JP5631513B1 - Method and apparatus for manufacturing replica thin film for specimen of electron microscope - Google Patents

Abstract

An object of the present invention is to provide a method and apparatus for producing a replica thin film for a specimen of an electron microscope capable of accurately forming a replica of a cross-sectional tissue of a biological sample. A gas reaction vessel 10 for depositing a thin film by direct current glow discharge of a metal gas has an anode 11 formed in a convex shape having a hemispherical shape and a cathode 12 formed in a bowl-like concave shape. And a sample holder 20 that holds the sample 4 on the cathode 12 side. The cutter blade 31 is inserted into the gap of the sample holder 20 and the cutter blade 31 is abutted only on the outer periphery of the sample 4, and at the same time, the sample holder 20 is expanded to cleave the sample 4 and expose it to the surface. A thin film is formed on the surface by direct current glow discharge. [Selection] Figure 1

Description

  The present invention relates to a method for manufacturing a replica thin film of a frozen sample fracture section for a specimen of an electron microscope and a manufacturing apparatus therefor. More specifically, the present invention relates to a replica thin film manufacturing method and a manufacturing apparatus therefor, in which a replica thin film is manufactured by depositing an osmium tetroxide gas plasma metal by a direct current glow discharge method.

  As a method for producing a high-resolution replica film for a transmission electron microscope, a plasma polymerization coating method of an organic compound gas by a direct current glow discharge method proposed by the present inventor is known (see, for example, Patent Documents 1 and 2). That is, as shown in the schematic diagram of the electrode part of the direct current glow discharge method in FIG. 5, the anode 51 and the cathode 52 made of two discs are arranged at an interval of about 45 mm, and the sample 60 to be coated is Then, after being fixed on the cathode 52 and evacuating a gas reaction vessel (not shown), a hydrocarbon gas is introduced to a specified gas pressure, and a DC voltage of about 1 to 1.5 kV is applied between the electrodes 51 and 52. When applied, glow discharge is generated, and for example, a plasma polymerized thin film of ethylene gas adheres to the surface of the sample 60 placed on the cathode 52 to produce a precise replica film. When only the coating film is examined with a transmission electron microscope, the surface fine structure of the sample 60 can be observed in a three-dimensional image. In FIG. 5, 53 is a positive column, 54 is a negative glow phase region, and 55 is a Faraday dark part.

  On the other hand, we examined that the specimen replica film of the scanning electron microscope is also formed by glow discharge. However, since most specimens are bulky and protrude from the shallow area of the negative glow phase, a uniform ultrathin film can be obtained. difficult.

  In the initial stage of the frozen section replica method for biological samples, the plasma polymerized film replica method of organic compound gas was used using two opposing disk-type electrodes. The glow phase region was shallow and the uniform coating on the entire surface was impossible. On the other hand, the room temperature sample apparatus has been rapidly spread by adopting an extremely simplified desktop osmium coating method. However, the frozen section replica method is left behind.

Japanese Patent No. 2,697,753 Japanese Examined Patent Publication No. 62-55095

  As mentioned above, there is no problem in hardness, density, and conductivity with the osmium plasma metal coating method, which has been reduced by an order of magnitude as long as the film thickness of the organometallic gas is limited. If the process of the method, freezing cleaving method, coating method, and microscopic method is performed more rationally, it seems that the utility value is sufficient.

  The present invention has been made in view of such a situation, and can be used for a scanning electron microscope using a plasma metal film of osmium, and a method for producing a replica thin film with an accurate frozen section of a sample. Another object is to provide a manufacturing apparatus.

  Another object of the present invention is to accurately expose a fractured surface of a frozen sample and to cleave a sample holder capable of obtaining both sides of the fractured surface and a sample fixed to the sample holder by impact. The object is to provide a sample cleaving apparatus.

  The present inventor has conducted extensive studies to form a replica thin film by a direct current glow discharge method even for a bulky specimen, and as a result, the discharge system not only expands the negative glow phase region but also exclusively expands the negative glow phase region. The examination was repeated repeatedly. As a result, we focused on the positive column region that occupies a wide area of weak light emission, and if there was a way to reduce this region, we thought that the negative glow phase region would surely spread and repeated experiments. As a result, the discharge voltage is found to change in the potential distribution in the positive column region, emission intensity, deviation from a fixed position, etc. depending on the type of gas, and the anode surface is made smaller and the cathode surface made larger to face each other. As a result of various considerations regarding the electrode shape and arrangement for achieving a stable and uniform electric field, as well as methods for arbitrarily selecting the electrode spacing, concentric, hemispherical large and small cathodes are made to face each other and extremely uneven Both negative and positive electrodes were produced. And this solved the problem that suffered for several years.

The method for producing a replica thin film for a specimen of an electron microscope according to the present invention is such that a convex anode having a hemispherical outer shape and a cathode formed in a bowl-like concave shape concentrically with the anode face each other at a constant interval. samples of use were taken into a rod, and freeze the samples taken in a rod shape was set on the sample holder in the closed position by hinged, or a sample of the bar was frozen after setting the sample holder hinged was placed on the bottom portion of the concave surface of the cathode Te, while developing the sample holder, fractured the sample, to characterized in that that form the metal thin replica by glow discharge method to a cross section exposed by該割sectional that.

  The sample holder can be set so as to be immersed in liquid nitrogen, and the rod-shaped sample can be cleaved when the temperature of the sample holder reaches −120 ° C. to −80 ° C.

The cleaving of the sample can be performed by abutting the cutting edge of the cutter against the sample and opening the sample holder in a closed state and opening the sample holder. More specifically, the sample holder is cleaved by causing the blade of the cutter to protrude by an extrusion spring, and the blade of the cutter is abutted against the surface of the rod-shaped sample and cut into the surface of the sample. The restraint that holds the two plate-like members of the sample holder in a closed state when the cutter blade is abutted against the surface of the sample when the cutter blade is retreated. It is preferable to unfold the sample holder by cutting the yarn because the sample can be cut easily and reliably.

The specimen replica thin film preparation apparatus of the present invention is provided with a gas reaction vessel, a convex anode having a hemispherical outer shape, facing the anode at a predetermined interval, and provided in the gas reaction vessel, A cathode having a hemispherical concave inner surface provided concentrically with the anode, and two plate-like members provided at the bottom of the concave surface of the cathode and fixed in a hinged manner in a closed state sample inserted in communication with the member, the the sample holder to be fractured by the two plate-like member is deployed, removably attached to the cathode, the two sheet members of the sample holder A cutter blade is inserted from the gap of the sample to cleave the sample, and the sample cleaving tool that expands the sample holder, an exhaust device that can evacuate the gas reaction vessel, and a reaction gas into the gas reaction vessel A gas introduction pipe to be introduced; There.

The sample holder has two plate-like members that are rotatably held around the axis in a hinge shape on one edge side, and when the two plate-like members are closed and overlapped with each other, a fixed gap portion is provided between them. And the two plate-like members are unfolded when there is no restraining force, and a restraining thread provided through the gap so that the two plate-like members are held closed. A spring member provided so as to open, and a through hole is formed through which the sample can be inserted through the two plate-like members in a state where the two plate-like members are closed. Is preferred.

  The hinge-type sample holder used in the specimen replica thin film manufacturing apparatus of the present invention has two plate-like members that are rotatably held around an axis in a hinge shape on one end edge side, and the two plate-like members. When the members are closed and overlapped with each other, there is a certain gap portion therebetween, and a restraining thread provided through the gap portion so as to hold the two plate-like members in a closed state, and a restraining force A spring member provided so that the two plate-like members are unfolded and opened when the two plate-like members are open, and the two plate-like members penetrate through the two plate-like members in a closed state. Thus, a through hole into which a sample can be inserted is formed.

  According to the method for producing a specimen replica thin film of the present invention, the sample is cut so as to strike the outer periphery of the sample, and an impact is applied. At the same time, the constraining yarn that closes the two plate-like members of the sample holder is cut. As a result, the two plate-like members are cleaved by the deployment force due to the force of the strong rotating spring. That is, the blade of the knife (cutter) is only cut by about 0.5 mm or less by hitting the periphery of the sample, and thereafter it is cleaved by the impact by hitting the sample and the pulling force when the sample holder is deployed. For this reason, the split section has a very clean split section without any scratches on the cutter blade. Then, since the plasma metal of osmium tetroxide is deposited on the fractured surface, a very thin and strong amorphous replica film can be obtained.

  Further, according to the specimen replica thin film manufacturing apparatus of the present invention, both electrodes for glow discharge are formed so that a hemispherical convex surface and a concave surface substantially concentric with the convex surface are opposed to each other, and the concave surface is formed on the cathode surface. Therefore, the negative glow phase region can be formed on the surface of the cathode in a wide range having a height of about 80% of the distance between the cathode and the anode. As a result, even if the thickness of the sample portion is increased, a uniform thin film can be formed on the entire surface. Even when the sample is inserted into the sample holder and the position of the film formation surface of the sample is separated from the cathode surface, it is uniform. A thin film can be formed. Therefore, the sample holder can be unfolded while the sample is inserted into the through hole of the sample holder and placed on the cathode, and the sample can be cleaved to form a thin film as it is, and can be microscopically examined.

  According to the sample holder of the present invention, when the two plate-like members are rotatably held at one edge side and have a hinge-like structure, and the two plate-like members have no binding force. Since it is attached via a spring member (rotating spring) so as to be unfolded when it is unfolded, the sample holder can be easily unfolded by releasing the fixing means (restraint thread) that becomes a restraining force. Therefore, for example, if the sample holder is closed (folded) and the sample is inserted into the through hole that penetrates the two plate-like members, the sample holder is automatically released by releasing the fixing means. The sample holder tries to expand, and at that time, the sample is cleaved by making a slight cut in the sample, and both surfaces of the divided section of the sample are exposed on the exposed surfaces of the two plate-shaped members that have been expanded. By forming two (two sets) of these through holes, two samples can be cleaved simultaneously to form a replica film on four cross sections.

BRIEF DESCRIPTION OF THE DRAWINGS It is the schematic of the apparatus which forms a thin film using the formation apparatus of the replica thin film for specimens of this invention, (a) is a figure which shows the state which closed the sample holder, (b) expands a sample holder by cleaving a sample. It is a figure which shows the state which carried out. FIG. 2 is a schematic view of a sample holder used for forming a replica thin film of the present invention, in which (a) shows a state in which two plate-like members are closed, and (b) shows a state in which two plate-like members are developed. is there. It is perspective explanatory drawing which shows an example of the sample cleaving apparatus used for the replica thin film formation method of this invention. FIG. 2 is a cross-sectional explanatory view mainly showing the structure of the anode and cathode portions of FIG. 1. It is a figure explaining the state of the conventional glow discharge.

  Next, a method for manufacturing a replica thin film for a specimen of an electron microscope according to the present invention, a manufacturing apparatus, and a sample holder and a sample cleaving apparatus used for the manufacturing will be described with reference to the drawings.

  The production apparatus of the present invention has a small hemispherical anode 11 arranged in the upper part of the gas reaction vessel 10 as shown in a schematic diagram of one embodiment in FIG. The concave cathode 12 concentric with the anode 11 is arranged opposite to the anode 11. When a direct current glow discharge is performed in this state, a uniform negative glow phase region 41 is formed in a wide region of about 80% of the distance between the anode 11 and the cathode 12 as shown in the cross-sectional explanatory diagram of FIG. . In FIG. 4, reference numeral 42 denotes a positive column.

  In FIG. 1, 11a and 12a are lead wires for applying a voltage to the anode 11 and the cathode 12, respectively, 13 is a sample stage (sample mounting table), and 14 is a gas introduction pipe for introducing a reaction gas such as osmium tetroxide. , 15 is an exhaust pipe connected to an exhaust device such as a rotary pump (not shown) in order to make the gas reaction vessel 10 low in pressure, and 19 is an insulating plate. A recess 16 (see FIG. 4) is formed on the bottom surface of the cathode 12, a sample stage 13 is placed in the recess 16, and a hinged sample holder 20 into which the sample 4 is inserted is placed on the sample stage 13. The sample 4 can be cleaved by the cleaving device 30.

  The hinge type sample holder 20 is shown in FIG. 2 (a) in a state in which the two plate-like members 21 and 22 are closed, and in a state in which the two plate-like members 21 and 22 are opened and unfolded (b). As shown, each of the two plate-like members 21 and 22 having a thickness of about 8 mm and a size of about 20 mm square, for example, is fixed to be rotatable around the support shaft 23 like a hinge. At the same time, the strong rotating spring 28 opens and opens when there is no restraining force (see FIG. 2B). Therefore, grooves 21a and 22a are formed to be sandwiched by clamps (not shown) so that the two plate-like members 21 and 22 can be kept closed (see FIG. 2A). Further, when the two plate-like members 21 and 22 are closed, a stopper 26 is formed so that a gap portion 27 of about 2 mm, for example, is formed between the two plate-like members 21 and 22. Has been.

  Further, as shown in FIG. 2 (a), when the two plate-like members 21 and 22 are closed, the through-hole 24 that penetrates the two plate-like members 21 and 22 has a diameter of about 2 mm, for example. The rod-shaped sample 4 can be inserted into the through hole 24. Further, when the sample 4 is inserted, the closed state can be held by a clamp (not shown) as described above. However, as will be described later, the two plate-like members 21, In order to release the restraining force so as to unfold 22, as shown in FIG. 2A, a groove 25 a through which the restraining thread 25 is passed is formed. In other words, during the operation, while holding the closed state by a clamp (not shown), when finally setting the bottom of the cathode 12, the closed state is held by the restraining thread 25, and the clamp is removed.

  The sample 4 to be inserted into the sample holder 20 is formed, for example, by collecting it in a rod shape having a diameter of about 2 mm, or packing the sample into a thin plastic tube having an outer diameter of about 2 mm and a thickness of about 0.2 mm. The sample may be frozen in advance and inserted into the through hole 24 of the sample holder 20, or the sample holder 20 may be frozen after being inserted into the through hole 24 of the sample holder 20.

  For example, as shown in FIGS. 1 and 3, the sample cleaving apparatus 30 has a total length of about 10 cm, a diameter of the cutter cover 34 of about 12 mm, and the cutter blade 31 is about 50 degrees with respect to the horizontal plane. It is attached to the upper part of the cathode 12 by a cutter support frame 36 at a position inclined to the upper side. By pressing the support cylinder 37a of the cutter support rod 37 and leveling the cutter cover 34, the cutter portion can be rotated to the outside of the cathode 12, and the sample cleaving device 30 can be operated as shown in FIG. As shown in FIG. 4, the light can be moved onto the insulating plate 19 outside the cathode 12.

  A thin operation rod (not shown) for external operation of the cutter is at the center. The cutter blade 31 is close to the sample holder 20 and protrudes about 5 mm so as to cut about 0.2 to 0.5 mm into the sample 4. The cutter blade 31 is fixed to the tip of the hammer ring 32. The hammer ring 32 is structured to be pushed out by a strong distance by a strong pushing spring 33. Normally, the hammer ring 32 is retracted against the biasing force of the push spring 33 by the push spring operating plate 33a. That is, by releasing the push-out spring operation plate 33a from the outside, the cutter blade 31 is pushed out to cut the restraint thread 25 of the sample holder 20, and a strong impact and a slight notch are applied to the sample 4, and the restraint thread In combination with the development of the two plate-like members 21 and 22 of the sample holder 20 by cutting 25, the sample 4 is cleaved. At the same time that the shallow cut is made, the cutter blade 31 is pulled back to its original position by a thin pulling spring (not shown). Accordingly, the scar of the cutter blade 31 does not enter the fractured surface of the sample 4, and the both sides that have been cleaved appear on both of the two plate-like members 21 and 22. Reference numeral 35 denotes a rotating shaft, 37 denotes a support rod, and 38 denotes a vertical movement spring. The spring 38 and the like are omitted in FIG. 1 for simplification.

  A sample stage 13 is provided in the recess 16 at the bottom of the cathode 12, and a temperature sensor 17 and a cylindrical heating heater 18 provided in contact with the sample holder 20 are provided therein. The recess 16 is formed to have a diameter of about 30 mm and a depth of about 8 mm, for example, and is formed to have a size that allows the sample holder 20 to be described later to be opened. Even if the setting of the sample holder 20 is completed, if liquid nitrogen does not evaporate or remains, or if the temperature of the sample holder 20 has not risen to a predetermined temperature, the heater 18 is turned on to adjust the temperature. It can be raised. By forming such cooling and heating means, the temperature of the sample holder 20 can be accurately controlled. For example, the temperature of the sample holder 20 when cleaving the sample 4 is adjusted such that the temperature is about −100 ° C. ± 20 ° C. from the frozen −190 ° C. This temperature is selected according to the type and density of the sample 4.

  A method for producing a replica with this apparatus will be described. In order to collect a sample for freezing a living body, a rod having a diameter of about 2 mm is put into liquid nitrogen. The two plate-like members 21 and 22 are closed with the grooves 21a and 22a of the sample holder 20 held between clamps, and the frozen sample 4 is inserted into the through hole 24 (see FIG. 2). In this state, the closed state can be maintained even when the clamp is removed with the restraining thread 25. This sample holder 20 is set in advance on a sample stage 13 disposed with liquid nitrogen in the recess 16 at the bottom of the cathode 12. Then, the clamp is removed so that the restraining thread 25 appears in the gap 27 of the sample holder 20, and the sample cleaving device 30 is set so that the cutter blade 31 enters the gap 27 with a certain distance. . After the liquid nitrogen in the recess (cooling hole) 13 disappears, the bell jar of the gas reaction vessel 10 is closed and evacuation is started.

  In this state, the temperature of the sample holder 20 is measured by the temperature sensor. If the temperature is too low, the heater 18 is flashed to increase the temperature, and when it reaches −100 ° C. ± 20 ° C., the sample cleaving device 30 is operated. Then, the two plate-like members 21 and 22 of the sample holder 20 are developed and the sample 4 is cleaved. Thereafter, the sample cleaving device 30 is rotated and lowered to the outside of the cathode 12 and moved to a fixed position of the insulating plate 19. The insulating plate 19 is formed with a square groove so that the cutter support frame 36 is fitted therein. Further, the cutter support frame 36 is easily detached from the cathode 12 by being only half-turned by the operation rod 37 and is easily detachably held. The fine ice crystals scattered during the cleaving of the sample are removed while being evaporated by the exhaust. What is important at the same time with these operations is the operation to remove the ice on the frozen section of the living body to expose the sample structure. From a shallow one of several nm, deep etching of several tens of μm was performed depending on the speculum purpose. Thereafter, formation of a plasma deposition metal deposition replica film of osmium tetroxide gas by glow discharge is performed.

  Thereafter, when the pressure in the gas reaction vessel 10 becomes 1 Pa, the main valve is throttled to stabilize to 4 Pa, and a certain amount of osmium tetroxide sublimated in the sublimation cylinder is adjusted in the gas reaction vessel 10 by adjusting the gas introduction pipe 14. When it is stabilized at 7 Pa, the glow discharge is turned on. As a result, an ultrathin film having a desired thickness can be obtained in 1 to 10 seconds (film thickness 0.5 nm / second). In this case, the glow discharge voltage is about 1 kV. When the glow discharge is turned off after a predetermined time, the nozzle of the sublimation tube is immediately closed, the main exhaust valve is fully opened, the residual osmium gas in the gas reaction vessel 10 is exhausted completely, and then the main exhaust valve is closed. The gas reaction vessel 10 is opened. If the sample holder 20 on which the two plate-like members 21 and 22 are spread out is taken out as it is and set on the sample stage of the scanning electron microscope and examined, a stereoscopic image and an ultrahigh magnification image of the double-faced replica can be observed. Can do.

This osmium tetroxide uses 0.5 g of osmium tetroxide crystals (OsO ₄ ) enclosed in ampoules, but when released into the atmosphere, it emits a strong irritating odor and must be handled with care. . The gas introduction pipe 14 is in the osmium sublimation cylinder chamber. An ampule is set, the inside of the cylinder is evacuated, the ampule is cleaved, and a predetermined amount is introduced into the gas reaction vessel 10 by the nozzle of the sublimation cylinder. In addition, most of the raw gas flowing before and after this adheres to the oil of the exhaust rotary pump and oxidizes, contaminating the oil black. The raw gas passed through is discharged from the exhaust port of the pump and gives off a strong odor, so the exhaust port of the pump must be inserted into the draft. If this is not possible, it is necessary to pass a filtration device dedicated to osmium gas. In short, it is necessary to connect a filtration device dedicated to osmium gas directly to the exhaust port of the gas reaction vessel and then connect a rotary pump. By doing so, it is possible to reliably eliminate oil contamination and release of raw gas. Exhaust efficiency is not reduced by this filtering device. An osmium-only filtering device is practically used in a small cylindrical shape (diameter 70 mm, length 130 mm).

As for organic compound gas, ethylene (CH ₂ ═CH ₂ ) and naphthalene (C ₁₀ H ₈ ) have been mainly used in the past. However, while investigating the characteristics of other gases, When the plasma polymerized film has a film thickness of about several tens of nanometers, the contrast between the biological film and the film disappears, and when it is reduced below that, the film strength is lost, which is considered to be the limit when using organic gas, To make it thinner than this is based on the idea that it is an osmium thin film region. The power of the osmium film has been proven in the literature. According to recent research using ultra-thin osmium films, examples of successful 150,000-fold stereoscopic image observation of silica nanoparticles, examples of successful Auger analysis (AES) with a 2 nm coating as an antistatic film, electron backscatter diffraction We can fully understand the results of research such as an example in which a polycrystal of lead titanate zirconate can be analyzed with a 0.25 nm film by the method (EBSD).

4 Sample 10 Gas reaction vessel 11 Anode 12 Cathode 13 Sample mounting table 14 Gas introduction pipe 15 Exhaust pipe 16 Recess 17 Temperature sensor 18 Heater 19 Insulating plate 20 Sample holder 21, 22 Plate member 23 Rotating shaft portion 24 Sample insertion hole 25 Fixed Means (restraint thread)
25a Fixing means insertion hole 26 Stopper 27 Gap 28 Spring member 30 Sample cleaving tool 31 Cutter blade 32 Hammer ring (extrusion member)
33 Extrusion spring (extrusion means)
34 Cutter cover 35 Rotating shaft 36 Cutter support frame 37 Cutter operation shaft 37a Cutter layer shaft cover / support cylinder 38 Spring

Claims (8)

A convex-shaped anode having a hemispherical outer shape and a cathode formed in a bowl-like concave shape concentrically with the anode are made to face each other at regular intervals.
Samples were taken for the specimen into bars, frozen and freeze the samples taken in a rod shape was set on the sample holder in the closed position by hinged, or a sample of the bar from the set in the sample holder of the hinged And placed on the bottom of the concave surface of the cathode,
While unfolding the sample holder, cleaving the sample ,
The method for manufacturing a sample replica thin film of the electron microscope, characterized in that that form the metal thin replica by glow discharge method to a cross section exposed by該割cross. Liquid nitrogen is injected into a recess formed in the bottom of the concave surface of the cathode, the sample holder is placed on the recess, the liquid nitrogen is evaporated to a predetermined temperature, and then the frozen sample is cleaved. A method for producing a replica thin film for a specimen of an electron microscope according to claim 1 . 3. The sample holder according to claim 1 or 2 , wherein the setting of the sample holder is performed so as to be immersed in liquid nitrogen, and the cutting of the rod-shaped sample is performed when the temperature of the sample holder reaches -120 ° C to -80 ° C. A method for producing a replica thin film for an electron microscope specimen. The specimen according to any one of claims 1 to 3, wherein the specimen is cleaved by abutting a cutting edge of a cutter against the specimen and releasing the specimen holder in a closed state to expand the specimen. Method for manufacturing a replica thin film. The development and the cleaving of the sample in the sample holder, the incision blades Ri該 cutter by the blade mosquito Potter to be protruded by extruding a spring on the surface of the abutment in the sample on the surface of the sample of the bar At the same time, the cutter blade is retracted, and when the cutter blade is abutted against the surface of the sample, the restraining yarn that holds the two plate-like members of the sample holder closed is cut. The method for producing a replica thin film for a specimen of an electron microscope according to claim 4, wherein the specimen holder is developed by doing so . A gas reaction vessel; a hemispherical convex anode provided inside the gas reaction vessel; and a hemispherical concave inner surface facing the anode at a predetermined interval and concentrically with the anode And a sample inserted in communication with the two plate-like members in a state in which the two plate-like members provided at the bottom of the concave surface of the cathode and fixed in a hinged manner are closed, A sample holder that is cleaved when the two plate-shaped members are developed , and a detachable attachment to the cathode, and a cutter blade is inserted through a gap between the two plate-shaped members of the sample holder, A specimen replica having a sample cleaving tool for cleaving a sample and developing the sample holder, an exhaust device capable of evacuating the gas reaction vessel, and a gas introduction pipe for introducing a reaction gas into the gas reaction vessel Thin film production equipment. The sample holder has two plate-like members that are rotatably held around the axis in a hinge shape on one edge side, and when the two plate-like members are closed and overlapped with each other, a fixed gap portion is provided between them. And the two plate-like members are unfolded when there is no restraining force, and a restraining thread provided through the gap so that the two plate-like members are held closed. And a spring member provided so as to open, and a through hole is formed through which the sample can be inserted through the two plate-like members while the two plate-like members are closed. Item 7. An apparatus for producing a replica thin film for specimen according to Item 6 . A hinge-type sample holder used in a replica thin film manufacturing apparatus for a specimen, comprising two plate-like members rotatably held around an axis in a hinge shape on one edge side, and the two plate-like members And a constraining force provided through the gap so that the two plate-like members are held in a closed state while the two sheets are closed. A spring member provided so that the two plate-like members are unfolded and opened when there is not, and the two plate-like members pass through the two plate-like members in a closed state. A sample holder in which a through hole into which a sample can be inserted is formed.

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