Sample holder, electron beam device, and method for manufacturing sample holder

Abstract

The purpose of the present invention is to provide a sample holding tool that can include therein a plurality of spaces which are hermetically sealed by a diaphragm. This sample holding tool comprises: a partitioning member that partitions an internal space into a first space and a second space; and a sealing material layer that is disposed further above the upper surface of the first space.

Description

[Technical Field]

[0001] The present invention relates to a sample holder having a space for holding a sample. [Background technology]

[0002] In recent years, toward the realization of carbon neutrality, technologies are being developed to analyze the structures and electromagnetic fields of environmentally friendly functional materials, such as catalysts and electrodes, during reactions in controlled liquid or gas environments. These materials are being commercialized for fuel cells, secondary batteries, hydrogen structures, and artificial photosynthesis. Environmental transmission electron microscopy is a technique for observing the reactions of samples in liquid or gas environments by enclosing a liquid or gas membrane through which an electron beam can pass inside a sample holder known as a membrane-type environmental cell. Electron holography is a measurement technique derived from transmission electron microscopy that measures the phase of an electron beam using the interference effect between a matter wave passing through a sample and a reference wave passing through a vacuum.

[0003] Non-Patent Document 1 describes a membrane-type environmental cell in which two silicon nitride membranes face each other via a spacer layer in the vacuum chamber of a transmission electron microscope, and a liquid or gas is injected into the gap between them and sealed.

[0004] Patent Document 1 describes a technique related to a sample support structure, stating in paragraph 0003, "We disclose a novel reinforced thin-film structure with integrated support features, and a fabrication method for the structure. The structure comprises a larger area of ​​membrane with support features that subdivide the large membrane into smaller areas. The structure comprises a large thin-film sample observation area that has the strength of the individual smaller membranes." [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Japanese Patent Application Laid-Open No. 2013-228403 [Non-patent literature]

[0006] [Non-Patent Document 1] F. Wu, N. Yao, Advances in windowed gas cells for in-situ TEM studies, Nano Energy. 13 (2015) 735-756. Summary of the Invention [Problem to be solved by the invention]

[0007] Patent Document 1 subdivides the region to increase the strength of the diaphragm, and does not seem to have clearly considered the formation of multiple spaces sealed with diaphragms. In order to form multiple spaces sealed with diaphragms in a sample holder, it is necessary to cover the spaces with a sealing layer and then adhesively fix the sealing layer, but the document does not disclose any specific method for doing so.

[0008] Electron holography is an example of a technique for observing the behavior of a sample housed in a diaphragm-type environmental cell by irradiating it with an electron beam. In electron holography, it is desirable to use an electron beam that propagates through a vacuum without passing through the sample as a reference wave. Therefore, it is desirable for a sample holder for holding a sample to be observed using electron holography to have a vacuum region located near the space holding the sample. However, the diaphragm-type environmental cell described in Non-Patent Document 1 forms only a single sealed space, so it is believed that there is no vacuum region near the sample (or, even if there is, it is a region outside the diaphragm-type environmental cell that is somewhat distant from the sample). Therefore, it is difficult to perform electron holography using the diaphragm-type environmental cell described in the same document. Even if electron holography were performed, the noise level of the reference wave would be so high that practical accuracy would not be achieved.

[0009] The present invention has been made in view of the above-mentioned problems, and has as its object to provide a sample holder capable of having a plurality of spaces therein sealed by diaphragms. [Means for solving the problem]

[0010] The sample holder according to the present invention comprises a partition member that divides the internal space into a first space and a second space, and further comprises a sealing material layer disposed above the first space. [Effects of the Invention]

[0011] The sample holder according to the present invention can have a plurality of spaces sealed by septa inside. Other configurations, problems, advantages, etc. of the present invention will become apparent from the following description of the embodiments. [Brief explanation of the drawings]

[0012] [Figure 1] 1 is a side cross-sectional view showing an example of the configuration of a diaphragm-type cell 100 according to a first embodiment. [Figure 2] FIG. 1 is a bird's-eye view of a membrane-type cell 100 obtained as a result of lamination. [Figure 3] FIG. 2 is a cross-sectional view of the sample support mechanism in the configuration of FIG. 1, in which the sample holding pocket is filled with a liquid or gas and a solid observation sample and is sealed. [Figure 4] FIG. 10 is a top view showing the flow path structure of a diaphragm-type cell 100 in a second embodiment. [Figure 5] FIG. 10 is a cross-sectional side view of a diaphragm-type cell 100 according to a second embodiment. [Figure 6] A method for fixing the diaphragm cell 100 to the sample holder 500 is shown. [Figure 7] FIG. 10 is a side cross-sectional view showing an example of the configuration of a diaphragm-type cell 100 according to a third embodiment. [Figure 8] FIG. 10 is a diagram showing the configuration of a transmission electron microscope for observing a sample using a diaphragm-type cell 100 according to a third embodiment. DETAILED DESCRIPTION OF THE INVENTION

[0013] <First Embodiment> 1 is a side cross-sectional view showing an example of the configuration of a diaphragm-type cell 100 according to a first embodiment of the present invention. The diaphragm-type cell 100 can be configured as a sample holder that accommodates a sample to be observed using, for example, a transmission electron microscope.

[0014] The lower chip 200 includes a lower silicon frame 202, a lower diaphragm 204, and a spacer layer 210. The heater 230 will be described later. A diaphragm material, typically 200 nm thick or less, is vapor-deposited on a silicon wafer. A typical material for the diaphragm material is a low-stress silicon nitride thin film formed by chemical vapor deposition. However, other thin-film materials with high mechanical strength and electron beam transparency may also be used. After forming a mask on the backside of the silicon wafer, the silicon wafer is selectively back-etched to form a lower diaphragm window 206, exposing the lower diaphragm 204 on both sides. The undissolved silicon wafer portion serves as the lower silicon frame 202, ensuring mechanical strength. A spacer layer 210 is formed on the surface of the lower diaphragm 204. As an in-plane structure of the spacer layer 210, two or more sample pockets (a first sample holder pocket 221 and a second sample holder pocket 222 in FIG. 1) are formed in the lower diaphragm window 206 portion. The sample pockets are recessed from the surface of the spacer layer 210. The spacer layer 210 is fabricated by lift-off lithography or other methods using silicon or a metal species that has high adhesion to the lower diaphragm 204 and low chemical activity. Alternatively, the resist layer forming the first sample holding pocket 221 and the second sample holding pocket 222 may be used as is if the layer has sufficient chemical and thermal resistance to the liquid or gas to be filled. The thickness of the spacer layer 210 determines the gap between the lower diaphragm window 206 and the upper diaphragm window 306, i.e., the electron beam transmission thickness of the liquid or gas to be filled. The width of the pocket partition wall in the spacer layer 210 determines the distance between the first sample holding pocket 221 (first space) and the second sample holding pocket 222 (second space).

[0015] The upper chip 300 has an upper silicon frame 302 and an upper diaphragm 304. An upper diaphragm window 306 is formed in the same manner as in the lower chip 200. The size of the lower diaphragm window 206 and the size of the upper diaphragm window 306 do not necessarily have to strictly match.

[0016] A sealed structure with two sample holding spaces can be fabricated by the following procedure. A thin layer of photocurable resin 310 is applied to the surface of upper diaphragm 304 by a method such as spin coating. Lower chip 200 and upper chip 300 are aligned so that the positions of lower diaphragm window 206 and upper diaphragm window 306 roughly coincide. Then, the surface of spacer layer 210 on lower chip 200 and the photocurable resin layer 310 on upper chip 300 are brought face to face and pressed together with a pressure sufficient to prevent damage to the diaphragms. The photocurable resin layer 310 is then solidified by irradiation with light such as ultraviolet light. Figure 1 is a cross-sectional view of the sealed structure fabricated by the above procedure, in which first sample holding pocket 221 and second sample holding pocket 222 contain only gas.

[0017] 2 is a bird's-eye view of the resulting diaphragm-type cell 100. Whether the sample-holding pocket has two or more chambers can be easily confirmed by using an optical microscope or other method through the upper diaphragm window 306.

[0018] Figure 3 shows a cross-sectional view of the sealed sample support mechanism shown in Figure 1, with the sample holding pocket filled with a liquid or gas and a solid observation sample. For convenience of illustration, the heater 230 is omitted. For environmentally controlled transmission electron microscopy, the lower tip 200 and upper tip 300 are supplied as separate components. The solid sample 410 and liquid / gas 400 are generally filled by the end user. The first sample holding pocket 221 and the second sample holding pocket 222 are filled with the solid sample 410 and the gas or liquid 400. As with the structure shown in Figure 1, a thin photocurable resin layer 310 is applied to the upper diaphragm 304 by spin coating or other methods, and the lower tip 200 and upper tip 300 are bonded together by photopolymerization. This seals the solid sample 410 and the gas or liquid 400 in the first sample holding pocket 221 and the second sample holding pocket 222.

[0019] The thickness of the spacer layer 210 determines the gap between the lower membrane window 206 and the upper membrane window 306, i.e., the electron beam transmission thickness of the liquid or gas to be filled. The width of the pocket partition 224 in the spacer layer 210 determines the distance between the first sample holding pocket 221 and the second sample holding pocket 222. The size of the lower membrane window 206 does not necessarily have to match the size of the upper membrane window 306. The solid sample 410 includes, for example, a metal catalyst or a ceramic support for hydrogen production or carbon dioxide reduction. If the highly corrosive gas or liquid 400 is strongly alkaline or acidic or has strong oxidizing or reducing properties, it is desirable to use a precious metal material such as gold or platinum or a ceramic material as the material for the spacer layer 210.

[0020] To study material behavior under heated or electrified conditions, a microheater for heating the sample and an electrode for applying a bias voltage may be formed in advance from metal on the lower diaphragm 204 below the first sample-holding pocket 221 and the second sample-holding pocket 222, followed by forming an insulating protective layer and then forming a spacer layer 210 on top of that. The heater 230 is an example of a heating element configured in this way.

[0021] The configuration of the diaphragm-type cell 100 in embodiment 1 seals the liquid or gas 400 and the solid sample 410 by hardening the photocurable resin layer 310, so that the sample can be observed using a normal type sample holder without using a sealing mechanism such as an O-ring of a specially designed sample holder.

[0022] <First embodiment: Summary> The sample holder according to the first embodiment is provided with multiple sealed spaces (first sample holder pocket 221 and second sample holder pocket 222) sealed by diaphragms by bonding the upper silicon frame 302 and the lower silicon frame 202 together using a photocurable resin layer 310. This allows samples to be observed by passing an electron beam or the like through the sample. Furthermore, different observations can be performed in each sealed space. This allows multiple trials of different observation conditions to be performed more quickly than preparing and replacing multiple sample holders. This is advantageous compared to a structure in which each sample holder pocket is not sealed but simply covered with a lid member. This is because simply covering the sample holder pocket with a lid member could result in the contents of one sample holder pocket spilling into another.

[0023] In the first embodiment, it has been described that the upper silicon frame 302 and the lower silicon frame 202 are bonded together using the photocurable resin layer 310. This is significant in that the upper and lower frames are bonded together, with the thin film portions exposed by forming the upper and lower diaphragm windows 306 and 206, respectively, to form a sample holder that is transparent to electron beams and the like. It should be noted that in this respect, the first embodiment differs from a typical manufacturing process in which substrates are simply bonded together using a photocurable resin.

[0024] <Embodiment 2> In embodiment 2 of the present invention, a structure is described in which, in a diaphragm-type cell 100, the first sample holding pocket 221 and the second sample holding pocket 222 are not sealed with a lower diaphragm 204 and an upper diaphragm 304 to create a simple closed space, but rather liquid or gas can be supplied to or discharged from the sample holding pockets.

[0025] 4 is a top view showing the flow path structure of the diaphragm cell 100 in embodiment 2. In embodiment 2, the first sample holding pocket 221 and the second sample holding pocket 222 also serve as flow paths for the liquid or gas 400. In this example of a two-chamber structure, two inlets and two outlets are required.

[0026] FIG. 5 is a side cross-sectional view of the diaphragm cell 100 in the second embodiment. FIG. 5 shows the A-A' cross section of FIG. 4. Solid samples 410 are placed in the first sample holding pocket 221 and the second sample holding pocket 222 in advance, and then the lower chip 200 and the upper chip 300 are bonded together by photopolymerization, as in the first embodiment. The channel 260 is formed in the lower silicon frame 202 by chemical etching, plasma etching, or the like. As a result, the channel 260 connects the underside of the lower silicon frame 202 to the first sample holding pocket 221. At this point, because the channel 260 has been formed in the lower silicon frame 202, the diaphragm cell 100 does not have a sealed structure.

[0027] FIG. 6 shows a method for fixing the diaphragm cell 100 to the sample holder 500. The diaphragm cell 100 is fixed to the sample holder 500 by fixing the cell retainer plate 530 to the sample holder frame using fixing screws 540. The sample holder frame 502 is provided with four liquid or gas inlet tubes 510 in this case. The outlets of the liquid or gas inlet tubes 510 are aligned with the flow paths 260, and the cell retainer plate 530 is fixed to the sample holder frame 502, thereby achieving a vacuum seal with the vacuum seal packing 520. As a result, a flow of liquid or gas 400 supplied from outside the vacuum is supplied through the liquid or gas inlet tubes 510 and the flow paths 260 to the sealed first sample holding pocket 221 and second sample holding pocket 222, and then returns to outside the vacuum through the return flow paths 260 and the liquid or gas inlet tube 510. The sample holder 500 and the diaphragm cell 100 can be collectively considered as a sample holder in the broad sense.

[0028] <Third Embodiment> In embodiments 1 and 2, a sample holder according to the present disclosure is used to hold a sample, and the sample can be observed, for example, using an electron microscope. Another possible use of the sample holder according to the present disclosure is observing a sample using electron holography. In embodiment 3 of the present disclosure, the configuration of a sample holder for this purpose and the configuration of a transmission electron microscope using the same will be described.

[0029] FIG. 7 is a side cross-sectional view showing an example of the configuration of a diaphragm-type cell 100 according to the third embodiment. When using a conventional diaphragm-type cell, it was difficult to determine the electric potential field around a solid sample immersed in a liquid or gas based on electron beam phase measurement using electron holography. In the third embodiment, the first sample holding pocket 221 is filled with a solid sample 410 and a gas or liquid 400, and the second sample holding pocket 222 is used as a hole for passing an undisturbed electron beam. Therefore, when the diaphragm-type cell 100 is placed in the sample chamber of a transmission electron microscope, the second sample holding pocket 222 is in a vacuum state, and the electron beam passes through this vacuum.

[0030] First, the first sample holding pocket 221 of the lower chip 200 is filled with a solid sample 410 and a gas or liquid 400. The second sample holding pocket 222 is filled with a gas without placing a solid sample 410 therein. Since the containment process is usually performed in a clean environment at normal pressure, the second sample holding pocket 222 is naturally filled with a gas. In this case, the gas in the second sample holding pocket 222 may be atmospheric air.

[0031] As in the first embodiment, the lower chip 200 and the upper chip 300 are bonded together via the photocurable resin layer 310 to form a sealed structure. This integrated structure is then introduced into a focused ion beam (FIB) processing device or a focused ion beam / scanning electron microscope (FIB / SEM) hybrid device, and only the upper and lower diaphragms located above and below the second specimen holding pocket 222 are removed by focused beam ion etching. Particularly when the spacer layer 210 is made of metal, the position of the second specimen holding pocket 222 can be easily estimated from a secondary electron image, making it easy to determine the area to be irradiated with the focused ion beam. By removing the upper and lower diaphragms, the second specimen holding pocket 222 loses its ability to seal the liquid or gas 400, becoming a vacuum hole 420 through which electron beams propagate in a vacuum without being scattered.

[0032] Taking advantage of this property, the electron beam transmitted through the liquid or gas 400 and solid sample 410 contained in the first sample holding pocket 221 is used as a matter wave 610, and the electron beam 612, which has no wavefront disturbance and propagated through the second sample holding pocket 222 (i.e., the vacuum hole 420), is used as a reference wave. These two waves can be superimposed using an electron biprism 608 (described below) to form interference fringes. In other words, electron holography can be used to determine the electric potential field formed around the solid sample 410 immersed in the liquid or gas 400.

[0033] In this case, since the electron beam interference region is at most on the order of microns, it is desirable that the width of the pocket partition 224 between the first specimen-holding pocket 221 and the vacuum hole 420 (the second specimen-holding pocket 222 before the diaphragm is removed) be 2 micrometers or less. In principle, it is possible to create a structure similar to that shown in FIG. 7 by precisely aligning the lower and upper diaphragm windows 206 and 306 with holes drilled in each, and then bonding them together. However, it is nearly impossible to achieve alignment with an accuracy of 1 micrometer or less under an optical microscope. The advantage of the third embodiment is that the position of the vacuum hole 420 is predetermined as the position of the second specimen-holding pocket 222, so the bonding accuracy of the lower chip 200 and the upper chip 300 can be coarse.

[0034] 8 is a configuration diagram of a transmission electron microscope for observing a sample using a diaphragm-type cell 100 according to embodiment 3. In this example, the sample held in the diaphragm-type cell 100 is measured by electron holography. For simplicity, the lower silicon frame 202, the lower diaphragm 204, the upper silicon frame 302, the upper diaphragm 304, and the photocurable resin layer 310 are omitted from FIG. 8.

[0035] The electron beam generated by the electron source 602 propagates through a solid angle, passes through the diaphragm cell 100, the objective lens 606, and the electron biprism 608, and reaches the detection surface of the detector 640. The regions through which the electron beam passes during this process are indicated by cones 682, 684, and a truncated cone 686. The diaphragm cell 100 is placed in the cone 682 through which the electron beam passes between the electron source 602 and the objective lens 606. The matter wave passes through the upper diaphragm 304, the photocurable resin layer 310, the solid sample 410 and gas or liquid 400 filled in the first sample holding pocket 221, and the lower diaphragm 204. The reference wave passes through the vacuum hole 420. The phase of the matter wave changes depending on the internal potential or electromagnetic field of the material that constitutes the material. The reference wave does not change phase. When this electron beam passes through the objective lens 606, it converges once and then diverges again, as shown in the cone 684. A typical path of a matter wave is shown by dotted line 610 and a typical path of a reference wave is shown by dotted line 612 .

[0036] The electron beam then passes through the electron biprism 608. The electron biprism 608 consists of an electron biprism wire 620, made of a conductive thin wire less than 1 micron wide and given a positive potential, and a pair of grounded counter electrodes 622 and 624. An electric field is generated between the electron biprism wire 620 and the counter electrodes 622 and 624. The electron beam passing through this region is deflected by Coulomb force, with the deflection directions opposite on the right and left sides of the electron biprism wire 620. In other words, the electron beam wavefront is split into two regions with different inclinations. The inclined material wave front 630 and reference wave front 632 overlap as they travel, forming electron interference fringes 642 on the detector 640. The electron beam phase can be determined by Fourier analysis of these interference fringes.

[0037] The electron biprism 608 can be arranged in a configuration in which multiple electron biprisms are arranged downstream of the objective lens 606, or in which one biprism is arranged upstream of the sample and multiple electron biprisms are arranged downstream.

[0038] In embodiment 3, to utilize the interference effect of the reference wave, it is desirable that the vacuum hole 420 be located at a distance of about several hundred nanometers from the solid sample 410, and at most about 2 micrometers. The sample holder according to the present disclosure makes this possible by providing the first sample holding pocket 221 and the second sample holding pocket 222 (vacuum hole 420). Therefore, it is possible to observe the behavior of the solid sample 410 in a gas or liquid 400 by electron holography, which was difficult to do with the conventional membrane-type environmental cell such as that described in Non-Patent Document 1.

[0039] In the third embodiment, in order to irradiate the electron beam in a symmetrical shape, it is preferable that the first specimen-holding pocket 221 and the second specimen-holding pocket 222 are configured in a symmetrical shape with the pocket partition 224 as the center.

[0040] <Embodiment 3: Summary> The sample holder according to the third embodiment forms a hole (vacuum hole 420) that penetrates the second sample-holding pocket 222, thereby enabling a reference wave to pass through the vacuum hole 420. This makes it possible to perform observations by electron holography using the sample holder according to the third embodiment. Furthermore, because the first sample-holding pocket 221 is sealed by the photocurable resin layer 310, there is no risk of the contents spilling out when the vacuum hole 420 is formed. In this respect as well, the sample holder according to the third embodiment is useful.

[0041] <Modifications of the present invention> Although the first and second embodiments have been described with respect to samples for transmission electron microscopes, similar environment-controlled observation can be performed on samples for optical microscopes, laser microscopes, scanning electron microscopes, and X-ray microscopes.

[0042] In the second embodiment, the sample holder 500 is shown as an example of a side entry type for a transmission electron microscope, but it may also be a sample stage for a scanning electron microscope or an X-ray microscope.

[0043] In the above embodiment, the upper silicon frame 302 and the lower silicon frame 202 are bonded together using the photocurable resin layer 310. It is also possible to use a sealing material other than photocurable resin, such as a thermosetting epoxy resin. However, in this case, viscosity and temperature control would be required over a period of several tens of minutes to several hours. On the other hand, photocurable resin requires a shorter time to harden, and the temperature control requirements are less stringent. In this respect, the use of the photocurable resin layer 310 in the sample holder according to the present invention is useful. However, a sealing material layer other than a photocurable resin layer may be used as long as it provides similar benefits. It should be noted that even when a thermosetting resin or the like is used, although the temperature control becomes more complicated as described above, a certain degree of effectiveness can still be achieved.

[0044] In the above embodiments, the sample holder may have three or more sample holding pockets. For example, each sample holding pocket may contain a different sample, a different liquid or gas, or a combination of these, and these may be observed individually. Alternatively, a heater 230 may be provided for each sample holding pocket, and controlled to maintain a different temperature. In this case, the same sample / liquid / gas may be placed in each sample holding pocket, and differences in behavior depending on temperature may be observed.

[0045] In embodiment 3, since electron holography is a technology derived from transmission electron microscopy, it is possible to switch between using electron holography and ordinary transmission electron microscopy using the same equipment. Examples of observation targets using transmission electron microscopy include atomic arrangement structures and phase distributions. Examples of observation targets using electron holography include electric field distributions and magnetic field distributions. Since electron holography requires a longer time to obtain observation data, the applications may be differentiated based on this perspective.

[0046] The following specific applications are conceivable for the above embodiments. (a) Embodiment 1: A transmission electron microscope can be used to investigate phase changes and structural changes that may cause a decrease in the efficiency of a catalyst in a closed, sealed system of liquid or gas. (b) Embodiment 2: A transmission electron microscope can be used to investigate phase changes and structural changes that may cause a decrease in the efficiency of a catalyst in a liquid or gas under liquid or gas flow. (c) Embodiment 3: A transmission electron microscope can be used to observe the potential gradient around a catalyst in a liquid or gas. Differences in reactivity due to heating mechanisms and applied voltage can also be verified. Controlling the surrounding potential gradient enables research into improving the operating efficiency of catalysts. [Explanation of symbols]

[0047] 100 Diaphragm-type cell 200 bottom tip 202 Lower Silicon Frame 204 Lower diaphragm 206 Lower diaphragm window 210 spacer layer 221 First sample holding pocket 222 Second sample holding pocket 224 Pocket partition wall 230 Heater 250 insulating layer 260 flow path 300 upper tip 302 Upper Silicon Frame 304 Upper septum 306 Upper diaphragm window 310 Photocured resin layer 400 Gas or Liquid 410 Solid Samples 420 Vacuum hole 500 sample holder 502 Sample holder frame 510 Liquid or gas introduction pipe 520 Vacuum Seal Packing 530 Cell retaining plate 540 Fixing screw 602 Electron source 606 Objective Lens 608 Electron Biprism 610 matter wave 612 Reference wave 620 Electron Beam Biprism Wire 622 opposing poles 624 opposing poles 640 detector 642 Electron interference fringes

Claims

1. A sample holder for holding a sample, a partition member that divides the internal space of the sample holder into a first space and a second space; a member through which at least one of a charged particle beam and an X-ray can pass toward the first space; a sealing material layer disposed above an upper surface of the first space; Equipped with The member is an upper diaphragm covering at least a portion of an upper region of the first space; a lower diaphragm that forms at least a portion of the bottom surface of the first space; It is composed of the sealing material layer is disposed between the upper diaphragm and an upper surface of the first space, The sealing material layer covers an upper surface of the first space and is in contact with an upper surface of the partition member. A sample holder characterized by:

2. The first space contains a liquid or a gas and also contains the sample.

2. The sample holder according to claim 1.

3. The sealing material layer covers an upper surface of the second space, and the upper diaphragm covers a portion above the upper surface of the second space.

2. The sample holder according to claim 1.

4. The lower diaphragm includes a heating element that is disposed in a position in contact with the bottom surface of the first space and that heats the first space when energized.

2. The sample holder according to claim 1.

5. the sample holder further comprises a lower frame disposed below the lower diaphragm; The lower frame has a flow path that communicates with the first space and allows a fluid to be introduced into the first space or a fluid to be discharged from the first space.

2. The sample holder according to claim 1.

6. The sample holder further comprises: a sample holder frame supporting the lower frame; a member for fixing the position between the lower frame and the sample holder frame; Equipped with The sample holder frame has an inlet pipe that communicates with the flow channel.

6. The sample holder according to claim 5.

7. the sealing material layer and the upper diaphragm have openings communicating with the second space; The lower diaphragm has an opening communicating with the second space.

2. The sample holder according to claim 1.

8. The first space and the second space have shapes symmetrical to each other with respect to the partition member.

8. The sample holder according to claim 7.

9. the sample holder further comprises an upper frame disposed below the upper diaphragm; the sample holder further comprises a lower frame disposed below the lower diaphragm; the upper frame includes an upper diaphragm window that exposes a surface of the upper diaphragm opposite to the first space, The lower frame includes a lower diaphragm window that exposes a surface of the lower diaphragm opposite to the first space.

2. The sample holder according to claim 1.

10. 2. The sample holder according to claim 1, wherein the sealing material layer is a photocurable resin layer.

11. 2. An electron beam apparatus equipped with the sample holder according to claim 1, the first space contains a liquid or a gas and also contains the sample; The member is an upper diaphragm covering at least a portion of an upper region of the first space; a lower diaphragm that forms at least a portion of the bottom surface of the first space; It is composed of the sealing material layer and the upper diaphragm have openings communicating with the second space; the lower diaphragm has an opening communicating with the second space, The electron beam device includes: an electron source that irradiates the first space and the second space with an electron beam; an electron biprism that causes the electron beam that has passed through the first space to interfere with the electron beam that has passed through each of the openings; Equipped with Electron beam apparatus characterized by:

12. A method for manufacturing the sample holder according to claim 1, comprising the steps of: accommodating a liquid or a gas in the first space and accommodating the sample in the first space; placing an upper frame having the sealing material layer on a surface of an upper diaphragm above each of the first space and the second space; bonding the upper frame to the upper surface of each of the first space and the second space by curing the sealing material layer; A method for manufacturing a sample holder having the above structure.

13. The method further comprises: forming a lower diaphragm on a surface of the lower frame; forming a spacer layer on a surface of the lower diaphragm; forming the first space and the second space within a plane of the spacer layer; forming a flow path inside the lower frame that communicates with the first space to introduce a fluid into the first space or to discharge a fluid from the first space; have 13. The method for manufacturing a sample holder according to claim 12.

14. The method further comprises: forming a lower diaphragm on a surface of the lower frame; forming a spacer layer on a surface of the lower diaphragm; forming the first space and the second space within a plane of the spacer layer; forming an opening in the sealing material layer and the upper diaphragm that communicates with the second space; forming an opening in the lower diaphragm that communicates with the second space; have 13. The method for manufacturing a sample holder according to claim 12.

15. 13. A method for manufacturing a sample holder according to claim 12, wherein the sealing material layer is a photocurable resin layer.

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