Sample holder, charged particle beam device, and charged particle beam system

Abstract

The purpose of the present invention is to provide a sample holder that can decrease stand-by time during observation and processing of a sample with use of a charged particle beam device. A sample holder according to the present invention comprises an inner cylinder and an outer cylinder, the relative position of which can be changed, wherein: the inner cylinder and the outer cylinder each have an opening; when the relative position is a first position, the inside and outside of the sample holder are in communication via the openings; and when the relative position is a second position, the openings are sealed (see fig. 3A).

Description

Sample holder, charged particle beam device, charged particle beam system

[0001] The present invention relates to a sample holder for holding a sample to be irradiated with a charged particle beam.

[0002] Observing sample structures is becoming increasingly important in the field of materials development. In recent years, there has been a growing demand for observing the crystalline structure of samples while avoiding reactions with atmospheric components, particularly in the fields of environmental energy materials such as organic electroluminescence (EL) devices and lithium-ion batteries. For example, samples for structural observation are prepared using sample preparation equipment such as focused ion beam (FIB) devices or focused ion beam-scanning electron microscope (FIB-SEM) devices, and then observed using sample observation equipment such as transmission electron microscopes (TEM). Among these, sample cooling has attracted attention as a means of suppressing sample damage during processing and observation.

[0003] For example, Patent Document 1 refers to a sample holder structure that allows the sample to be cooled during processing or observation.

[0004] Patent Document 2 mentions a cooling holder structure that reduces the effects of drift and bubbling during observation by devising a dewar shape, which is a liquid nitrogen storage tank.

[0005] JP 2014-010965 A JP 2013-537689 A

[0006] While Patent Documents 1 and 2 have structures that meet the requirements for sample cooling and atmosphere isolation, when considering future improvements in throughput, there is room for improvement in vacuuming the inside of a holder equipped with an atmosphere isolation structure and in handling the holder after cooling.

[0007] Holders with an atmosphere isolation mechanism have a bag-like structure inside to keep out the outside air, and require vacuuming through limited openings. To shorten the exhaust time without changing the vacuum system, it is sufficient to reduce the exhaust volume or increase the exhaust conductance. However, in the case of holders that have a cooling mechanism in addition to an atmosphere isolation mechanism, it becomes difficult to take the above measures.

[0008] Possible cooling mechanisms include the use of a refrigerant such as liquid nitrogen stored in an external refrigerant storage tank, or the use of a Peltier element. However, the latter is less efficient than the former, so for cryogenic applications, the former refrigerant method is the mainstream.

[0009] In structures that use a refrigerant, the sample is cooled through a heat transfer element that runs through the center of the holder. The heat transfer element is in contact with the refrigerant in the refrigerant storage tank and is thermally connected to the tip of the sample holder, achieving sample cooling. To maximize heat transfer efficiency, only a minimum amount of support material is in contact with the heat transfer element. Because the sample is in a vacuum, the heat transfer element connected to the sample stage is also placed in a vacuum. Therefore, a sample holder that can simultaneously achieve both atmospheric isolation and cooling must be evacuated, including the space near the heat transfer element. While it is conceivable that the evacuated volume could be reduced if a vacuum seal could be achieved somewhere between the sample stage and the rear end of the heat transfer element, there is a concern that a sealing element such as an O-ring would reduce cooling efficiency. Therefore, in holders equipped with both an atmospheric isolation mechanism and a cooling mechanism, it is difficult to resolve the issue by simply reducing the evacuated volume.

[0010] The structures shown in Patent Documents 1 and 2 show a heat transfer member that runs through the center and a sample stage connected to the heat transfer member, but no vacuum sealing structure is seen in the space between the end of the heat transfer member that comes into contact with the refrigerant and the sample stage. Current technology is unable to reduce the exhaust volume of the heat transfer section.

[0011] On the other hand, the increase in exhaust conductance can be achieved by adding a structure such as increasing or widening the opening.

[0012] In Patent Documents 1 and 2, an opening called a shutter, through which the sample mounting part passes, is designed at the tip of the holder to evacuate the holder. It can be seen that the inside of the holder is evacuated through this opening.

[0013] In Patent Document 2, it can be seen that a vacuum exhaust port is further provided at the rear end of the holder. However, this port is a structure intended to increase cooling efficiency and extend the coolant retention time by evacuating the inside of the coolant storage tank. The claims of this document also clearly state that the storage container and the housing side (sample holder side) are separate, and this port is not considered to be an opening for evacuating the inside of the holder. Therefore, it can be interpreted that this document does not describe a structure for intentionally increasing exhaust conductance.

[0014] There is a limit to how much the exhaust conductance can be increased by enlarging the opening at the tip of the specimen holder. The distance between pole pieces (magnetic pole pieces of the magnetic lens) in electron microscopes is becoming increasingly narrower due to the focusing performance of the objective lens. While recent improvements in the performance of aberration correctors have alleviated this narrowing trend, in the future, the distance between pole pieces may become even narrower as the performance of electron microscopes improves. This means that the specimen holder tip structure required will likely become thinner.

[0015] Considering this situation, it is expected that the current atmosphere isolation structure, which is established by using the tip of the holder as a lid, will limit the expansion of the opening in the future. In other words, narrowing the distance between the pole pieces directly leads to a deterioration of exhaust conductance.

[0016] Therefore, if we could increase the number of openings that are only open during evacuation, we could increase the evacuation conductance, which would shorten the evacuation time and improve the throughput of sample observation.

[0017] Regarding handling of the cooled specimen holder, it is basically impossible to take it out into the atmosphere until it returns to room temperature. This is because, in the cooled state, the O-ring loses its elasticity, making it difficult to vacuum seal the atmosphere isolation part. Furthermore, if the cooling part is left open, moisture in the atmosphere will condense, causing rust and corrosion inside the specimen holder.

[0018] Therefore, if the time required to return the sample holder to room temperature can be shortened by using a heater mounted on the heat transfer member, it is thought that this will lead to further improvement in throughput.

[0019] In Patent Document 1, the temperature control function is provided by embedding a thermal sensor and a heater inside, but the system does not explicitly state that this temperature control function is used to return the temperature to room temperature when the sample holder is removed.

[0020] The present invention has been made in view of the above-mentioned problems, and has an object to provide a sample holder that can shorten the waiting time during processing or observation of a sample using a charged particle beam device.

[0021] The sample holder of the present invention has an inner tube and an outer tube whose relative position can be changed, and the inner tube and the outer tube each have an opening, and when the relative position is in a first position, the opening connects the inside and outside of the sample holder, and when the relative position is in a second position, the opening is sealed.

[0022] The present invention provides a sample holder that can shorten the waiting time during sample processing or observation using a charged particle beam device. Other problems, configurations, novel features, etc. will become apparent from the description of this specification and the accompanying drawings.

[0023] 5 is a configuration diagram of a charged particle beam device 100 according to a first embodiment. It is a schematic diagram showing the external configuration of a sample holder 1. It is a cross-sectional view of a portion of the tip of the sample holder 1. It is a cross-sectional view of a portion of the tip of the sample holder 1. It is a cross-sectional view of a portion of the tip of the sample holder 1. It is a cross-sectional view of an enlarged schematic cross-sectional view of the periphery of the tip and the sample placement portion 2 of the sample holder 1. It is a schematic diagram of an analysis system 200 including a plurality of charged particle beam devices and operating a sample holder 1. It is a flowchart of operating the embodiment in FIG. 5 for sample processing. It is a flowchart of operating the embodiment in FIG. 5 for sample observation. It is a schematic diagram of an analysis system 200 including a charged particle beam device 100 and a sample mounting system 203 that operates the sample holder 1 using a sealed device 151 such as a glove box. It is an example of a flowchart of a sample preparation method for operating the embodiment in FIG. 7. It is a schematic diagram of an analysis system 200 including a charged particle beam device 100 and a holder preparation system 204 that operates the sample holder 1 using a vacuum chamber 152. 10 is a flowchart of a holder pretreatment method when the embodiment in Fig. 9 is used. Fig. 11 is a flowchart of sample processing in embodiment 4. Fig. 12 is a flowchart of sample observation in embodiment 4.

[0024] Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. In all drawings for explaining the embodiments, components having the same functions are designated by the same reference numerals, and repeated explanations thereof will be omitted. In the following embodiments, explanations of the same or similar parts will not be repeated unless particularly necessary.

[0025] The X, Y, and Z directions described herein are used to describe the orientation of each component of the sample holder, and they intersect and are perpendicular to each other. In the following, the plane defined by the X and Y directions, as viewed from the Z direction, may be described as a planar view.

[0026] 1 is a configuration diagram of a charged particle beam device 100 according to a first embodiment of the present invention. The charged particle beam device 100 includes a charged particle beam source 101, a charged particle beam 102, an illumination lens 103, an objective lens 104, a sample stage 105 for introducing a sample holder into a microscope body, a sample SAM mounted on the sample holder 1, a detector 106 for detecting emitted particles or electromagnetic waves, a device control unit 107 for exchanging electrical signals with the charged particle beam device 100, and a screen display unit 108 for outputting information obtained by the device control unit 107 on a screen. If the charged particle beam device 100 is a processing device, it further includes at least a microprobe 120 and a deposition gun 121. If the charged particle beam device 100 is an observation device, it further includes at least an imaging lens 130 and an imaging device 131 at the imaging plane.

[0027] The sample holder 1 includes a heat transfer member 10, a coolant tank 30, and a temperature regulator 50 (temperature control device). The sample holder 1 has a structure that allows it to be inserted into a desired charged particle beam device 100 by attaching a holder adapter 150 corresponding to the charged particle beam device 100. The temperature regulator 50 may be connected to the sample holder 1 and the device control unit 107 and may have a structure for transmitting and receiving electrical signals.

[0028] A charged particle beam 102 generated from a charged particle beam source 101 is converged by the action of an illumination lens 103 and an objective lens 104 and irradiated onto a sample SAM. The irradiated charged particles interact with the sample SAM, generating electrons, ions, neutral particles, and electromagnetic waves. The generated particles and electromagnetic waves are amplified inside a detector 106 and an imaging device 131, and a spectrum is constructed. The constructed spectrum is transferred to an apparatus control unit 107 and visualized on a screen display unit 108. The structure of the sample holder 1 will be described in detail with reference to FIGS. 2 to 4 in the case where a refrigerant such as liquid nitrogen is poured into a refrigerant tank 30 and the sample is cooled through a heat transfer member 10 in order to cool the sample.

[0029] FIG. 2 is a schematic diagram showing the external configuration of the sample holder 1. The sample holder 1 includes a sample support portion 2 provided at an end of the sample holder 1, a heat transfer member 10 connected to the sample support portion 2 and penetrating the center of the sample holder 1, a heater 11 and a thermal sensor 12 (described below) installed on the heat transfer member 10, a connector portion 13, a refrigerant tank 30 for storing a refrigerant, and a temperature regulator 50. The heater 11 and the thermal sensor 12 are connected to the connector portion 13, and the connector portion 13 is connected to the temperature regulator 50 by a cable. The heat transfer member 10 is inserted into the refrigerant tank 30 and comes into contact with the refrigerant stored in the refrigerant tank 30. When a refrigerant such as liquid nitrogen is injected into the refrigerant tank 30, the sample support portion 2 and the sample SAM are cooled by thermal conduction via the heat transfer member 10. The refrigerant tank 30 is suspended by a suspension structure 31 provided on the sample holder 1 and is detachable from the sample holder 1.

[0030] The temperature regulator 50 includes at least an OFF button 51, an ON button 52, a pair of temperature adjustment buttons 54, and a screen display 55. The screen display 55 displays at least the set temperature and a numerical value obtained by processing the reading of the thermal sensor 12. An ON button 53 may be attached for use in a manner different from the ON button 52. These operate as a user interface (operation interface and screen interface) for the temperature regulator 50. A user using the temperature regulator 50 sets the set temperature to a desired value using the pair of temperature adjustment buttons 54. If the set temperature is higher than the temperature read by the thermal sensor 12, the temperature regulator 50 outputs an appropriate command to the heater 11 through feedback control, adjusting the output of the heater 11 so that the reading of the thermal sensor 12 is the same as the set temperature.

[0031] 3A and 3B show cross-sectional views of a portion of the tip of the sample holder 1. Figure 3A is referred to as the atmospherically isolated state, and Figure 3B is referred to as the open state. The sample holder 1 includes an inner cylinder 21 and an outer cylinder 20 arranged outside the heat transfer member 10, a supporter portion 3 (described below) thermally insulated from the heat transfer member 10 and arranged at the tip of the sample holder, a shutter portion 7 extending from the tip of the supporter portion 3, a shutter sealing member 6 installed to exert an effect on the shutter portion 7, a shutter opening 5 provided in the outer cylinder 20, at least one opening 23 and one opening 24 provided on the side surfaces of the inner cylinder 21 and the outer cylinder 20, and a sealing member 22 provided at a position to exert an effect on the openings 23 and 24.

[0032] The outer cylinder 20 and the inner cylinder 21 have a structure that allows them to transition between a sealed state and an open state by changing their relative positions. In the sealed state, the shutter section 7 contacts the shutter sealing member 6, and the openings 23 and 24 are separated from the space outside the sample holder by the sealing member 22 (the interior and exterior of the sample holder 1 are hermetically sealed). In the open state, the shutter section 7 moves away from the shutter sealing member 6, and the openings 23 and 24 are spatially connected, opening the interior of the sample holder 1 to the outside. In the atmosphere-blocked state, the periphery of the sample holder 2 is isolated from the gas pressure outside the sample holder 1, and in the open state, the pressure is approximately equal to the gas pressure outside the sample holder. In the following explanation, the terms "atmospheric block" and "open" refer to the periphery of the sample holder 2 being in the above-mentioned state.

[0033] FIG. 4 is a schematic cross-sectional view of the sample holder 1, enlarging the area around the tip and sample placement portion 2. The sample SAM is fixed on the sample placement portion 2, or on a half mesh or full mesh installed on the sample placement portion 2. FIG. 4 shows an example using a half mesh 8A. The shutter portion 7 and supporter portion 3 are connected, and the supporter portion 3 is connected to an inner tube 21. The sample placement portion 2 is fixed to the supporter portion 3 by a holding member 4 with low thermal conductivity, allowing the supporter portion 3 and sample placement portion 2 to pass through the shutter opening 5 and be stored inside the outer tube 20. The shutter sealing member 6 is installed in the outer tube 20, and the shutter opening 5 is isolated from the atmosphere by the contact between the shutter portion 7 and the shutter sealing member 6.

[0034] FIG. 5 is a schematic diagram of an analysis system 200 equipped with multiple charged particle beam devices and operating a sample holder 1. The two charged particle beam devices are intended for sample processing and sample observation, respectively. Each system includes a charged particle beam device 100, a holder adapter 150, and a sample holder 1, thereby forming a sample processing system 201 and a sample observation system 202. The holder adapter 150 corresponding to each charged particle beam device allows the same sample holder 1 to be used in different devices. The holder adapter corresponding to the processing device and the holder adapter corresponding to the observation device do not need to be identical. After sample processing, the sample holder 1 is removed in an atmosphere-shielded state and inserted directly into another observation device for sample observation, thereby forming a series of analysis systems 200 including the sample processing system 201 and the sample observation system 202.

[0035] Regarding the analysis system 200 shown in FIG. 5 , a sample processing procedure not shown in FIG. 1 will now be described. When a charged particle beam 102 is irradiated onto a sample, the sample can be efficiently processed by using gallium or argon as the charged particle beam source 101. The processed sample SAM is cut off and attached to the microprobe 120 by the deposition gun 121. The sample SAM is then brought close to the sample mounting portion 2 of the sample holder 1 or to the mesh 8 installed on the sample mounting portion 2. The deposition gun 121 bridges the sample SAM to the intended installation location, and the charged particle beam 102 separates the sample SAM from the microprobe 120, allowing the sample SAM to be placed at the desired location. The series of operations, including mounting the cut sample SAM on the sample holder 1, is called microsampling. As described above, the sample SAM mounted by microsampling can be observed in the desired charged particle beam device 100 using a single sample holder 1 by replacing the holder adapter 150.

[0036] Figures 6A and 6B are examples of flowcharts for operating the embodiment in Figure 5. Figure 6A is a flowchart intended for sample processing applications, and Figure 6B is a flowchart intended for sample observation applications.

[0037] Steps S1 to S3 in Figure 6A are a flowchart showing the operation of changing the sample holder 1 from an atmosphere-blocked state to an open state, steps S4 to S6 shown in Figure 6A are a flowchart showing the operation when cooling the sample SAM, and steps S7 to S8 shown in Figure 6A are a flowchart showing the operation when removing the sample holder 1 from the charged particle beam device 100 in the atmosphere-blocked state.

[0038] In step S1, a holder adapter 150 compatible with the charged particle beam device 100 is attached to the sample holder 1, and inserted into the charged particle beam device 100 in the atmosphere-blocked state shown in FIG. 3A.

[0039] In step S2, the space outside the sample holder is evacuated. By evacuating the sample stage 105 provided in the charged particle beam device 100, an environment is created so that the vicinity of the sample does not come into contact with the atmosphere when the atmosphere shield is released.

[0040] In step S3, the state transitions from the atmosphere-blocked state shown in Fig. 3A to the open state shown in Fig. 3B. By changing the relative positions of the outer cylinder 20 and the inner cylinder 21, the shutter opening 5 and the opening 23 on the side surface of the outer cylinder 20 are spatially connected to the opening 24 on the side surface of the inner cylinder 21, so that the inside of the sample holder 1 shares the same space as the outside of the sample holder 1. Since the environment outside the sample holder is maintained at a vacuum in step S2, the transition to the open state prevents the inside of the sample holder 1 from being exposed to the atmosphere.

[0041] In step S4, a coolant such as liquid nitrogen is poured into the coolant tank 30 shown in Fig. 2 to cool the sample mounting part 2 through the heat transfer member 10. At this time, the sample before micro-sampling may be placed in a cooled location near the sample mounting part 2 for cooling.

[0042] Temperature adjustment may be performed between steps S3 and S4. For example, the following temperature adjustments may be performed: (1) heating the sample to remove gas components adhering to the sample holder 1; (2) automatically adjusting the temperature according to a pre-programmed operation to bring the sample to the desired temperature. The gas components may be removed before cooling the sample or immediately after cooling and processing the sample. Similar temperature adjustments may also be performed in FIG. 6B.

[0043] In step S5, the sample SAM microsampled by FIB processing is fixed on a half mesh 8A or full mesh 8B installed on the sample mounting unit 2. The sample SAM fixed on the mesh 8 is cooled through the sample mounting unit 2 cooled in step S4. During this process, the temperature can be detected by a thermal sensor 12 attached to the heat transfer member 10. Furthermore, the heater 11 also attached to the heat transfer member 10 heats the heat transfer member 10, thereby adjusting the cooling temperature of the sample SAM. At this time, a desired cooling temperature is set using a pair of temperature adjustment buttons 54 attached to the temperature regulator 50, and current is output to the heater 11 by pressing the ON button 52 attached to the temperature regulator 50, thereby maintaining the cooling temperature constant. Furthermore, the output to the heater 11 can be stopped by pressing the OFF button 51 attached to the temperature regulator 50. The heating time by the heater 11 can also be set in advance, and the heater 11 can be automatically turned off when that time has elapsed. The cooled sample SAM is irradiated with the FIB to perform thin film processing. By cooling the sample, thermal damage to the sample caused by the irradiation of the charged particle beam 102 can be reduced.

[0044] In step S6, after sample processing is completed, the temperature of the heat transfer member 10 is quickly returned to room temperature. The coolant tank 30 is removed from the suspension structure 31 to prevent the coolant from coming into contact with the heat transfer member 10. By pressing the ON button 52 provided on the temperature regulator 50, a current is output to the heater 11 attached to the heat transfer member 10, allowing the heat transfer member 10 to be quickly heated to room temperature.

[0045] In step S7, the open state shown in Fig. 3B is transitioned to the atmosphere-blocked state shown in Fig. 3A. By changing the relative positions of the outer cylinder 20 and the inner cylinder 21, the shutter opening 5 and the opening 23 on the side surface of the outer cylinder 20 are spatially isolated from the opening 24 on the side surface of the inner cylinder 21, and the inside of the sample holder is blocked off from the outside of the sample holder. Since the environment outside the sample holder is maintained at a vacuum, the transition to the atmosphere-blocked state maintains the inside of the sample holder as a vacuum.

[0046] In step S8, the sample holder 1 is removed from the charged particle beam device 100. Even if the sample holder 1 in the atmosphere-shielded state is removed into the atmosphere, the vicinity of the sample SAM is not exposed to the atmosphere because it is spatially isolated by the atmosphere shielding.

[0047] Steps T1 to T3 in Figure 6B are a flowchart showing the operation of changing the sample holder 1 from an atmosphere-blocked state to an open state, steps T4 to T7 shown in Figure 6B are a flowchart showing the operation when cooling the sample SAM, and steps T8 to T9 shown in Figure 6B are a flowchart showing the operation when removing the sample holder 1 from the charged particle beam device in the atmosphere-blocked state.

[0048] In step T1, in the atmosphere-blocked state of FIG. 3A, a holder adapter 150 compatible with the charged particle beam device 100 is attached to the sample holder 1, and the sample holder 1 is inserted into the charged particle beam device 100.

[0049] In step T2, the space outside the sample holder is evacuated. By evacuating the sample stage 150 provided in the charged particle beam device 100, an environment is created so that the vicinity of the sample does not come into contact with the atmosphere when the atmosphere shield is released.

[0050] In step T3, the state transitions from the atmosphere-blocked state shown in Fig. 3A to the open state shown in Fig. 3B. By changing the relative positions of the outer cylinder 20 and the inner cylinder 21, the shutter opening 5 and the opening 23 on the side of the outer cylinder 20 are spatially connected to the opening 24 on the side of the inner cylinder 21, so that the inside of the sample holder shares the same space as the outside of the sample holder. In step T2, the environment outside the sample holder is maintained at a vacuum, so that the inside of the sample holder 1 is not exposed to the atmosphere by opening.

[0051] In step T4, a coolant such as liquid nitrogen is poured into the coolant tank 30 shown in FIG. 2 to cool the heat transfer member 10 and the sample support portion 2.

[0052] In step T5, the sample SAM is observed using a TEM. The sample SAM fixed on the sample support section 2 or the mesh 8 installed on the sample support section 2 is cooled through the sample support section 2, which was cooled in step T4. During this process, the temperature can be detected by a thermal sensor 12 attached to the heat transfer member 10. Furthermore, a heater 11 also attached to the heat transfer member heats the heat transfer member 10, thereby adjusting the cooling temperature of the sample SAM. A desired cooling temperature is set using a pair of temperature adjustment buttons 54 attached to the temperature regulator 50, and current is output to the heater 11 by pressing the ON button 52 attached to the temperature regulator 50, thereby maintaining the cooling temperature constant. The output to the heater 11 can also be stopped by pressing the OFF button 51 attached to the temperature regulator 50.

[0053] In step T6, after sample processing is completed, the temperature of the heat transfer member 10 is quickly returned to room temperature. The coolant tank 30 is removed from the suspension structure 31 to prevent the coolant from coming into contact with the heat transfer member 10. By pressing the ON button 52 provided on the temperature regulator 50, a current is output to the heater 11 attached to the heat transfer member 10, allowing the heat transfer member 10 to be quickly heated to room temperature.

[0054] In step T7, the sample holder transitions from the open state shown in Fig. 3B to the atmosphere-blocked state shown in Fig. 3B. By changing the relative positions of the outer tube 20 and the inner tube 21, the shutter opening 5 and the opening 23 on the side surface of the outer tube 20 are spatially isolated from the opening 24 on the side surface of the inner tube 21, and the inside of the sample holder is blocked from the outside of the sample holder. Because the environment outside the sample holder is maintained at a vacuum, the inside of the sample holder is maintained at a vacuum by transitioning to the atmosphere-blocked state.

[0055] In step T8, the sample holder 1 is removed. Even if the sample holder 1 in the atmosphere-blocked state is removed into the atmosphere, the vicinity of the sample is not exposed to the atmosphere because it is spatially isolated by the atmosphere blockage.

[0056] 5 can be operated by combining the above steps S1 to S8 and steps T1 to T8. This effect allows a single specimen holder 1 to be applied to multiple charged particle beam devices, and also allows the entire process from specimen processing to observation to be carried out using a single specimen holder 1. In this case, the pumping speed when evacuating the interior of the specimen holder is increased, and the time required to return the specimen holder 1 from a cooled state to room temperature is shortened, thereby realizing a reduction in the time required for the specimen holder 1 to be returned to room temperature.

[0057] Second Embodiment A second embodiment of the present invention will be described with reference to Figures 7 and 8. The following description will focus on the differences from the first embodiment, and common parts will be omitted.

[0058] 7 is a schematic diagram of an analysis system 200 having a charged particle beam device 100 and including a sample mounting system 203 that operates the sample holder 1 using a sealed device 151 such as a glove box. In FIG. 7, a sample observation system 202 is shown as being representatively included in the analysis system 200, but a sample processing system 201, or both the sample processing system 201 and the sample observation system 202, may also be included in the analysis system 200. The configuration of the charged particle beam device 100 and other configurations are the same as those in the first embodiment.

[0059] The inside of the sealed device 151 is vacuum or filled with an inert gas such as nitrogen or argon, and samples that react with atmospheric components can be stored inside. Part or all of the sample holder 1 can be placed inside the sealed device 151, and the sample SAM can be loaded onto the sample holder 1 inside the sealed device 151 by operating it from outside. Figure 7 is a schematic diagram of a case where the entire sample holder 1 can be placed inside the sealed device 151.

[0060] By blocking the atmosphere inside the sealed device 151, the sample holder 1 can be taken out into the atmosphere while maintaining the atmosphere inside the sealed device 151. Then, by combining the sample holder 1 with the holder adapter 150 and inserting it into the charged particle beam device 100, it becomes possible to process and observe the sample SAM. For example, when it is necessary to receive and observe a processed sample, it is useful to store the sample in the sample holder 1 inside the sealed device 151.

[0061] The present invention is highly effective when the sample SAM is inserted into the charged particle beam device 100, particularly when the inside of the sealing device 151 is filled with an inert gas at a pressure close to atmospheric pressure. By rapidly evacuating the inert gas filling the sample holder 1 through the opening 23 provided on the side of the outer cylinder 20 and the opening 24 provided on the side of the inner cylinder 21, the processing and observation of the sample SAM can be speeded up.

[0062] Fig. 8 is an example of a flowchart of a sample pre-preparation method when operating the embodiment in Fig. 7. Fig. 8 shows operations corresponding to pre-processing for processing and observation, and assumes a procedure for placing a sample SAM inside a sealed device 151. A series of analysis flows can be achieved by carrying out the flowchart in Fig. 6A or Fig. 6B after the flowchart in Fig. 8, or by continuously connecting Fig. 8 to Fig. 6A, or Fig. 8 to Fig. 6B.

[0063] Steps M1 to M3 in Figure 8 are a flowchart showing the operation of loading the sample SAM onto the sample holder 1 in a vacuum or gas, and steps M4 to M5 shown in Figure 8 are a flowchart showing the operation of removing the sample holder 1 from the sealing device 151 in an atmosphere-blocked state.

[0064] In step M1, the sample holder 1 is inserted into the sealing device 151. At this time, it is not necessary to store the entire sample holder 1 inside the sealing device 151. As with a side-entry sample holder (a type of sample holder that can be attached to and detached from the sample chamber via the holder adapter 150, as described in the first embodiment), it is sufficient that at least the sample placement portion 2 is stored inside the sealing device 151, and that the sample SAM or the mesh 8 on which the sample SAM is mounted can be mounted onto the sample placement portion 2 by operating inside the sealing device 151. At this time, the tip of the sample holder 1 is in an open state.

[0065] In step M2, the inside of the sealing device 151 is evacuated or replaced with an inert gas. Since the tip of the sample holder 1 is in an open state, the inside of the sample holder 1 is replaced with the environment inside the sealing device 151.

[0066] In step M3, the sample SAM is loaded onto the sample holder 1 inside the sealed device 151. For example, the sample SAM is loaded onto the sample holder 1 using gloves or a manipulator that can operate the inside of the sealed device 151 from outside the sealed device 151.

[0067] In step M4, the sample holder 1 is put into an atmosphere-blocked state. By putting the inside of the sealed device 151 into an atmosphere-blocked state, the environment inside the sealed device 151 can be maintained in the vicinity of the sample.

[0068] In step M5, the sample holder 1 is removed from the sealing device 151. Since the sample holder 1 is in an atmosphere-blocking state in step M4, even if the sample holder 1 is removed into the atmosphere, the sample SAM does not react with the atmosphere. This allows samples that react with the atmosphere to be transported to a processing device or an observation device. Since the sealing device 151 is intended to receive processed samples, the sample is not irradiated with a charged particle beam within the sealing device 151. Therefore, a step of cooling the sample is not required.

[0069] The connection of the flowchart shown in FIG. 8 will be described in detail. In FIG. 8, after the sample SAM is mounted on the sample holder 1 inside the sealed device 151, if it is necessary to process the sample SAM, the sample processing is performed according to the flowchart in FIG. 6A. If it is necessary to observe the sample SAM, the sample observation is performed according to the flowchart in FIG. 6B. At this time, if the sample mounting, sample processing, and sample observation are performed consecutively, the process may proceed from FIG. 8 to FIG. 6A and then to FIG. 6B. Furthermore, if additional processing is performed after sample observation, the process may return from FIG. 6B to FIG. 6A and then to FIG. 6B. In this way, a series of analysis system 200 is realized by mounting the sample SAM stored in a place isolated from the atmosphere on the sample holder 1 inside the sealed device 151 and processing or observing the sample SAM, or both.

[0070] Third Embodiment A third embodiment of the present invention will be described with reference to Figures 9 and 10. The following description will focus on the differences from the first and second embodiments, and will omit commonalities.

[0071] FIG. 9 is a schematic diagram of an analysis system 200 having a charged particle beam device 100 and a holder pretreatment system 204 that operates a sample holder 1 using a vacuum chamber 152. The vacuum chamber 152 may be a sample processing device or observation device as described above, as long as it has a structure that allows the tip of the sample holder 1 to be placed inside the vacuum. First, the tip of the sample holder 1 is placed inside the vacuum chamber 152. The heat transfer member 10 is heated to a temperature higher than room temperature by adjusting the output of the heater 11 installed on the heat transfer member 10. By raising the temperature, vacuum deterioration and contamination effects due to gas adsorbed to the sample holder 1 can be quickly eliminated. At this time, the sample holder 1 is left open to allow degassing inside the sample holder 1.

[0072] Fig. 10 is an example of a flowchart of a holder pretreatment method for operating the embodiment in Fig. 9. Fig. 9 is intended to be used as a holder pretreatment method before mounting a sample, but depending on the sample characteristics, this flowchart may also be performed after mounting the sample or during processing and observation. By connecting the flowchart in Fig. 10 to the flowchart in Fig. 8, Fig. 6A, or Fig. 6B, a series of analysis system 200 is formed.

[0073] Step H1 in Fig. 10 is a flowchart showing the operation of inserting the sample holder 1 into the vacuum chamber 152, steps H2 and H3 shown in Fig. 10 are a flowchart showing the operation of heating the heat transfer member 10 using the temperature regulator 50, and steps H4 and H5 shown in Fig. 10 are a flowchart showing the operation of removing the sample holder 1 in an atmosphere-blocked state. Steps H4 and H5 are the same operations as steps S7 and S8 in Fig. 6A and steps T7 and T8 in Fig. 6B, and therefore will not be described here.

[0074] In step H1, at least the tip of the sample holder 1 is placed in the vacuum chamber 152. At this time, the sample holder 1 is placed in an open state so that the inside of the sample holder 1 can be evacuated.

[0075] In step H2, the output of the temperature regulator 50 is turned on to raise the temperature of the heat transfer member 10 above room temperature. At this time, the sample SAM is also heated, so if the sample is heat-sensitive, this step should be performed without a sample being mounted. The ON button 53 may be assigned to operate the temperature regulator 50 for this purpose. In this case, it is possible to adjust the temperature to a preset appropriate temperature without specifying a temperature. It is also possible to program the output of the temperature regulator 50 to automatically turn off after heating and maintaining the temperature for a certain period of time. Maintaining a temperature higher than room temperature in a vacuum is expected to have a degassing effect.

[0076] In step H3, the output of the temperature regulator 50 is stopped by operating the OFF button 51, and the process waits until the heat transfer member 10 returns to approximately room temperature after heating. It is essential to operate the device at a temperature below the upper heat resistance limit of the O-ring, which is a sealing member, and it is necessary to ensure safety in contact with the heated components and to ensure that the atmosphere isolation performance is not impaired by the expansion of the components.

[0077] Fourth Embodiment In a fourth embodiment of the present invention, a configuration example will be described in which an operation equivalent to the degassing operation in the vacuum chamber 152 described in the third embodiment is performed in a charged particle beam device 100. The configuration of the charged particle beam device 100 is the same as that of the first embodiment.

[0078] 11A and 11B are flowcharts of the sample processing and observation method according to the fourth embodiment. In FIG. 10, the heating of the sample holder 1 shown in FIG. 9 is performed in a vacuum chamber 152 without a sample SAM mounted thereon. However, in FIGS. 11A and 11B, the heating is performed with a sample SAM mounted thereon. The heating steps described above correspond to steps S11 to S12 in FIG. 11A and steps T11 to T12 in FIG. 11B. FIGS. 11A and 11B are modifications of FIGS. 6A and 6B, and since steps other than steps S11 to S12 and steps T11 to T12 are common, their explanations are omitted. Furthermore, steps S11 to S12 are inserted between steps S3 and S4, but they can be inserted between any steps between S3 and S7, as long as the sample holder 1 is in an open state. Similarly, steps T11 to T12 can be inserted between any steps between T3 and T7.

[0079] Step S11 in FIG. 11A is a flowchart showing an operation of heating the heat transfer member 10 using the temperature regulator 50, and step S12 shown in FIG. 11A is a flowchart showing an operation of turning off the output of the temperature regulator 50 and ending heating.

[0080] In step S11, the output of the temperature regulator 50 is turned on to heat the heat transfer member 10. Since a sample SAM is mounted, the temperature must be adjusted to suit the purpose of the sample SAM. That is, if the sample is heat-sensitive, the temperature should be set to a level below which any chemical reaction will not occur.

[0081] In step S12, the output of the temperature regulator 50 is stopped by operating the OFF button 51, thereby completing the degassing. Although natural cooling is possible, cooling using a refrigerant may be used to reduce the time required.

[0082] Steps T11 and T12 in Fig. 11B correspond to steps S11 and S12 in Fig. 11A, respectively. Since the operation contents are the same, the explanation will be omitted.

[0083] <Modifications of the Present Invention> The present invention is not limited to the above-described embodiments and includes various modifications. For example, the above-described embodiments have been described in detail to clearly explain the present invention, and it is not necessary to include all of the configurations described. Furthermore, a part of one embodiment can be replaced with a configuration of another embodiment. Furthermore, a configuration of another embodiment can be added to a configuration of one embodiment. Furthermore, a part of the configuration of each embodiment can be added to, deleted from, or substituted for a part of the configuration of another embodiment.

[0084] In the above embodiment, the heater 11 and the coolant tank 30 function as a temperature adjustment unit that can heat or cool the sample. These heating and cooling functions may be achieved by separately configuring a device that provides the heating function and a device that provides the cooling function, or by forming these devices integrally.

[0085] In the above embodiment, the sealing device 151 and the vacuum chamber 152 may be configured as components of the charged particle beam device 100 , or may be configured as devices configured separately from the charged particle beam device 100 .

[0086] REFERENCE SIGNS LIST 1 sample holder 2 sample placement section 3 supporter section 4 holding member 5 shutter opening 6 shutter sealing member 7 shutter section 8 mesh 8A half mesh 8B full mesh 10 heat transfer member 11 heater 12 thermal sensor 13 connector section 20 outer cylinder 21 inner cylinder 22 sealing member 23 opening 24 opening 30 refrigerant tank 31 suspension structure 50 temperature regulator 51 OFF button 52 ON button 53 ON button 54 temperature adjustment button 55 screen display section 100 charged particle beam device 101 charged particle beam source 102 charged particle beam 103 irradiation lens 104 objective lens 105 sample stage 106 detector 107 device control section 108 screen display section 120 microprobe 121 Deposition gun 130 Imaging lens 131 Imaging device 150 Holder adapter 151 Sealing device 152 Vacuum chamber 200 Analysis system 201 Sample processing system 202 Sample observation system 203 Sample mounting system 204 Holder preparation system SAM Sample

Claims

1. A sample holder for holding a sample to be irradiated with a charged particle beam by a charged particle beam device, an inner cylinder extending along a first direction, which is the longitudinal direction of the sample holder; an outer cylinder located outside the inner cylinder and extending along the first direction; a first opening provided on a side surface of the inner cylinder; a second opening provided on a side surface of the outer cylinder; a sealing member disposed at a position capable of airtightly sealing a fluid path connecting the inside of the sample holder and the outside of the sample holder via the first opening and the second opening, depending on the relative positions of the inner cylinder and the outer cylinder along the first direction; Equipped with The inner cylinder and the outer cylinder are configured so that the relative position can be changed, when the relative position is a first position, the first opening and the second opening communicate with each other, thereby connecting the inside of the sample holder to the outside of the sample holder without being hermetically sealed by the sealing member; when the relative position is a second position, the first opening and the second opening do not communicate with each other, thereby hermetically sealing the inside of the sample holder from the outside of the sample holder by the sealing member; the sample holder further includes a support portion extending along the first direction and on which the sample can be placed, one end of the outer cylinder along the first direction includes a shutter opening that is arranged so that the supporter portion penetrates from the inside of the outer cylinder toward the outside of the outer cylinder when the relative position is moved along the first direction, the sample holder further includes a shutter sealing member disposed at a position capable of airtightly sealing the shutter opening in accordance with the relative position; when the relative position is the first position, the first opening and the second opening communicate with each other and the shutter sealing member does not hermetically seal the shutter opening, thereby connecting the inside of the sample holder with the outside of the sample holder without hermetically sealing it, When the relative position is the second position, the first opening and the second opening do not communicate with each other and the shutter sealing member hermetically seals the shutter opening, thereby hermetically sealing the inside of the sample holder from the outside of the sample holder. A sample holder characterized by:

2. the sample holder further includes a support portion extending along the first direction and capable of mounting a mounting portion on which the sample is to be placed, the sample holder further includes a heat transfer member extending along the first direction and thermally connected to the placement portion; The heat transfer member is configured to be able to adjust the temperature of the sample via the mounting portion.

2. The sample holder according to claim 1.

3. A charged particle beam device that irradiates a sample with a first charged particle beam, 2. The sample holder according to claim 1 , a heat transfer member thermally connected to the sample holder; a temperature adjusting unit that heats or cools the heat transfer member; a sensor for measuring the temperature of the heat transfer member; a temperature control device that controls the operation of the temperature adjustment unit based on the measurement result by the sensor; Equipped with The temperature control device controls the operation of the temperature adjustment unit to heat or cool the sample mounted on the sample holder. A charged particle beam device characterized by:

4. the charged particle beam device receives the sample holder whose relative position is the second position; After receiving the sample holder, the charged particle beam device evacuates a space around the sample holder; the charged particle beam device moves the relative position to the first position after performing the evacuation; the temperature control device cools the sample mounted on the sample holder; the temperature control device increases the temperature of the sample to a temperature higher than the temperature to which the sample has been cooled; After the relative position is moved to the second position, the charged particle beam device ejects the sample holder to the outside of the charged particle beam device, thereby removing the sample from the charged particle beam device without exposing it to the atmosphere.

4. The charged particle beam device according to claim 3.

5. After performing the evacuation and moving the relative position to the first position, the temperature control device heats the sample to remove gas components adhering to the sample holder.

5. The charged particle beam device according to claim 4.

6. The temperature control device includes an operation interface that allows a user to specify the temperature of the sample.

4. The charged particle beam device according to claim 3.

7. The temperature control device has a screen interface; The screen interface includes: the temperature of the sample specified by the user; the temperature measured by the sensor; Display 7. The charged particle beam device according to claim 6.

8. the charged particle beam device further includes a sample chamber that accommodates the sample holder; The charged particle beam device further includes a holder adapter that has a structure that can be inserted into the sample chamber and is detachable from the sample holder.

4. The charged particle beam device according to claim 3.

9. The charged particle beam device according to claim 3, a second charged particle beam device for irradiating the sample with a second charged particle beam; Equipped with the first charged particle beam is configured to process the sample; the second charged particle beam device is configured to observe the sample by irradiating the sample with the second charged particle beam; the charged particle beam device processes the sample, and then transfers the sample holder, whose relative position is the second position, to the second charged particle beam device; The second charged particle beam device observes the sample mounted on the sample holder received from the second charged particle beam device. An analysis system characterized by:

10. An analysis system comprising the charged particle beam device according to claim 4, The analysis system further includes a sealing device that can accommodate the sample holder while isolating it from the atmosphere; the sample holder receives the sample in a state in which the sample holder is isolated from the atmosphere inside the sealed device; After the sample holder receives the sample, the charged particle beam device receives the sample holder, whose relative position is the second position, from the sealing device. An analysis system characterized by:

11. An analysis system comprising the charged particle beam device according to claim 3, the analysis system further includes a vacuum chamber that accommodates at least a portion of the sample holder within a vacuum space; the vacuum chamber accommodates the sample holder in the vacuum space, the sample holder being in the first position relative to the sample holder; the temperature control device heats the sample holder housed in the vacuum chamber to remove gas components adhering to the sample holder; The charged particle beam device receives the sample holder after it has been heated inside the vacuum chamber. An analysis system characterized by: