WO2014080987A1 - 荷電粒子線装置、試料台ユニット、及び試料観察方法 - Google Patents
荷電粒子線装置、試料台ユニット、及び試料観察方法 Download PDFInfo
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- WO2014080987A1 WO2014080987A1 PCT/JP2013/081411 JP2013081411W WO2014080987A1 WO 2014080987 A1 WO2014080987 A1 WO 2014080987A1 JP 2013081411 W JP2013081411 W JP 2013081411W WO 2014080987 A1 WO2014080987 A1 WO 2014080987A1
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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
- H01J37/16—Vessels; Containers
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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 objects or the material; Means for adjusting diaphragms or lenses associated with the support
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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
- H01J37/224—Luminescent screens or photographic plates for imaging ; Apparatus specially adapted therefor, e.g. cameras, TV-cameras, photographic equipment, exposure control; Optical subsystems specially adapted therefor, e.g. microscopes for observing image on luminescent screen
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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
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2002—Controlling environment of sample
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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
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2002—Controlling environment of sample
- H01J2237/2003—Environmental cells
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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
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2002—Controlling environment of sample
- H01J2237/2003—Environmental cells
- H01J2237/2004—Biological samples
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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
- H01J2237/2602—Details
- H01J2237/2605—Details operating at elevated pressures, e.g. atmosphere
- H01J2237/2608—Details operating at elevated pressures, e.g. atmosphere with environmental specimen chamber
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
Definitions
- the present invention relates to a charged particle beam apparatus that can be observed in a predetermined gas atmosphere at atmospheric pressure or a slightly negative pressure state from atmospheric pressure.
- a scanning electron microscope (SEM), a transmission electron microscope (TEM), or the like is used.
- SEM scanning electron microscope
- TEM transmission electron microscope
- a housing for placing a sample is evacuated and the sample atmosphere is evacuated to image the sample.
- biochemical samples, liquid samples, and the like are damaged or changed in state by vacuum.
- an SEM device, a sample holding device, and the like that can observe an observation target sample at atmospheric pressure have been developed.
- these devices provide a diaphragm capable of transmitting an electron beam between an electron optical system and a sample to partition a vacuum state and an atmospheric state, and both of them provide a diaphragm between the sample and the electron optical system.
- a diaphragm capable of transmitting an electron beam between an electron optical system and a sample to partition a vacuum state and an atmospheric state, and both of them provide a diaphragm between the sample and the electron optical system.
- an electron source side of an electron optical column is disposed downward and an objective lens side is disposed upward, and an electron beam is placed on an electron beam exit hole at the end of the electron optical column via an O-ring.
- An SEM provided with a diaphragm that can pass through is disclosed.
- a liquid containing an observation target sample is placed directly on a diaphragm, a primary electron beam is irradiated from the lower surface of the sample, and reflected electrons or secondary electrons are detected to perform SEM observation.
- the sample is held in a space constituted by an annular member and a diaphragm installed around the diaphragm, and the space is filled with a liquid such as water.
- the sample surface is not parallel to the diaphragm due to surface tension in the natural state. Observation is not possible unless they are brought close to each other until they come into contact with each other, and the diaphragm needs to be replaced every time the sample is replaced.
- the present invention has been made in view of such a problem, and provides a sample observation method and a charged particle beam apparatus capable of exchanging a sample placed at an atmospheric pressure or an atmosphere at a pressure of the same pressure at a high throughput.
- the purpose is to provide.
- the present invention provides a space between a first diaphragm capable of maintaining an airtight state of a case to be evacuated and transmitting or passing the primary charged particle beam, and the sample. Further, the first charged particle beam is provided with a second diaphragm that can pass through or pass through the primary charged particle beam, and the sample is irradiated with the primary charged particle beam through the second diaphragm.
- the present invention it is possible to provide a sample observation method and a charged particle beam apparatus capable of exchanging a sample placed in an atmosphere having an atmospheric pressure or a pressure of the same level with a high throughput.
- FIG. 1 is an overall configuration diagram of a charged particle microscope according to Embodiment 1.
- FIG. Detailed view of sample loading method. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed drawing of a contact prevention member. Detailed view of the vicinity of the diaphragm, sample, and detector. Configuration example of diaphragm, sample, sample stage. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. Detailed view of the vicinity of the diaphragm, sample, and detector. FIG.
- FIG. 3 is an overall configuration diagram of a charged particle microscope according to a second embodiment.
- FIG. 5 is an overall configuration diagram of a charged particle microscope according to a third embodiment.
- FIG. 5 is an overall configuration diagram of a charged particle microscope according to a third embodiment.
- FIG. 6 is an overall configuration diagram of a charged particle microscope according to a fourth embodiment.
- a charged particle beam microscope will be described as an example of a charged particle beam apparatus.
- this is merely an example of the present invention, and the present invention is not limited to the embodiments described below.
- the present invention can also be applied to a scanning electron microscope, a scanning ion microscope, a scanning transmission electron microscope, a combined device of these and a sample processing device, or an analysis / inspection device to which these are applied.
- atmospheric pressure means an atmospheric atmosphere or a predetermined gas atmosphere, and means a pressure environment of atmospheric pressure or a slight negative pressure state. Specifically, the pressure is about 10 5 Pa (atmospheric pressure) to about 10 3 Pa.
- FIG. 1 shows an overall configuration diagram of the charged particle microscope of the present embodiment.
- the charged particle microscope shown in FIG. 1 mainly includes a charged particle optical column 2, a casing (vacuum chamber) 7 connected to and supporting the charged particle optical column 2, and a sample stage 5 arranged in an atmospheric atmosphere. And a control system for controlling them.
- the charged particle microscope When the charged particle microscope is used, the charged particle optical column 2 and the inside of the first housing are evacuated by the vacuum pump 4.
- the start / stop operation of the vacuum pump 4 is also controlled by the control system.
- only one vacuum pump 4 is shown in the figure, two or more vacuum pumps may be provided. It is assumed that the charged particle optical column 2 and the housing 7 are supported by a base 270 such as a pillar (not shown).
- the charged particle optical column 2 includes an element such as a charged particle source 8 that generates a charged particle beam, an optical lens 1 that focuses the generated charged particle beam and guides it to the lower part of the column and scans the sample 6 as a primary charged particle beam. Consists of.
- the charged particle optical column 2 is installed so as to protrude into the housing 7 and is fixed to the housing 7 via a vacuum sealing member 123.
- a detector 3 for detecting secondary charged particles (secondary electrons or reflected electrons) obtained by irradiation with the primary charged particle beam is disposed at the end of the charged particle optical column 2.
- the charged particle microscope of the present embodiment has a control system such as a computer 35 used by the user of the apparatus, a host controller 36 connected to the computer 35 for communication, and a vacuum pumping system and a charge according to a command transmitted from the host controller 36.
- a lower control unit 37 that controls the particle optical system and the like is provided.
- the computer 35 includes a monitor on which an operation screen (GUI) of the apparatus is displayed, and input means for an operation screen such as a keyboard and a mouse.
- GUI operation screen
- the upper control unit 36, the lower control unit 37, and the computer 35 are connected by communication lines 43 and 44, respectively.
- the lower control unit 37 is a part that transmits and receives control signals for controlling the vacuum pump 4, the charged particle source 8, the optical lens 1, and the like, and further converts the output signal of the detector 3 into a digital image signal to perform higher control. It transmits to the part 36.
- the output signal from the detector 3 is connected to the lower control unit 37 via an amplifier 154 such as a preamplifier. If an amplifier is not necessary, it may not be necessary.
- the upper control unit 36 and the lower control unit 37 may include a mixture of analog circuits, digital circuits, etc., and the upper control unit 36 and the lower control unit 37 may be unified.
- the configuration of the control system shown in FIG. 1 is merely an example, and modifications of the control unit, valve, vacuum pump, communication wiring, and the like can be applied to the SEM of this embodiment as long as the functions intended in this embodiment are satisfied. It belongs to the category of charged particle beam equipment.
- the housing 7 is connected to a vacuum pipe 16 having one end connected to the vacuum pump 4 so that the inside can be maintained in a vacuum state.
- a leak valve 14 for opening the inside of the housing to the atmosphere is provided, and the inside of the housing 7 can be opened to the atmosphere during maintenance.
- the leak valve 14 may not be provided, and may be two or more. Further, the arrangement location of the leak valve 14 in the housing 7 is not limited to the location shown in FIG. 1, and may be arranged at another position on the housing 7.
- a first diaphragm 10 is provided at a position directly below the charged particle optical column 2 on the lower surface of the housing.
- the first diaphragm 10 can transmit or pass the primary charged particle beam emitted from the lower end of the charged particle optical column 2, and the primary charged particle beam passes through the first diaphragm 10 and is finally passed through.
- the sample 6 mounted on the sample stage 52 is reached.
- the closed space formed by the first diaphragm 10 can be evacuated. Therefore, in this embodiment, the airtight state of the space evacuated by the first diaphragm 10 is maintained, so that the charged particle optical column 2 can be maintained in a vacuum state and the sample 6 is maintained at atmospheric pressure for observation. can do. Further, the sample 6 can be freely exchanged during observation.
- the first diaphragm 10 is formed or deposited on the base 9.
- the first diaphragm 10 is a carbon material, an organic material, a metal material, silicon nitride, silicon carbide, silicon oxide, or the like.
- the base 9 is a member such as silicon or a metal member.
- the first diaphragm 10 may be a plurality of windows arranged in plural.
- the thickness of the diaphragm capable of transmitting or passing the primary charged particle beam is about several nm to several ⁇ m.
- the first diaphragm must not break under the differential pressure to separate atmospheric pressure and vacuum. Therefore, the area of the first diaphragm 10 is about several tens ⁇ m to at most several mm.
- the shape of the first diaphragm 10 is not square but may be a rectangle or the like. Any shape may be used.
- the base 9 that supports the first diaphragm 10 is provided on the diaphragm holding member 155. Although not shown, it is assumed that the base 9 and the diaphragm holding member 155 are bonded by an adhesive capable of vacuum sealing, a double-sided tape, or the like.
- the diaphragm holding member 155 is detachably fixed to the lower surface side of the housing 7 via a vacuum sealing member 124.
- the first diaphragm 10 is very thin with a thickness of about several nanometers to several micrometers or less because of the requirement that the charged particle beam permeates, and therefore, the first diaphragm 10 may be deteriorated with time or damaged during observation preparation.
- the first diaphragm 10 and the base 9 that supports the first diaphragm 10 are small, it is very difficult to handle them directly. Therefore, as in this embodiment, the first diaphragm 10 and the base 9 are integrated with the diaphragm holding member 155 so that the base 9 can be handled via the diaphragm holding member 155 instead of directly. Handling (especially replacement) of the diaphragm 10 and the base 9 becomes very easy. That is, when the first diaphragm 10 is damaged, the entire diaphragm holding member 155 may be replaced. Even if the first diaphragm 10 must be replaced directly, the diaphragm holding member 155 is taken out of the apparatus, Exchange for every first diaphragm 10 or base 9 can be performed outside the apparatus.
- a sample stage 5 arranged in an air atmosphere is provided below the first diaphragm 10 provided in the housing 7.
- the sample stage 5 is provided with a Z-axis drive mechanism having a height adjusting function capable of causing at least the sample 6 to approach the diaphragm 10.
- an XY drive mechanism that moves in the sample plane direction may be provided.
- a base 51 on which the sample 6 can be mounted and the second diaphragm 50 is provided is disposed between the first diaphragm 10 and the sample stage 5, a base 51 on which the sample 6 can be mounted and the second diaphragm 50 is provided is disposed.
- the sample 6 and the second diaphragm 50 are disposed on a sample stage on the sample stage 5.
- the second diaphragm 50 is supported by a base 51.
- the surface (observation surface) of the sample 6 placed on the sample stage 5 is covered with the second diaphragm 50. That is, the primary charged particle beam is irradiated in a state where the sample is in contact with the surface of the second diaphragm 50 on the sample table side (the surface opposite to the surface facing the first diaphragm).
- the 2nd diaphragm 50 is comprised so that a charged particle beam can permeate
- sample stage unit The sample stage, base, second diaphragm and the like are collectively referred to as a sample stage unit, but the “sample stage unit” may be composed of only a part of them.
- a suitable sample 6 is a sample containing a liquid.
- a sample containing a liquid such as an aqueous solution, an organic solvent, oil, sol, gel, or jelly.
- a biological or biosample such as cells, bacteria, blood cells, and viruses.
- nano / micro fine particles such as organic substances and metals, and nanowires are mixed.
- a sample is “liquid” or “liquid”, as mentioned in the above example, it is a general term for a sample having no regularity, that is, a sample other than a sample having a solid surface. . In the following, such a liquid sample will be described as an observation object unless otherwise specified.
- the first diaphragm 10 If the first diaphragm 10 is accidentally contacted, there is a risk that the first diaphragm 10 is broken and the sample 6 enters the housing 7 that is in a vacuum state. In order to solve these problems, it can be solved by extending the liquid thinly, but in this case, the sample containing the liquid starts to dry. On the other hand, in the method of disposing the second diaphragm 50 in the present embodiment, it is possible to reduce the drying by the diaphragm through which the charged particle beam can be transmitted to the maximum, and the liquid droplet shape is forced. Since it can be made flat, it is possible to bring the sample near the first diaphragm very easily and with high throughput.
- FIG. 2 shows a sample arrangement method using the second diaphragm 50.
- the sample shape becomes flat along the diaphragm surface. That is, after the sample 6 containing the liquid disposed on the sample stage 52 is mounted by dropping or the like as shown in FIG. 2A, the sample 6 is mounted immediately below the second diaphragm 50 as shown in FIG.
- the base 51 provided with the second diaphragm 50 may be mounted as described. Thereby, the sample is held in the space formed by the second diaphragm 50, the base 51, and the sample table 52, and the upper surface (irradiated surface of the primary charged particle beam) of the sample 6 containing the liquid can be flattened.
- a hydrophilic material may be applied or vapor-deposited in order to enhance the adhesion of the sample containing the liquid to the lower surface of the second diaphragm 50 or the sample stage 52 in the drawing. Thanks to the second diaphragm 50, the observation surface of the liquid sample is forced to be flat, so that the first diaphragm 10 and the second diaphragm 50 are likely to be close to each other.
- the base 51 may have a thickness of about several millimeters, or may be a very thin foil such as several hundreds of nanometers. Any thickness can be used as long as the second diaphragm 50 can maintain its shape. Further, as described above, the base 51 may be omitted as long as the shape of the sample can be controlled.
- the alignment of the optical axis 53 of the charged particle optical column and the central axis 54 of the first diaphragm can be performed by moving the diaphragm holding member 155 in the horizontal direction or the vertical direction in the drawing. This movement may be performed by using any jig or by hand.
- the central axis 54 of the first diaphragm is exactly the optical axis 53 of the charged particle optical column. You may make it fit.
- the center axis 54 of the first diaphragm and the center axis 55 of the second diaphragm can be aligned by operating the sample stage 5 having an XY drive mechanism for holding the second diaphragm.
- the primary charged particle beam emitted from the charged particle optical column is irradiated to the first diaphragm 10 from the inner space 11 side of the housing 7.
- the primary charged particle beam passes through or passes through the diaphragm.
- the primary charged particle beam that has passed through or passed through the first diaphragm 10 passes over the atmospheric space between the first diaphragm 10 and the second diaphragm 50.
- Charged particle beams are scattered by atmospheric space.
- the mean free path of the charged particle beam in the atmosphere depends on the energy of the charged particle beam, but is about several ⁇ m to 1 mm or less.
- the distance between the first diaphragm 10 and the second diaphragm 50 should be as small as possible.
- the approach of the first diaphragm 10 and the second diaphragm 50 can be made closer by the Z-axis operation of the sample stage 5.
- the primary charged particle beam is applied to the second diaphragm 50.
- the second diaphragm 50 is thin enough to transmit the primary charged particle beam, and is specifically about several nm to several ⁇ m. Further, since the second diaphragm 50 does not need to separate the atmospheric pressure and the vacuum, it does not need to be as strong as the first diaphragm 10. Therefore, the second diaphragm 50 is thinner than the first diaphragm 10, and the window area can be increased. If the window area of the second diaphragm is larger than the window area of the first diaphragm 10, the entire sample 6 cannot be seen from the charged particle optical column side, but the XY drive mechanism of the sample stage can be moved.
- the sample 6 immediately below the second diaphragm can be observed anywhere.
- the positional relationship between the first diaphragm 10 and the second diaphragm 50 can be changed in a non-contact state.
- a plurality of second diaphragms 50 are arranged in the vertical direction (for example, directly below) of the windows of the first diaphragm 10, and the windows of the first diaphragm 10 are used to simultaneously observe a plurality of samples.
- the window area of the second diaphragm 50 may be made smaller than the area.
- the primary charged particle beam that has passed through or passed through the first diaphragm 10 is simultaneously irradiated to some or all of the plurality of second diaphragms 50. Accordingly, if the sample stage on which the second diaphragm and the sample to be observed are placed within the field of view of the window of the first diaphragm 10, a plurality of samples can be observed within the same field of view.
- the “window” refers to a region through which the primary charged particle beam passes or transmits.
- the charged particle beam transmitted or passed through the second diaphragm 50 is irradiated onto the sample 6 to generate secondary charged particles such as secondary electrons and reflected electrons.
- the secondary charged particles can be detected by the detector 3 in the housing 7.
- this detector does not necessarily have to be in the housing 7 and may be in the atmospheric space in the vicinity of the first diaphragm 10.
- a detector capable of detecting these photon beams is used as an atmosphere in the vicinity of the housing 7 and the first diaphragm 10. It may be in space. Also.
- the secondary charged particle or photon detector may be directly under the sample 6.
- the scattering probability of charged particle beams is proportional to the mass number and density of gas molecules. Therefore, gas molecules having a lighter mass number than the atmosphere may be disposed between the first diaphragm 10 and the second diaphragm 50.
- the type of the replacement gas if the gas is lighter than the atmosphere, such as nitrogen or water vapor, the effect of improving the image S / N can be seen, but helium gas or hydrogen gas having a lighter mass has a better image S / N. Great improvement effect.
- the liquid sample 6 is covered with the second diaphragm, so that it becomes easy to approach the first diaphragm. Even if the sample 6 is brought close to the first diaphragm 10, the sample and the first diaphragm are not in direct contact because the second diaphragm 50 exists between the sample 6 and the first diaphragm 10. For this reason, it is possible to perform sample exchange easily and with high throughput without removing the first diaphragm between the vacuum and the atmospheric space.
- a detector 59 capable of detecting the charged particle beam transmitted through the sample 6 is provided on the opposite side of the second diaphragm 50 of the sample 6.
- the detector 59 is a detection element that can detect and amplify a charged particle beam that comes in with an energy of several keV to several tens of keV.
- a semiconductor detector made of a semiconductor material such as silicon, a scintillator capable of converting a charged particle signal into light on or inside a glass surface, a luminescent light emitting material, a YAG (yttrium aluminum garnet) element, etc. It is.
- a signal from the detector 59 is transmitted to the preamplifier 61 via the wiring 60.
- a signal from the preamplifier 61 is sent to the lower control unit 37 via a wiring (not shown) and used as an image forming signal.
- the preamplifier is arranged in the atmospheric space in the figure, it may be provided in the housing 7 or the sample stage 5. If the detector 59 is a detection element that converts a charged particle signal into light, the wiring 60 is an optical transmission line, and the preamplifier 61 is an photoelectric signal amplifier that can amplify the optical signal into an electrical signal.
- FIG. 5 a configuration having a contact preventing member for preventing the diaphragm from being damaged when the first diaphragm 10 and the second diaphragm 50 (or the diaphragm and the foundation thereof) are in contact with each other. Will be described. In the figure, only the vicinity of each diaphragm is shown, and the charged particle optical column 2 and the housing 7 are omitted.
- FIG. 5A shows a state in which the contact preventing member 56 is provided in the vicinity of the second diaphragm 50.
- the contact preventing member 56 may be around the diaphragm or may be disposed somewhere on the diaphragm.
- the contact preventing member 56 can be manufactured by forming a film or vapor deposition when the second diaphragm 50 is manufactured. Examples of the material include an organic film and a metal film. The thickness is about several tens of nm to 100 ⁇ m or less. Although the contact preventing member 56 is provided on the second diaphragm 50 in the drawing, it may be on the first diaphragm 10 side or both. The contact prevention member 56 limits the minimum proximity distance between the first diaphragm 10 and the second diaphragm 50, and can prevent the diaphragms from approaching each other beyond this distance.
- a foil material whose thickness is known may be disposed on the first diaphragm 10 or the second diaphragm 50 later.
- a foil material whose thickness is known may be disposed on the first diaphragm 10 or the second diaphragm 50 later.
- an aluminum foil or the like is disposed in the vicinity of the first diaphragm 10 or the second diaphragm 50. Since the foil material can be mounted after the diaphragm 10 and the diaphragm 50 are manufactured, the thickness and material of the contact preventing member 56 can be easily changed later.
- FIG. 5B shows a state where the contact preventing member 57 is mounted on the sample stage 52.
- the contact preventing member 57 hits the diaphragm holding member 155, so that the diaphragms do not contact each other.
- the contact preventing member 57 is, for example, a male screw, and the sample stage 52 is provided with a female screw, so that it can be attached.
- the contact preventing member 57 is mounted on the sample stage 52, but may be provided in the diaphragm holding member 155 or in both of them.
- a rotating ball bearing 58 may be disposed at the tip of the contact prevention member 57 as shown in FIG. In this case, the ball bearing 58 comes into contact with the diaphragm holding member 155.
- the sample can be moved in the horizontal direction or the paper surface direction in the figure with the contact prevention member 57 in contact with the diaphragm holding member 155.
- the charged particle optical column is placed on the sample stage while the distance between the sample stage and the diaphragm holding member 155 (or the distance between the sample surface and the diaphragm) is constantly limited by the contact preventing member 57.
- the structure can be driven in the direction perpendicular to the optical axis, it is not limited to a ball bearing.
- This member is referred to as a fine adjustment member.
- the fine adjustment member may not be a ball bearing.
- a material having a small friction coefficient among organic substances such as a fluororesin represented by polytetrafluoroethylene may be used, and the contact prevention member 57 and the diaphragm holding member 155 are reduced by reducing the contact area as much as possible. You may improve the slip.
- the sample stage 5 has an automatic transfer function, the throughput is further increased.
- an automatic transfer function for example, in order to automatically transfer a desired second diaphragm 50 under the first diaphragm 10, the sample stage 5 is provided with an automatic transfer mechanism such as an electric motor.
- FIG. 6 shows a state in which the second diaphragm 50 is arranged only in the horizontal direction in the drawing, but the second diaphragm is two-dimensionally two-dimensionally on the sample stage 52 as shown in FIG.
- a plurality of the diaphragms 50 may be arranged.
- the base 51 is common, and there may be a plurality of the second diaphragm 50 and the sample 6 alone.
- FIG. 7B since there are a plurality of sample mounting portions as shown in FIG. 7C when viewed from the lower surface side of the base 51 in the drawing, it is possible to mount the sample 6 very efficiently. Become. In this case, the sample may be placed on each diaphragm in the state of FIG.
- the base 51 may be turned over, and placed on the sample table 52. By doing so, the sample can be confined between the sample stage 52 and the second diaphragm 50.
- a liquid leakage prevention member such as rubber (not shown) may be disposed between the sample stage 52 and the base 51.
- the contact prevention member 56 and the contact prevention member 57 described above for preventing contact and breakage between the first diaphragm 10 and the second diaphragm 50 may be provided. Further, in FIG.
- only one second diaphragm 50 is disposed under the first diaphragm 10, but if the window area of the second diaphragm 50 is smaller than the window area of the first diaphragm 10, A plurality of second diaphragms 50 may be disposed under the first diaphragm 10. In this case, it is possible to collectively observe and analyze a plurality of samples under the plurality of second diaphragms 50.
- the sample 6 it is possible to mount the sample 6 in a state where the distance between the first diaphragm 10 and the second diaphragm 50 is constant and the charged particle beam is applied to the second diaphragm 50.
- This configuration is useful when the sample 6 is adjusted externally and it is desired to immediately observe and analyze with photon beams such as secondary charged particles or X-rays.
- the sample may be introduced from the opening 62 outside the apparatus in a state where the sample stage 52 to which the base 51 is adhered or bonded is removed from the apparatus.
- a flow path 63 through which a liquid flows is provided in a base 51 that supports the second diaphragm 50.
- the flow path is formed by the base 51, the sample base 52, and the second diaphragm 50.
- the present invention is not limited to this, and the member integrated with the second diaphragm 50 has a portion that forms the flow path of the sample. If you do.
- the flow path 63 for example, it is possible to flow the liquid sample in the direction of the arrow in the figure.
- a flow path for discharging the liquid together with the inlet may be provided.
- a sample transmission path such as a nozzle for introducing a sample into the flow path 63 may be provided.
- FIG. 10 shows a configuration in which a plurality of samples are in contact with the flow path 63 and the second diaphragm 50.
- the direction in which the sample is introduced is the direction perpendicular to the paper surface in the figure.
- observation and analysis of the sample flowing through the plurality of flow paths 63 are collectively performed. It becomes possible.
- optical microscope 64 is disposed on the sample side with respect to the second diaphragm 50.
- the positions of the optical axis 53 of the charged particle optical column, the central axis 54 of the first diaphragm, the central axis 55 of the second diaphragm, and the optical axis 65 of the optical microscope 64 are substantially aligned.
- the sample stage 5 is arranged in a configuration that avoids the optical microscope 64. In the case of this configuration, observation and analysis of the sample 6 can be performed not only with the charged particle beam microscope but also with the optical microscope 64.
- the sample stage 52 needs to be transparent to the light of the optical microscope.
- the transparent member include transparent glass, transparent plastic, and transparent crystal.
- a transparent sample table such as a slide glass (or a preparation) or a dish (or a petri dish).
- the “microscope” is described for convenience.
- the behavior of the sample irradiated with the charged particle beam may be observed with an optical microscope, or the sample may be irradiated with light from the optical microscope to observe the behavior. You may observe with a charged particle beam microscope.
- a temperature heater or a voltage application unit capable of generating an electric field in the sample may be provided in the vicinity of the second diaphragm. In this case, it is possible to observe how the sample is heated or cooled and how the electric field is applied to the sample.
- the number of diaphragms may be three or more. For example, there may be a diaphragm inside the charged particle optical column 2. In the present invention, the number of diaphragms does not matter, so long as the intended function is satisfied in this embodiment, it belongs to the category of SEM or charged particle beam apparatus of this embodiment.
- FIG. 12 the whole block diagram of the charged particle microscope of a present Example is shown. Similar to the first embodiment, the charged particle microscope of the present embodiment also includes a charged particle optical column 2, a casing (vacuum chamber) 7 that supports the charged particle optical column with respect to the apparatus installation surface, a sample stage 5, and the like. Composed. Since the operations and functions of these elements or additional elements added to the elements are substantially the same as those in the first embodiment, detailed description thereof is omitted.
- This configuration includes a second casing (attachment) 121 that is used by being inserted into the casing 7 (hereinafter referred to as a first casing).
- the second casing 121 includes a rectangular parallelepiped body portion 131 and a mating portion 132. As will be described later, at least one side surface of the rectangular parallelepiped side surface of the main body 131 is an open surface 15.
- the surface other than the surface on which the diaphragm holding member 155 is installed may be configured by the wall of the second casing 121, or the second casing 121 itself has no wall and is the first. You may be comprised by the side wall of the 1st housing 7 in the state integrated in the 1 housing 7.
- the position of the second housing 121 is fixed to the side surface or inner wall surface of the first housing 7 or the charged particle optical lens barrel.
- the main body 131 has a function of storing the sample 6 to be observed, and is inserted into the first housing 7 through the opening.
- the mating portion 132 forms a mating surface with the outer wall surface on the side surface side where the opening of the first housing 7 is provided, and is fixed to the outer wall surface on the side surface side via the vacuum sealing member 126.
- the entire second housing 121 is fitted into the first housing 7.
- the opening is most easily manufactured using the opening for loading and unloading the sample originally provided in the vacuum sample chamber of the charged particle microscope. That is, if the second casing 121 is manufactured according to the size of the hole that is originally open and the vacuum sealing member 126 is attached around the hole, the modification of the apparatus is minimized.
- the second housing 121 can be detached from the first housing 7.
- the side surface of the second housing 121 is an open surface 15 that communicates with the atmospheric space with a surface that is at least large enough to allow the sample to be taken in and out.
- the sample 6 stored in the space is placed in an atmospheric pressure state during observation.
- 12 is a cross-sectional view of the device in the direction parallel to the optical axis, so that only one open surface 15 is shown, but it is vacuum-sealed by the side surface of the first casing in the back direction and the near side in FIG. If so, the open surface 15 of the second casing 121 is not limited to one surface. It is sufficient that at least one open surface is provided in a state where the second housing 121 is incorporated in the first housing 7.
- a vacuum pump 4 is connected to the first housing 7, and a closed space (hereinafter referred to as a first space) constituted by the inner wall surface of the first housing 7, the outer wall surface of the second housing and the diaphragm 10.
- a first space constituted by the inner wall surface of the first housing 7, the outer wall surface of the second housing and the diaphragm 10.
- the second space can be isolated in pressure in this embodiment. That is, the first space 11 is maintained in a high vacuum by the diaphragm 10, while the second space 12 is maintained in a gas atmosphere having an atmospheric pressure or almost the same pressure as the atmospheric pressure.
- the particle optical column 2 and the detector 3 can be maintained in a vacuum state, and the sample 6 can be maintained at atmospheric pressure. Further, since the second casing 121 has an open surface, the sample 6 can be freely exchanged during observation.
- the first diaphragm 10 On the upper surface side of the second housing 121, the first diaphragm 10 is provided at a position directly below the charged particle optical column 2 when the entire second housing 121 is fitted to the first housing 7. .
- the first diaphragm 10 can transmit or pass the primary charged particle beam emitted from the lower end of the charged particle optical column 2, and the primary charged particle beam passes through the first diaphragm 10 and is finally passed through. Sample 6 is reached.
- the attachment of the present embodiment can be easily increased in size because it is inserted from the side surface of the sample chamber.
- the sample stage 5 is arranged inside the second housing 121.
- a sample stage 52 is disposed on the sample stage 5.
- a base 51 including a second diaphragm 50 is disposed on the sample base 52.
- an apparatus configuration including a liquid introduction / extraction part 300 capable of introducing a sample 6 containing a liquid in a state where the first diaphragm 10 and the second diaphragm 50 are close to each other will be described.
- An opening 62 is provided in the lower part of the sample stage 5 inside the second housing 121, and a liquid introduction / extraction unit 300 is provided. The sample introduced / extracted from the liquid introduction / extraction unit 300 is transmitted to the sample 6 via the opening 62.
- the liquid inlet / outlet part 300 may be fixed on the sample stage 5 or the second casing 121 using a member such as metal, an adhesive, a tape, or the like.
- the sample stage 52 may be fixed on the stage 5 using any member. The sample 6 or the sample stage 52 can be easily transported into the second housing 121 via the open surface 15.
- the liquid introduction / extraction unit 300 is, for example, a tube material such as a nozzle or a straw capable of feeding liquid.
- the liquid introduction / extraction unit 300 may be provided in the sample stage 5 or may be detachable. Further, the function of the liquid introducing / extracting unit 300 may be a spoon such that a few drops of liquid can be mounted. For example, the liquid is supplied to the sample by a procedure in which the liquid is placed on a spoon outside the apparatus, the spoon placed on the liquid is brought close to the sample, and the sample is brought into contact with the liquid from the lower side of the sample.
- the liquid is placed on the sample stage 5, and then the sample is placed under the diaphragm to be charged.
- the sample may be irradiated with a particle beam. Any form may be used as long as the liquid can be introduced from a lower side (for example, a lower surface direction or a side surface direction of the sample) than the sample surface irradiated with the charged particle beam.
- this configuration is an explanatory diagram of an apparatus configuration adopting the structure of FIG. 8, the liquid introduction / extraction section 300 and the opening 62 may not be provided, and the second sample is mounted on the sample stage as described above. After the diaphragm 50 is provided, it may be carried inside the second housing 121.
- the second diaphragm 50 arrangement in the second casing 121 in the second embodiment has been described.
- the second diaphragm 50, its base, and the arrangement place and arrangement method of the liquid introduction / extraction section 300 are places other than the above.
- the SEM or charged particle beam apparatus of the present embodiment belongs to the category.
- FIG. 13 shows an overall configuration diagram of the charged particle microscope of this example. Similar to the first and second embodiments, the charged particle microscope of the present embodiment also includes the charged particle optical column 2, the first casing (vacuum chamber) 7 that supports the charged particle optical column with respect to the apparatus installation surface, the first A second housing (attachment) 121 used by being inserted into one housing 7, a control system, and the like. Since the operations and functions of these elements or additional elements added to the elements are substantially the same as those in the first and second embodiments, detailed description thereof is omitted.
- the open surface that forms at least one side surface of the second housing 121 can be covered with the lid member 122, and various functions can be realized. This will be described below.
- the charged particle microscope of the present embodiment includes a sample stage 5 as a means for moving the observation field of view by changing the sample position on the lid member 122.
- the sample stage 5 includes an XY drive mechanism in the in-plane direction and a Z-axis drive mechanism in the height direction.
- a support plate 107 serving as a bottom plate for supporting the sample stage 5 is attached to the lid member 122, and the sample stage 5 is fixed to the support plate 107.
- the support plate 107 is attached so as to extend toward the inside of the second casing 121 toward the surface of the lid member 122 facing the second casing 121.
- Support shafts extend from the Z-axis drive mechanism and the XY drive mechanism, respectively, and are connected to the operation knob 108 and the operation knob 109 of the lid member 122, respectively.
- the apparatus user adjusts the position of the sample 6 in the second housing 121 by operating these operation knobs 108 and 109.
- the charged particle microscope of the present embodiment has a function of supplying a replacement gas into the second casing or a function of forming a pressure state different from the first space 11 and the outside air outside the apparatus.
- the charged particle beam emitted from the lower end of the charged particle optical column 2 passes through the first diaphragm 10 through the first space maintained at a high vacuum, and further, the atmospheric pressure or the (first space). Intrudes into the second space maintained at a lower vacuum. Then, the charged particle beam is irradiated to the sample 6 through the second diaphragm 50. Since the electron beam is scattered by the gas molecules in the atmospheric space, the mean free path is shortened.
- the scattering probability of charged particle beams is proportional to the mass number and density of gas molecules. Therefore, if the second space is replaced with gas molecules having a lighter mass number than the atmosphere, or if the vacuum is slightly evacuated, the scattering probability of the electron beam is lowered and the charged particle beam can reach the sample. Become.
- the lid member 122 is provided with an attachment portion (gas introduction portion) for the gas supply pipe 100.
- the gas supply pipe 100 is connected to the gas cylinder 103 by the connecting portion 102, whereby the replacement gas is introduced into the second space 12.
- a gas control valve 101 is arranged in the middle of the gas supply pipe 100, and the flow rate of the replacement gas flowing through the pipe can be controlled.
- a signal line extends from the gas control valve 101 to the lower control unit 37, and the apparatus user can control the flow rate of the replacement gas on the operation screen displayed on the monitor of the computer 35.
- the gas control valve 101 may be manually opened and closed.
- the gas is lighter than the atmosphere, such as nitrogen or water vapor, the effect of improving the image S / N can be seen, but helium gas or hydrogen gas having a lighter mass has a better image S / N. Great improvement effect.
- an opening that communicates the inside and outside of the second space is provided below the attachment position of the gas supply pipe 100 by the lid member 122.
- an opening is provided at the attachment position of the pressure adjustment valve 104.
- a pressure regulating valve 104 may be provided instead of the opening described above.
- the pressure regulating valve 104 has a function of automatically opening the valve when the internal pressure of the second housing 121 becomes 1 atm or more. By providing a pressure regulating valve with such a function, when light element gas is introduced, it automatically opens when the internal pressure reaches 1 atm or more and discharges atmospheric gas components such as nitrogen and oxygen to the outside of the device.
- the element gas can be filled in the apparatus.
- the illustrated gas cylinder or vacuum pump 103 may be provided in a charged particle microscope, or may be attached later by an apparatus user.
- the gas cylinder 103 may be a vacuum pump. Then, by slightly evacuating, the inside of the second housing can be brought into an extremely low vacuum state (that is, an atmosphere having a pressure close to atmospheric pressure). That is, the space between the first diaphragm 10 and the second diaphragm 50 can be evacuated.
- a vacuum exhaust port is provided in the second casing 121 or the lid member 122, and the inside of the second casing 121 is slightly evacuated. Thereafter, a replacement gas may be introduced.
- the vacuum evacuation in this case does not require high vacuum evacuation because the atmospheric gas component remaining in the second housing 121 may be reduced to a certain amount or less, and rough evacuation is sufficient.
- the vacuum sealing member may be bonded to the base 51 and the sample base 52 with an adhesive or the like, or the pressure state on the second diaphragm 121 side and the second casing 121 side is separated using an O-ring or packing (not shown). May be.
- a structure in which the metal member is pressed using a metal member, a screw, or the like may be used so that the airtight state is stably maintained.
- the space in which the sample is placed can be controlled to an arbitrary degree of vacuum from atmospheric pressure (about 10 5 Pa) to about 10 3 Pa.
- atmospheric pressure about 10 5 Pa
- the electron beam column and the sample chamber communicate with each other, so if the pressure in the sample chamber is reduced to a pressure close to atmospheric pressure, the pressure in the electron beam column also changes accordingly. Therefore, it has been difficult to control the sample chamber to a pressure of atmospheric pressure (about 10 5 Pa) to 10 3 Pa.
- the second space and the first space are separated by the thin film, the pressure of the atmosphere in the second space 12 surrounded by the second casing 121 and the lid member 122. And the gas species can be controlled freely.
- the sample chamber can be controlled to a pressure of atmospheric pressure (about 10 5 Pa) to 10 3 Pa, which has been difficult to control until now. Furthermore, not only the observation at atmospheric pressure (about 10 5 Pa) but also the state of the sample can be observed by continuously changing the pressure in the vicinity thereof.
- the cylinder 103 may be a complex gas control unit in which a gas cylinder and a vacuum pump are combined.
- a heating mechanism for heating the sample 6 below the second diaphragm 50 may be disposed inside the second casing 121.
- FIG. 14 shows a configuration for setting a sample in a state covered with the second diaphragm 50 from the atmospheric space outside the apparatus.
- the liquid introduction / extraction section 300 is provided around the sample stage 5 and in the vicinity of the sample 6.
- the liquid introduction / extraction part 300 is connected to the lid member 122. If the connecting part 310 is provided on the lid member 122, it is easier to attach a liquid introduction / extraction control unit such as a liquid introduction / extraction pump or a syringe from the outside of the apparatus.
- the second casing internal space may be in a desired gas state or a low vacuum state.
- the vacuum sealing member 66 between the base 51 and the sample stage 52 that supports the second diaphragm 50 is provided.
- a structure in which the metal member is pressed with a metal member, a screw, or the like may be used so that the airtight state is stably maintained.
- the configuration according to the present embodiment is characterized in that the second space 12 inside the second casing is closed as compared with the configuration described above. Therefore, for example, it is possible to provide a charged particle beam apparatus that can introduce gas or evacuate between the first diaphragm 10 and the second diaphragm 50.
- the sample stage 5 and its operation knobs 108 and 109, the gas supply pipe 100, the pressure adjustment valve 104, and the connecting portion 310 are all attached to the lid member 122. Therefore, the apparatus user performs the operation of the operation knobs 108 and 109, the sample replacement work, or the operation of controlling the gas supply pipe 100, the pressure regulating valve 104, and the liquid introduction / extraction on the same surface of the first housing. Can do. Therefore, the operability is greatly improved as compared with the charged particle microscope in which the above-described components are separately attached to the other surfaces of the sample chamber.
- a contact monitor that detects the contact state between the second housing 121 and the lid member 122 may be provided to monitor whether the second space is closed or open.
- an X-ray detector and a photodetector may be provided so that EDS analysis and fluorescent light detection can be performed.
- the X-ray detector or the photodetector it may be arranged in either the first space 11 or the second space 12.
- the replacement gas can be introduced from the atmospheric pressure in addition to the effects of the first and second embodiments.
- the sample can be observed in the same vacuum state as the first space. Is realized.
- FIG. 15A shows a configuration diagram of the charged particle microscope of the present embodiment.
- a vacuum pump and a control system are not shown in the figure.
- the housing 7 and the charged particle optical column 2 that are vacuum chambers are supported by columns, supports, and the like on the apparatus installation surface. Since the operation / function of each element or additional elements added to each element are substantially the same as those in the above-described embodiment, detailed description thereof is omitted.
- the apparatus includes a sample stage 5 that brings the first diaphragm 10 close to the second diaphragm 50 on which the sample 6 is mounted.
- the sample surface below the sample 6 in the drawing that is, the contact surface between the second diaphragm 50 and the sample 6 is observed.
- the upper part of the apparatus is open and the second diaphragm surface is on the lower side of the apparatus, it is possible to mount the sample 6 on the second diaphragm using gravity.
- a base 51 provided with the second diaphragm 50 may be directly mounted on the first diaphragm 10 side (arrow in the figure).
- the sample stage 5 is not necessarily required, but a contact prevention member 56 such as a thin film with a predetermined thickness and a removable foil material is placed between the first diaphragm 10 and the second diaphragm 50.
- the base 51 including the second diaphragm 50 can be safely arranged. If the positional relationship between the first diaphragm 10 and the second diaphragm 50 is to be changed, the base 51 may be moved in the horizontal direction or the paper surface direction in the figure.
- the base 51 may be moved by hand or a jig, or a sample stage having moving means only in the XY directions may be arranged.
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Abstract
Description
本実施例では、基本的な実施形態について説明する。図1には、本実施例の荷電粒子顕微鏡の全体構成図を示す。
第一の隔膜10は土台9上に成膜または蒸着されている。第一の隔膜10はカーボン材、有機材、金属材、シリコンナイトライド、シリコンカーバイド、酸化シリコンなどである。土台9は例えばシリコンや金属部材のような部材である。第一の隔膜10部は複数配置された多窓であってもよい。一次荷電粒子線を透過または通過させることが可能な隔膜の厚みは数nm~数μm程度である。第一の隔膜は大気圧と真空を分離するための差圧下で破損しないことが必要である。そのため、第一の隔膜10の面積は数十μmから大きくとも数mm程度の大きさである。第一の隔膜10の形状は正方形でなく、長方形などのような形状でもよい。形状に関してはどのような形状でもかまわない。
第一の隔膜10と試料ステージ5との間には試料6を搭載可能で第二の隔膜50が具備された土台51が配置される。試料6と第二の隔膜50は試料ステージ5上の試料台上に配置される。第二の隔膜50は土台51によって支持されている。言い換えれば、試料ステージ5の上に載置された試料6は第二の隔膜50によってその表面(観察面)が覆われる。すなわち、第二の隔膜50の試料台側の面(第一の隔膜に対向する面と反対側の面)に試料が接触した状態で一次荷電粒子線が照射される。このため第二の隔膜50は荷電粒子線が透過または通過可能で着脱可能に構成されている。
次に、図4を用いて試料6の透過像観察を行うための構造を図示する。試料6の第二の隔膜50の反対側に試料6を透過した荷電粒子線を検出することが可能な検出器59を備える。検出器59は数keVから数十keVのエネルギーで飛来してくる荷電粒子線を検知及び増幅することができる検出素子である。例えば、シリコン等の半導体材料で作られた半導体検出器や、ガラス面または内部にて荷電粒子信号を光に変換することが可能なシンチレータやルミネッセンス発光材、YAG(イットリウム・アルミニウム・ガーネット)素子等である。検出器59からの信号は配線60を経由してプリアンプ61に送信される。プリアンプ61からの信号は図示しない配線にて下位制御部37に送られ、画像形成信号として使用される。プリアンプは図中大気空間上に配置してあるが、筺体7や試料ステージ5に具備されていてもよい。検出器59が荷電粒子信号を光に変換する検出素子ならば、配線60は光伝送路であり、プリアンプ61は光信号を電気信号に増幅可能な光電気信号増幅器となる。
次に、図5を用いて、第一の隔膜10と第二の隔膜50(または隔膜とそれら土台)とが接触することによって、隔膜が破損するのを防止するための接触防止部材を有する構成に関して説明する。図では、各隔膜の近傍だけを図示し、荷電粒子光学鏡筒2や筺体7などは省略する。図5(a)には第二の隔膜50近傍に接触防止部材56が具備された様子を図示している。接触防止部材56は隔膜の周囲にあってもよいし、隔膜上のどこかに配置してもよい。このように、接触防止部材56を配置すれば、第二の隔膜50を第一の隔膜10に近接させても、隔膜同士が接触することはないので、ユーザは安心して試料ステージ5のZ軸駆動機構を操作できる。この接触防止部材56は第二の隔膜50を製作する際に成膜または蒸着することにより製作が可能である。材料としては例えば有機膜や金属膜などである。厚みとしては、数十nmから100μm以下程度である。この接触防止部材56は図中第二の隔膜50上に具備されているが、第一の隔膜10側にあってもよいし、また両方にあってもよい。接触防止部材56により、第一の隔膜10と第二の隔膜50との最小の近接距離が制限され、この距離以上隔膜同士が近づくことを防止できる。
前記までは試料台52上に第二の隔膜50は一つだけ図示していたが、図6で示したように大気空間の中に複数配置してもよい。この場合のように、一つの板部材(試料台または試料ステージ等)に複数の試料搭載箇所を設け、板部材の移動により様々な種類の試料を隔膜50の下に配置すれば、非常に高スループットに多くの試料の荷電粒子線による観察または分析が可能である。この場合の観察や分析は検出器3による二次的荷電粒子検出だけでなく、前述の図示しないX線などの光子線検出器や透過荷電粒子線の検出を行ってもよい。この複数の検出器による観察や分析は別々に行ってもよいし、同時に行ってもよい。また、試料ステージ5に自動搬送機能を備えていれば、さらに高スループットになるのはいうまでもない。自動搬送機能としては例えば第一の隔膜10下に所望の第二の隔膜50が自動搬送されるために、試料ステージ5に電動モータなどの自動搬送機構を備える。
次に、第一の隔膜10と第二の隔膜50との距離が一定の状態でも、試料6を第二の隔膜を一部として形成される試料保持空間に搭載可能な方法に関して説明する。図8では試料台52の直下(第二の隔膜と対向する面内)に試料6が導入可能な開口部62を備える。試料ステージ上に配置された状態で試料6を第二の隔膜50の直下に配置したい場合は、試料ステージにも図示しない開口部を備えてもよい。この構成の場合は、第一の隔膜10と第二の隔膜50との距離が一定で荷電粒子線が第二の隔膜50に照射させている状態で試料6を搭載することが可能となる。本構成は試料6を外部で調整して、すぐに二次的荷電粒子やX線などの光子線にて観察及び分析したい場合に有用である。また、土台51が密着または接着している試料台52を装置外部に取り外した状態で、装置外部にて開口部62から試料を導入してもよい。
次に、図11に、試料台52の下に光学顕微鏡64を備えた構成に関して説明する。光学顕微鏡64は第二の隔膜50に対して試料側に配置されている。荷電粒子光学鏡筒の光軸53と、第一の隔膜の中心軸54と、第二の隔膜の中心軸55と、光学顕微鏡64の光軸65のそれぞれの軸の位置がほぼ合っているとする。図示しないが試料ステージ5は光学顕微鏡64を避ける構成で配置されるものとする。この構成の場合、試料6の観察及び分析が荷電粒子線顕微鏡だけでなく光学顕微鏡64でも可能となる。但し、この場合は、試料台52は光学顕微鏡の光に対して透明である必要がある。透明な部材としては、透明ガラス、透明プラスチック、透明の結晶体などである。より一般的な試料台としてスライドグラス(又はプレパラート)やディッシュ(又はシャーレ)などの透明試料台などがある。なお、前述では便宜上「顕微鏡」と記載したが、荷電粒子線を試料に照射した試料の挙動を光学顕微鏡にて観察してもよいし、光学顕微鏡からの光を試料に照射してその挙動を荷電粒子線顕微鏡により観察してもよい。
また、図示しないが、第二の隔膜近傍に温度ヒータや試料中に電界を発生可能な電圧印加部などを備えてもよい。この場合、試料が加熱または冷却していく様子や、試料に電界が印加されている様子を観察することが可能となる。また、前述では第一の隔膜と第二の隔膜の二種類の隔膜を配置することに関して説明したが、隔膜の数は三種類以上あってもよい。例えば、荷電粒子光学鏡筒2の内部に隔膜があってもよい。本発明では隔膜の数は問わず、本実施例で意図する機能を満たす限り、本実施例のSEMないし荷電粒子線装置の範疇に属する。
本実施例の荷電粒子顕微鏡は、試料位置を変更することで観察視野を移動する手段としての試料ステージ5を蓋部材122に備えている。試料ステージ5には、面内方向へのXY駆動機構および高さ方向へのZ軸駆動機構を備えている。蓋部材122には試料ステージ5を支持する底板となる支持板107が取り付けられており、試料ステージ5は支持板107に固定されている。支持板107は、蓋部材122の第2筐体121への対向面に向けて第2筐体121の内部に向かって延伸するよう取り付けられている。Z軸駆動機構およびXY駆動機構からはそれぞれ支軸が伸びており、各々蓋部材122が有する操作つまみ108および操作つまみ109と繋がっている。装置ユーザは、これらの操作つまみ108および109を操作することにより、試料6の第2筐体121内での位置を調整する。
本実施例の荷電粒子顕微鏡においては、第2筐体内に置換ガスを供給する機能または第一の空間11や装置外部である外気とは異なった気圧状態を形成可能な機能を備えている。荷電粒子光学鏡筒2の下端から放出された荷電粒子線は、高真空に維持された第1の空間を通って、第一の隔膜10を通過し、更に、大気圧または(第1の空間よりも)低真空度に維持された第2の空間に侵入する。その後、第二の隔膜50を通過し試料6に荷電粒子線が照射される。大気空間では電子線は気体分子によって散乱されるため、平均自由行程は短くなる。つまり、隔膜10と試料6の距離が大きいと一次荷電粒子線または荷電粒子線照射により発生する二次電子、反射電子もしくは透過電子等が試料及び検出器3まで届かなくなる。一方、荷電粒子線の散乱確率は、気体分子の質量数や密度に比例する。従って、大気よりも質量数の軽いガス分子で第2の空間を置換するか、少しだけ真空引きすることを行えば、電子線の散乱確率が低下し、荷電粒子線が試料に到達できるようになる。また、第2の空間の全体ではなくても、少なくとも第2の空間中の荷電粒子線の通過経路、すなわち第一の隔膜10と第二の隔膜50との間の空間の大気をガス置換または真空引きできればよい。
次に、図14に装置外部の大気空間から第二の隔膜50に覆われた状態に試料をセットするための構成を示す。前述の実施例と同様に、試料ステージ5周辺及び試料6近傍に液体導入出部300を備える。液体導入出部300は蓋部材122に接続されている。蓋部材122につなぎ部310を設ければ装置外部から液体導入出用ポンプや注射器などの液体導入出制御部を取り付ける際により簡便となる。前述の通り、第2筺体内部空間は所望のガス状態や低真空状態になる場合がある。そのため、第二の隔膜50を支持する土台51と試料台52間の真空封じ部材66だけでなく、試料台52と試料ステージ5間にも真空封じ部材66を備える。図示しないが気密状態が安定的に維持されるように、金属部材やねじ等で押さえつけるような構造としてもよい。
以上説明したように、本実施例では、試料ステージ5およびその操作つまみ108、109、ガス供給管100、圧力調整弁104、つなぎ部310が全て蓋部材122に集約して取り付けられている。従って装置ユーザは、上記操作つまみ108、109の操作、試料の交換作業、またはガス供給管100、圧力調整弁104や液体導入出の制御の操作を第1筐体の同じ面に対して行うことができる。よって、上記構成物が試料室の他の面にバラバラに取り付けられている構成の荷電粒子顕微鏡に比べて操作性が非常に向上している。
Claims (15)
- 一次荷電粒子線を試料上に照射する荷電粒子光学鏡筒と、
当該荷電粒子線装置の一部を成し、内部が真空ポンプにより真空排気される筐体と、
前記真空排気される空間の気密状態を維持可能であり、かつ前記一次荷電粒子線を透過または通過させる第一の隔膜と、
前記第一の隔膜と前記試料との間に前記一次荷電粒子線を透過または通過可能で第二の隔膜と、を備え、
前記第二の隔膜に接触した状態の試料に対して前記一次荷電粒子線を照射することを特徴とする荷電粒子線装置。 - 請求項1に記載の荷電粒子線装置において、
前記第二の隔膜と前記試料とを搭載可能な試料ステージを有し、
前記第一の隔膜と前記第二の隔膜とが非接触の状態で、当該第一の隔膜と当該第二の隔膜との位置関係と変更可能であることを特徴とする荷電粒子線装置。 - 請求項1に記載の荷電粒子線装置において、
前記第一の隔膜と前記第二の隔膜との距離が一定の状態で、前記第二の隔膜を一部として形成される試料保持空間に前記試料を導入することが可能であることを特徴とする荷電粒子線装置。 - 請求項1に記載の荷電粒子線装置において、
前記第二の隔膜が試料台または試料ステージ上に複数配置されることを特徴とする荷電粒子線装置。 - 請求項4に記載の荷電粒子線装置において、
前記第一の隔膜よりも前記第二の隔膜の窓面積が小さいことを特徴とする荷電粒子線装置。 - 請求項1に記載の荷電粒子線装置において、
前記第二の隔膜に対して前記試料側に配置される光学式顕微鏡を有することを特徴とする荷電粒子線装置。 - 一次荷電粒子線を透過または通過させる第一の隔膜により、試料が載置された空間の圧力が前記一次荷電粒子線を発生する荷電粒子光学鏡筒内部の圧力より大きく保たれるように前記試料が載置された空間が隔離された状態で、前記試料に前記一次荷電粒子線を照射することで前記試料を観察する試料観察装置向けの試料台ユニットであって、
前記一次荷電粒子線を透過または通過させる第二の隔膜と、
前記第二の隔膜を保持する保持部材と、
前記第二の隔膜の保持部材が載置される試料台を有し、
前記第二の隔膜、前記保持部材、前記試料台によって形成される空間に試料が保持されること特徴とする試料観察装置向けの試料台ユニット。 - 請求項7に記載の試料観察装置向けの試料台ユニットにおいて、
前記第一の隔膜と前記第二の隔膜との間の最小距離を制限する部材を有することを特徴とする試料観察装置向けの試料台ユニット。 - 請求項7に記載の試料観察装置向けの試料台ユニットにおいて、
前記第二の隔膜が前記試料台上に複数配置されることを特徴とする試料観察装置向けの試料台ユニット。 - 請求項7に記載の試料観察装置向けの試料台ユニットにおいて、
前記試料を保持する試料台は、前記第二の隔膜と対向する面に、前記試料を導入する開口部を有することを特徴とする試料観察装置向けの試料台ユニット。 - 請求項7に記載の試料観察装置向けの試料台ユニットにおいて、
前記試料保持部材は前記試料の流路を有することを特徴とする試料観察装置向けの試料台ユニット。 - 荷電粒子光学鏡筒から照射される一次荷電粒子線が、試料が載置された空間の圧力が前記荷電粒子光学鏡筒内部の圧力より大きく保たれるように前記試料が載置された空間と前記荷電粒子光学鏡筒の内部の空間とを隔離する第一の隔膜を透過または通過するステップと、
前記第一の隔膜を透過または通過した前記一次荷電粒子線が第二の隔膜を透過または通過するステップと、
前記第二の隔膜を透過または通過した前記一次荷電粒子線が前記第二の隔膜に接触した前記試料に照射されるステップと、
前記一次荷電粒子線の照射によって前記試料から発生した信号を検出するステップを有することを特徴とする試料観察方法。 - 請求項12に記載の試料観察方法において、
前記第一の隔膜と前記第二の隔膜とが非接触の状態で、前記第二の隔膜と前記試料とを保持している試料ステージを移動させて、前記第一の隔膜と前記第二の隔膜との位置関係を変更することを特徴とする試料観察方法。 - 請求項12に記載の試料観察方法において、
前記第一の隔膜と前記第二の隔膜との距離が一定の状態で、前記第二の隔膜を一部として形成される空間に前記試料を導入することを特徴とする試料観察方法。 - 請求項12に記載の試料観察方法において、
前記第二の隔膜は複数設けられており、
前記複数の第二の隔膜のうち一部または全部に前記第一の隔膜を通過または透過した前記一次荷電粒子線が照射されるように、前記複数の第二の隔膜が配置された試料台を移動することを特徴とする試料観察方法。
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