 1 into the atmosphere. Become. This eliminates the waiting time at the time of sample exchange and shortens the sample exchange time, thereby improving the throughput of sample observation.
  • the configuration of the second sample stage 7 may be the same as that shown in FIG. 2 or, depending on the size of the one introduced via the air lock chamber 700, larger or smaller than the sample stage 6 It does not matter.
  • the sample stage 6 is mounted on the sample stage 6 at a position orthogonal to the sample holder 2.
  • the third sample stage may be mounted on substantially the same plane as the sample 3 to be processed.
  • FIG. 4 is a view for explaining a vacuum evacuation system of a transmission electron microscope (TEM) according to the first embodiment.
  • TEM transmission electron microscope
  • the transmission electron microscope 100 includes a turbo molecular pump (vacuum pumping unit) 60, a scroll pump (vacuum pumping unit) 61, and a plurality of valves 62, 63, 64, 65, 66 as a vacuum pumping system.
  • a turbo molecular pump vacuum pumping unit
  • a scroll pump vacuum pumping unit
  • valves 62, 63, 64, 65, 66 as a vacuum pumping system.
  • the sample holder 2 When the sample holder 2 is introduced into the mirror 1 from the sample stage 6, first, all the valves 62, 63, 64, 65, 66 shown in FIG. 4 are closed. Next, the sample holder 2 is introduced into the air lock chamber 600 of the sample stage 6. Next, the valve 63 is opened. Then, the air lock chamber 600 in the sample stage 6 is evacuated to about 10 Pa using the scroll pump 61. Thereafter, the valve 63 is closed and the valve 66 is opened, and the valve 62 is opened. Then, the air lock chamber 600 of the sample stage 6 is evacuated to about 10 ⁇ 4 Pa using the turbo molecular pump 60. Thereafter, the air lock valve 34 is opened to introduce the sample holder 2 into the mirror 1.
  • the sample holder 701 of the second sample stage 7 is introduced into the mirror 1, first, the sample holder 701 is introduced into the air lock chamber 700 of the second sample stage 7. Next, the valves 63, 64, 66 are closed, the valve 65 is opened, and the air lock chamber 700 is evacuated to about 10 Pa using the scroll pump 61. Thereafter, the valve 65 is closed and the valves 66 and 64 are opened. Then, the air lock chamber 700 of the second sample stage 7 is evacuated to about 10 ⁇ 4 Pa using the turbo molecular pump 60. Thereafter, the air lock valve 67 is opened to introduce the sample holder 701 into the mirror 1.
  • the two air lock chambers 600 and 700 can be evacuated using the turbo molecular pump 60 and the scroll pump 61.
  • FIG. 5 is a view for explaining a stage control system of a transmission electron microscope (TEM) according to the first embodiment.
  • the transmission electron microscope 100 includes a main control unit 57, a first stage controller 53, and a second stage controller 58 as a control system.
  • the main control unit 57 is configured by an information processing apparatus such as a personal computer or a work station.
  • the main control unit 57 includes a central processing unit such as a CPU (Central Processing Unit), a memory, a hard disk (storage device), an input device such as a keyboard, and an output device such as a display.
  • the main control unit 57 controls the entire transmission electron microscope 100.
  • the main control unit 57 can capture a signal detected by the detector 55 to form an image and display the image on an output device.
  • the first stage controller 53 is connected to the main control unit 57 and to an actuator (not shown) that drives the sample stage 6.
  • the first stage controller 53 includes a track ball 56, and the driving of the sample stage 6 is performed by the operator of the electron microscope operating the track ball 56.
  • the second stage controller 58 is connected to the main control unit 57 and to an actuator (not shown) for driving the second sample stage 7.
  • the second stage controller 58 includes a track ball 59, and driving of the second sample stage 7 is performed by the electron microscope operator operating the track ball 59.
  • the first and second stage controllers 53 and 58 and the track balls 56 and 59 are provided for each of the sample stages 6 and 7, but the sample stage 6 and the track balls are one stage controller and one track ball. It is also possible to control the second sample stage 7. In that case, a changeover switch or the like may be provided between the stage controller and the sample stage 6 and the second sample stage 7.
  • FIG. 6A is a top view of the outer cylinder 38 of the sample stage 6 of the transmission electron microscope (TEM) according to the first embodiment.
  • the sample holder 2 is provided with a guide pin 5.
  • the guide pin 5 moves along the holder guide groove 39 provided in the inner cylinder 33 and the outer cylinder 38, whereby the sample holder 2 can be introduced to the observation position.
  • the holder guide groove 39 has a crank shape.
  • the state where the guide pin 5 is located at the position “A” in FIG. 6A is the position where the air lock chamber 600 is evacuated.
  • the state in which the guide pin 5 is at the position “B” in FIG. 6A is a state in which the sample 3 is introduced into the mirror 1 but not at the sample observation position.
  • the state in which the guide pin 5 is at the position “C” in FIG. 6A is the state in which the sample 3 is at the sample observation position.
  • the gate 101 for closing the holder guide groove 39 is provided at a position between "A” and “C”.
  • the gate 101 is provided at the position of “B”, and the guide pin 5 is controlled to stop at the position of “B”.
  • the gate 101 is provided at a position between “A” and “C” on the upper surface of the outer cylinder 28.
  • FIG. 6B is a cross-sectional view of the transmission electron microscope (TEM) according to the first embodiment on the sample surface.
  • the transmission electron microscope 100 includes an area sensor light emitting unit 120 and an area sensor light receiving unit 121 on substantially the same plane as the sample 3.
  • the area sensor light emitting unit 120 and the area sensor light receiving unit 121 are disposed to face each other.
  • the area sensor of this embodiment is a transmission type sensor having an area sensor light emitting unit 120 and an area sensor light receiving unit 121 on the opposite surface thereof.
  • the sample holder 2 of the sample stage 6 or the sample holder 701 of the second sample stage 7 is an electron beam irradiation position (sample observation position) It is possible to detect the presence of
  • the transmission type sensor is used in the example of FIG. 6B
  • a reflection type sensor in which a light receiving unit is built in the area sensor light emitting unit 120 may be used.
  • FIGS. 6A and 6B in the configuration in which the plurality of sample holders 2 and 701 are introduced from the plurality of sample stages 6 and 7, it is possible to prevent the sample holders from colliding and breaking. Become.
  • the configuration for introducing the sample holder 701 from the second sample stage 7 has been described, but instead of the sample holder 701, components used for observation and analysis in a cylindrical member having the same shape as the sample holder 701 (for example, Detectors, apertures, cold blocks, etc.) can be attached to introduce those components from the second sample stage 7 into the mirror 1. Specific examples will be described below.
  • FIG. 7 is a view for explaining the second sample stage 7 of the transmission electron microscope (TEM) according to the second embodiment.
  • the second sample stage 7 includes a cylindrical member 703 that can be introduced into the mirror 1, and the tip of the cylindrical member 703 includes an EDX detector 704.
  • the EDX detector 704 is introduced into the mirror 1 through the air lock chamber 700.
  • the sample holder 2 is inserted between the gap between the top and the bottom of the objective pole piece 105.
  • the electron beam 107 is focused by the magnetic field generated by the objective pole piece 105.
  • the EDX detector 704 is a pole piece insertion type EDX detector, and is configured to be inserted between the upper objective pole piece 105 and the sample holder 2.
  • the EDX detector 704 may be a detector of a type that detects characteristic X-rays from the side surface of the objective pole piece 105.
  • an EDX detector equipped with a large-area X-ray detection element has been commercialized for the purpose of improving analysis sensitivity.
  • an EDX detector can be introduced from the second sample stage 7 different from the sample stage 6.
  • the EDX detector 704 can be replaced and introduced via the air lock chamber 700 without releasing the mirror 1 to the atmosphere. This makes it possible to significantly reduce the time required for replacement and maintenance of the detector, and improves the throughput of sample observation.
  • the sample holder has a cylindrical shape of about 10 mm ⁇ , and mounting the detector or the like inside the sample holder is very difficult There are many cases. According to this embodiment, it is not necessary to mount the detector on the sample holder itself, and the EDX detector 704 can be introduced from the second sample stage 7 different from the sample stage 6.
  • FIG. 8 is a view for explaining the second sample stage 7 of the transmission electron microscope (TEM) according to the third embodiment.
  • the second sample stage 7 includes a cylindrical member 703 which can be introduced into the mirror 1, and the tip of the cylindrical member 703 includes a gas introduction nozzle 705.
  • the gas introduction nozzle 705 is introduced into the mirror 1 through the air lock chamber 700. According to this embodiment, it is possible to spray a gas on the sample 3 introduced from the sample stage 6 by the gas introduction nozzle 705 introduced from the second sample stage 7 and to observe the reaction by TEM.
  • a pipe 151 for supplying gas is mounted on the sample holder 150, and the gas is sprayed to the sample 152 through the pipe 151.
  • a sample holder 150 it is necessary to mount the pipe 151 on the sample holder 150 itself, and it is difficult to spray gas on any sample mounted on any holder.
  • the gas introduction nozzle 705 can be introduced to any sample through the air lock chamber 700 of the second sample stage 7 different from the sample stage 6 .
  • the gas introduction nozzle 705 can be introduced without releasing the mirror 1 to the atmosphere, the time taken for sample observation can be shortened, and the throughput of the sample observation can be improved.
  • FIGS. 9A and 9B are diagrams for explaining the second sample stage 7 of the transmission electron microscope (TEM) according to the fourth embodiment.
  • FIG. 9A is a side view of a sample surface of a transmission electron microscope
  • FIG. 9B is a cross-sectional view of a cold block.
  • the sample holder is provided with a refrigerant (liquid nitrogen) tank, and the sample is cooled by removing the heat of the sample by good heat conduction conducted to the vicinity of the sample.
  • a member (cold block) cooled around the sample may be installed to reduce radiation heat to the sample. There is.
  • the second sample stage 7 includes a cylindrical member 703 which can be introduced into the mirror 1, and the tip of the cylindrical member 703 includes a cold block 706. Further, a refrigerant (liquid nitrogen) tank (not shown) is attached to the other end of the cylindrical member 703. The cylindrical member 703 is introduced into the mirror 1 through the air lock chamber 700.
  • the cold block 706 is formed in a cylindrical shape so that the sample 3 of the sample holder 2 is introduced into the internal space.
  • the cold block 706 has a hole 706 a for passing the electron beam 107. Therefore, it is possible to irradiate the sample 3 with the electron beam 107 while covering the whole of the sample 3 by the cold block 706.
  • the cold block 706 may be introduced to an arbitrary sample via the air lock chamber 700 of the second sample stage 7 different from the sample stage 6 according to the need for cooling. It becomes possible. Therefore, it is possible to make effective use of vacant ports without the cold block occupying one port. Furthermore, in the present embodiment, since the cold block 706 is introduced from another second sample stage 7 located at a position facing the sample stage 6, the cold block 706 is formed in a cylindrical shape. It becomes possible to cover the whole. Therefore, the cooling efficiency of the sample 3 is also improved.
  • the cold block needs to be disposed in the vicinity of the sample holder, and may collide with the sample holder or the like to be broken, and it is necessary to open the mirror to the atmosphere for maintenance.
  • the cold block 706 since the cold block 706 is formed in a cylindrical shape to cover the sample 3 from the periphery, it is possible to avoid a collision with the sample holder 2 .
  • the cold block 706 since the cold block 706 is introduced into the mirror 1 through the air lock chamber 700, maintenance of the cold block 706 is also possible without opening the mirror to the atmosphere.
  • FIG. 10 is a view for explaining the second sample stage 7 of the transmission electron microscope (TEM) according to the fifth embodiment.
  • TEM transmission electron microscope
  • the second sample stage 7 includes a cylindrical member 703 which can be introduced into the mirror 1, and the tip of the cylindrical member 703 includes an aperture unit (TEM aperture) 707.
  • the aperture unit 707 is introduced into the mirror 1 through the air lock chamber 700.
  • the aperture unit 707 has the same shape as the sample holder 2 and has apertures 111 and 112 of different diameters.
  • either of the diaphragms 111 and 112 having different diameters can be disposed immediately below the sample 3.
  • the diaphragm unit 707 can be introduced from the second sample stage 7 only at the time of TEM observation with respect to the sample 3 introduced from the sample stage 6.
  • the diaphragm unit 707 is a mirror through the air lock chamber 700. As it is introduced into the housing 1, maintenance of the diaphragm unit 707 becomes possible without opening the mirror 1 to the atmosphere.
  • the TEM aperture is fixed to the mirror, and one port of the mirror is occupied by the TEM aperture.
  • the TEM aperture was unnecessary except at the time of TEM observation (STEM observation), and the port could not be used effectively.
  • STEM observation TEM observation
  • FIG. 11 is a view for explaining the second sample stage 7 of the transmission electron microscope (TEM) according to the sixth embodiment.
  • TEM transmission electron microscope
  • the second sample stage 7 includes a cylindrical member 703 which can be introduced into the mirror 1, and the tip of the cylindrical member 703 includes a plasma cleaner 708.
  • the plasma cleaner 708 is introduced into the mirror 1 through the air lock chamber 700. According to this embodiment, the plasma cleaner 708 can be introduced from the second sample stage 7 to the sample 3 introduced from the sample stage 6. After the introduction, the plasma cleaner 708 irradiates plasma to the sample 3 introduced from the sample stage 6.
  • the hydrocarbon-based gas in the atmosphere is adsorbed there, and the effect of the plasma irradiation is reduced.
  • the plasma cleaner 708 can be introduced through the air lock chamber 700 without releasing the mirror 1 to the atmosphere, the effect of the plasma irradiation can be maintained without exposing the sample to the atmosphere after the plasma irradiation.
  • FIG. 12 is a view of the sample surface as viewed from above, and FIG. 13 is an enlarged view of a sample stage.
  • TEM transmission electron microscope
  • the tip of the sample holder 2 of the sample stage 6 includes the sample rotation holder 76
  • the tip of the sample holder 701 of the second sample stage 7 includes the sample rotation holder 71.
  • the sample rotation holders 71 and 76 are formed in such a shape that they do not interfere with each other when they are simultaneously introduced to the irradiation position of the electron beam.
  • the tip end portions of the sample rotation holders 71 and 76 are L-shaped in top view.
  • the sample rotation holder 76 has a bevel gear 74 having a sample table 80 and a bevel gear 75 having a rotation shaft 77. As shown in FIG. 13, the sample holder 80 holds a sample 82 for sample rotation holder.
  • the bevel gear 74 and the bevel gear 75 are disposed to mesh with each other, and when the bevel gear 75 is rotated by the rotation shaft 77, the bevel gear 74 in contact with the bevel gear 75 is rotated, and as a result, the sample of the sample table 80 82 can be rotated.
  • the sample rotation holder 71 also has a bevel gear 72 having a sample stage 79 and a bevel gear 73 having a rotation shaft 78. As shown in FIG. 13, the sample holder 79 holds a sample 81 for sample rotation holder.
  • the bevel gear 72 and the bevel gear 73 are disposed so as to mesh with each other. When the bevel gear 73 is rotated by the rotation shaft 78, the bevel gear 72 in contact with the bevel gear 73 is rotated, and as a result, the sample of the sample table 79 81 can be rotated.
  • the bevel gear 72 having the sample table 79 and the bevel gear 74 having the sample table 80 are disposed to face each other across the irradiation position of the electron beam.
  • the sample 81 is mounted on the tip of the sample stage 79
  • the sample 82 is mounted on the tip of the sample stage 80. Therefore, the sample 81 of the sample table 79 and the sample 82 of the sample table 80 are both arranged in the beam irradiation area.
  • the sample rotation holders 71 and 76 are sufficiently separated at the time of sample introduction (e.g., separated by about several hundred microns within the low magnification observation field of the electron microscope). 71 and 76 are introduced to avoid holder interference at the time of sample holder introduction. Further, the sample stage 6 and the second sample stage 7 are controlled such that the respective samples 81 and 82 approach a desired distance in a state where the observation field of view is about 100 ⁇ m. Alternatively, the sample 81 introduced from the second sample stage 7 may be fixed, and the sample stage 6 may be operated to bring each sample to a desired position.
  • the sample 81 introduced from the second sample stage 7 by using the sample 82 introduced from the sample stage 6 as a reference sample.
  • the sample rotation holders 71 and 76 are introduced into the mirror 1 through the air lock chambers 600 and 700, respectively, the samples 81 and 82 are simultaneously introduced into the beam irradiation area without opening the mirror 1 to the atmosphere. It is possible to This improves the throughput of sample observation.
  • the mirror 1 is It is possible to introduce a sample to be observed next without opening to the atmosphere.
  • components such as a detector and an aperture mechanism
  • the components used for observation and analysis can be introduced in a state where the mirror 1 is in a vacuum without releasing the mirror 1 to the atmosphere, observation throughput is improved.
  • the present invention is not limited to the embodiments described above, but includes various modifications.
  • the embodiments described above are described in detail to explain the present invention in an easy-to-understand manner, and are not necessarily limited to those having all the configurations described.
  • a part of the configuration of one embodiment may be replaced with the configuration of another embodiment, and the configuration of another embodiment may be added to the configuration of one embodiment.
  • control lines and information lines in the drawings indicate what is considered necessary for explanation, and not all control lines and information lines in the product are necessarily shown. All configurations may be connected to each other.

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  • Analysing Materials By The Use Of Radiation (AREA)
PCT/JP2013/078807 2012-10-31 2013-10-24 電子ビーム顕微装置 Ceased WO2014069325A1 (ja)

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JP6421041B2 (ja) * 2015-01-13 2018-11-07 株式会社日立ハイテクノロジーズ 荷電粒子線装置
US11152189B2 (en) * 2020-03-18 2021-10-19 Fei Company Method and system for plasma assisted low vacuum charged-particle microscopy
DE112021007286T5 (de) * 2021-05-17 2024-01-25 Hitachi High-Tech Corporation Probenhalter und analysesystem
JP2023051864A (ja) * 2021-09-30 2023-04-11 エフ イー アイ カンパニ モジュール式超高真空電子顕微鏡

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JPH04306547A (ja) * 1991-04-02 1992-10-29 Fujitsu Ltd 電子顕微鏡用試料ホルダおよび真空装置用ロードロック機構
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