JP2014041711A - Methods of mounting and removing grid on/from sample holder for transmission electron microscope - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a means capable of easily placing and removing a grid having an observation sample attached thereto on/from a sample holder of an electron microscope.SOLUTION: After a projection 1c of an auxiliary tool for grid installation equipped with the columnar projection 1c at the end of a plate-like substrate 1b is inserted into a through-hole of a sample holder 3 from the lower side to the upper side thereof, and a grid is placed on the upper surface of the protruded columnar projection 1c, the auxiliary tool for the grid installation is descended, the protrusion 1c is removed from the through-hole, and the grid 5 is detained at a prescribed position in the through-hole.

Description

  The present invention relates to a method of using an auxiliary instrument for installing a grid used for attaching a grid on which an observation sample is attached to a transmission electron microscope sample holder, and a structure thereof.

  An electron microscope is a microscope that uses an electron beam instead of light, but a transmission electron microscope uses an electron gun as an electron source, irradiates a sample with a focused electron beam, and transmits or scattered electrons from the sample to an electric or magnetic field. This is an apparatus that bends an electron beam and forms an image for observation. As a structure, a focusing lens, a sample, an objective lens, an intermediate lens, a projection lens, a fluorescent plate, a camera, and the like are installed in this order under an electron gun, and an image is connected to the camera. Since it is necessary to pass an electron beam below the sample, the sample holding portion of the sample holder of the transmission electron microscope (or scanning transmission image) has a hole (hereinafter also referred to as a through hole, which is synonymous). It has a structure.

  In addition, since an electron microscope, particularly a transmission electron microscope, forms an image with transmission electrons, it is necessary to slice the sample to a thickness that allows the electron beam to pass therethrough, and various thinning methods have been used. Thinning methods include pulverization method in which a sample is crushed in a mortar, ion polishing method using polishing and ion milling, microtome method using an ultramicrotome cross-section cutting device, flake processing method using FIB, and a sample in an electrolytic solution. Examples thereof include an electropolishing method in which the material is dissolved and a chemical etching method in which etching is performed with an acid or an alkali.

  In a transmission electron microscope, since the thickness of the sample is such that the electron beam passes, generally 0.1 μm or less, it is very difficult to directly hold the sample with a hand or the like. Therefore, the sample is handled by attaching a sample flake to a grid foil (hereinafter simply referred to as a grid) made of metal or carbon with a thickness of about 20 to 30 μm by electrostatic force or a deposition film. To do.

  In general, the grid is handled with tweezers having a sharp tip and high adhesion. There are various forms of grids. A type that is circular and has a single hole in the center and a supporting film pasted to such an extent that an electron beam passes through the single hole, or a type in which a mesh is stretched on a polygonal or circular grid frame (FIG. 2A) See), a type with a support film affixed thereon, a type that is simply a mesh such as a polygon or a circle, a substantially semi-circular type (see FIG. 2B), a substantially semi-circular shape with protrusions at both ends, and There is a type in which a plurality of fine protrusions are formed on the diameter (see FIG. 2C).

  In the case of a mesh-like grid, a sample (thin piece) is directly attached so as to cross the mesh, or a support film made of a thin carbon-based material or organic component material is formed on the mesh, and the sample is attached on the support film. Often. In the case of a semicircular grid (FIG. 2B), the sample is often fixed by deposition or the like so as to protrude from the diameter portion of the semicircular grid into the semicircular surface. In addition, in a grid (FIG. 2C) in which a semi-circular and fine protrusion is formed in a direction perpendicular to the diameter, the sample is often fixed to the protrusion with a deposition film or the like.

In both cases, the thickness of the sample (thin piece) is sufficiently thin compared to the 20-30 μm thickness of the grid, and it is fixed in the middle of the thickness direction of the grid, and even when the grid is placed flat, the sample protrudes outside the grid thickness. It is generally fixed at a position where it will not be damaged. There are a plurality of grid materials, and Cu, Mo, Pt, SUS, Ni, Au, Be, Al, C, and nylon are commercially available. The outer diameter of each grid is a diameter that fits the accommodating portion of the microscope sample holder, and is approximately about 3 mm. The diameter of the hole through which the electron beam passes varies depending on the type, but is generally within 2 mm.

  The grid integrated with the flake sample needs to be preserved until observation with an electron microscope. Methods for storage include placing in a dent case that matches the grid diameter, attaching a portion of the grid to a weakly sticky sheet, fixing it, wrapping it with a low-contamination medicine-wrapping paper or aluminum foil, etc. There are various ways. In the case of a disk-shaped grid, it is easy to store in a case having a dent matched to the grid diameter. However, in the case of a grid that is not a disk, such as for FIB, the grid is slightly smaller than the mesh grid, so the grid may move in the case without being fixed by the dent, and inserted into the bag, Using the method of fixing with an adhesive sheet or sandwiching a part of the end of the grid can avoid a situation where the sample piece collides with the surroundings and can be safely stored.

  There are various types of sample holders for electron microscopes. In particular, in the case of a specification for observing a transmission image, an electron beam transmitting hole is required below the sample. When the electron beam is irradiated from above the sample holder in the apparatus, the electrons transmitted through the hole are directed to the electron lens and imaged by a camera, a fluorescent plate or the like. In addition, the observation sample has a structure that is fixed so as not to move from above the hole after being placed on the sample holder regardless of whether or not the grid is used. There are various fixing methods, such as fixing from above with a screw and a metal plate, and fixing a metal plate with a spring. In many cases, a slight recess is provided so as to surround the hole of the sample holder, and a grid is fitted into the recess to fix the approximate position (see FIG. 3). In addition, the sample holder itself is usually fixed to a predetermined location in the microscope tube with a predetermined instrument, and the grid is usually placed on the sample holder.

  At the time of observation, the grid with the sample is taken out from the storage tool described above using tweezers, and the grid is attached to the sample holder. Recently, there is a case where the handling of the grid is not necessary by inserting a sample holder for observation directly into the FIB apparatus, processing the final thin piece, and bringing the sample holder together with the observation apparatus. However, if the manufacturers of the processing apparatus and the observation apparatus are different, or if there are a plurality of samples, they are often observed after storage, and handling of the grid with tweezers or the like is indispensable. In this operation, a portion that does not affect the passage of the electron beam through the grid is held by tweezers and handled.

JP 2012-68033 A Utility Model Registration No. 3085261

Edited by Kentaro Asakura and Yasuhisa Hirohata, “Ultra Microtome Technique Q & A for Electron Microscope Researchers”, Agne Jofusha, 1999.

  However, gripping the grid with tweezers and placing it in the specified dent of the electron microscope sample holder is a task that uses nerves, and it is difficult to perform reliably depending on the observation environment, the condition of the worker, etc. There is. Also, when removing from the sample holder after observation, the grid may not be grasped well with tweezers, and removal may fail. For example, the tweezers tip and the grid may adhere due to static electricity or transfer of a small amount of adhesive component of the sample storage tool, and the grid may not be separated even if the tweezer tip is opened. Since the grid is very thin and light, it cannot be removed from tweezers due to slight adhesive force or electrostatic force.

  Furthermore, the FIB grid has a semi-circular shape (Fig. 2 (b)), which is slightly smaller than the mesh-type circular shape, so if it cannot be put in place properly, it will fall from the hole of the sample holder to the lower part. There is a case. If the grid surface stays in the middle of the hole in a flat state, when collecting the dropped grid, the tip of the tweezers must be submerged in the bottom surface of the grid, even if the grid edge is suppressed on one side and the grid is tilted, The grid may fly, fall further from the initial drop position, or bend the grid itself.

  In addition, foreign matter may adhere to the sample surface due to dropping, and elemental analysis with an electron microscope using characteristic X-rays may not be possible. In addition, the sample flakes may be damaged by the impact of dropping, and an image may not be acquired. In addition, the whereabouts of the grid that flew may not be known and analysis may be impossible. If the specimen having only one specimen is lost, the process cannot be performed again. Therefore, the process of stationary fixing the grid at a predetermined position so as not to fall from the hole is very important.

  Also, when removing the grid from the sample holder after observation, especially if there is a possibility of observing multiple times, such as reworking a thin piece and observing it again, it must be picked up without damaging the grid. I must. However, the grid is flat on the sample holder, and when picking up the grid with tweezers, the grid may be accidentally dropped from the hole or dropped under the sample holder when the tip of the tweezers is submerged in the bottom surface of the grid. There is a risk of deforming the grid. If there is such damage, additional processing and re-observation may be difficult. Therefore, it is very important to remove the grid from the sample holder without failure.

  Therefore, the present invention can easily place the grid with the observation sample on a predetermined position of the sample holder of the transmission electron microscope and ensure that even a beginner unfamiliar with handling or fatigue when the hand is likely to go wrong. It was intended to provide a means that can be removed.

In order to solve the above-mentioned problem, the invention according to claim 1 is a method of mounting a grid for holding an observation thin piece sample to a predetermined position of an electron beam transmitting through-hole provided in a transmission electron microscope sample holder,
A step of inserting the protrusion of the grid installation auxiliary instrument having a columnar protrusion at the end of the plate-like base material upward from below the through hole; and
Placing the grid on the upper surface of the columnar protrusion protruding from the through hole; and
Mounting the grid to the sample holder for a transmission electron microscope, the method comprising: lowering the grid installation auxiliary tool, extracting the protrusion from the through hole, and retaining the grid in a predetermined position in the through hole. It is a method.

The invention according to claim 2 is a method for removing the grid holding the observation thin piece sample held in a predetermined position of the electron beam transmission through-hole from the sample holder for the transmission electron microscope,
A step of lifting the grid by inserting the protrusions of the grid-installing auxiliary instrument having columnar protrusions at the end of the plate-like base material upward from below the through holes; and
A step of grasping the edge of the lifted grid and removing it from the sample holder; and a step of lowering the grid installation auxiliary device, extracting the protrusion from the through hole, and removing the auxiliary device. This is a method of removing the grid from the transmission electron microscope sample holder.

  Further, the invention according to claim 3 is characterized in that the plate-like base material has a shape in which two plate-like base materials or two “he” -shaped plate-like base materials are connected. This is a method of attaching a grid to a sample holder for a transmission electron microscope.

  The invention according to claim 4 is characterized in that the columnar protrusion has a height in a range of 1.0 mm to 3.0 mm and a diameter in a range of 1.0 mm to 2.5 mm. The method of attaching a grid to the transmission electron microscope sample holder according to claim 1 is used.

  The invention according to claim 5 is characterized in that the columnar protrusion has a height in a range of 1.0 mm to 3.0 mm and a diameter in a range of 1.0 mm to 2.5 mm. The method of removing the grid from the transmission electron microscope sample holder according to claim 2 is used.

  By using a grid installation auxiliary tool having a columnar protrusion at the tip according to the present invention, the sample thin piece for observation can be obtained by taking the columnar protrusion into and out of the electron beam transmitting hole formed in the sample holder. The affixed grid can be easily and reliably attached to a predetermined site in the hole, and can be removed. Therefore, even if it is difficult to remove the grid from the tweezers due to the influence of static electricity, adhesive, etc., it is difficult to attach / remove the tweezers alone. It can be attached to the recess for installing the grid of the holder and can be floated from the site.

  The invention of claim 3 allows for a shape in which two plates bent in a “he” shape are connected in addition to a flat shape from the cylindrical projection portion to the handle portion of the auxiliary equipment for grid installation. It is. This is because the grid can be easily attached and detached when bent.

It is the upper surface external view (a) and side external view (b) explaining the structure of a grid installation auxiliary tool. (A)-(b) is a figure which shows an example of a grid shape. (A)-(b) It is a cross-sectional schematic diagram explaining the process of attaching a grid to a sample holder using a grid installation auxiliary tool. (A)-(c) It is a cross-sectional schematic diagram explaining the process of removing a grid from a sample holder using a grid installation auxiliary tool. The grid installation auxiliary instrument tip protrusion enlarged view. (A) a cylinder, (b) a cylinder. It is an external view explaining another example of a grid installation auxiliary instrument. It is an external view explaining the shape to the holding part of a grid installation auxiliary instrument. (A) Perspective view, (b) Cross-sectional view.

Embodiments of the present invention will be described with reference to the drawings.
The basic structure of an auxiliary device for grid installation (hereinafter referred to as an auxiliary device) is an elongated plate shape as shown in FIG. 1, and is provided with a columnar protrusion 1c at the center of the tip of a plate-like substrate 1a. . On the other hand, the basic structure of a sample holder for a transmission electron microscope (hereinafter referred to as a sample holder) paired with the auxiliary instrument is shown in the upper drawing of FIG. The sample holder is provided with a recess 3d having a depth that allows the grid to be placed flat and accommodated in the middle of the thickness direction of the sample holder, and a flat bottom having a size, and is slightly smaller than the bottom of the recess 3d. A hole 3c for transmitting an electron beam having a diameter is formed. The minute cylindrical protrusion 1 c can be inserted into the hole 3 c for transmission electrons of the sample holder 3. The columnar protrusion 1c has a column height that is slightly higher than the upper surface of the sample holder 3 (broken line portion in FIGS. 3A and 3B) when the protrusion is inserted.

  As shown in FIG. 2, there are various shapes for the thin-film holding grid for an electron microscope, but a circular shape having a mesh portion (FIG. 2A), a pseudo semicircular shape obtained by removing a part from a disk, or a semi-circular shape. There are a circular shape (FIG. 2B), or a shape in which a minute protrusion protrudes in the plate direction at the center (FIG. 2C). The grid is made of Cu, Mo, Pt, SUS, Ni, Au, Be, Al, C, nylon, etc., and the thickness of the grid is about 20 to 30 μm and the diameter is about 3 mm. When using a circular grid having a mesh portion, the sample is placed on the sample holder of the electron microscope with the observation sample attached to the surface of the support film stretched on the grid. In a semi-circular shape with a part removed from the disk, or a grid with a small protrusion at the center protruding in the plate direction, the observation sample is attached to the disk cross-section or protrusion with a deposition film or adhesive.・ Apply.

  In observing the observation sample with a transmission electron microscope, the observation sample is put on the hole 3c on the concave portion 3d opened in the sample holder 3 with the flaky observation sample attached to the grid. (FIG. 3 (c)). After the sample observation, the grid 5 is detached from the sample holder 3 and taken out of the microscope in a state where the flaky observation sample is stuck on the grid.

  The present invention provides a method for attaching and detaching a grid to a sample holder. This will be described in detail below.

  The thin piece used as the observation sample is produced by a known method. Specifically, it can be formed by fine processing using a focused ion beam apparatus (FIB), cutting processing using a microtome, or the like.

  FIG. 3 shows an outline of a method of installing and attaching the thin grid for an electron microscope according to the present invention to the sample holder. In the mounting method of the present invention, the cylindrical protrusion 1c at the tip of the auxiliary instrument 1b is inserted from the bottom surface of the through hole 3c for transmission electrons of the sample holder 3 toward the top surface (FIG. 3 (a)). Next, with the protruding portion 1c protruding from the through hole 3c, the grid 5 frame gripped by the tweezers 4 is placed on the upper surface of the columnar protruding portion 1c in a state of being attached to the bottom surface of the recessed portion 3d. At this time, the protruding portion 1c is set near the center of the through hole 3c. Then, the metal part of the grid frame comes into contact with the side wall (FIG. 3B).

  Whether the grid is a mesh or a semicircular grid, there is no sample to be observed in the peripheral frame portion of the grid, so that the sample can be prevented from being damaged by contact. In semicircular grids, the sample is often attached so that it protrudes from the cut surface of the disk, but the foil thickness of the grid mesh is sufficiently thick compared to the thickness of the sample flakes, so the sample is a protrusion of the instrument. It will not be damaged by touching the part.

  If the tip of the tweezers 4 for gripping the grid (particularly the lower tip) and the grid 5 are difficult to attach and separate, the frame of the grid 5 is put on the corner of the cylindrical protrusion 1c, and the grid of the cylinder 1c and the sample holder 3 is placed. If the tweezers 4 are pulled out at a slight height difference from the installation position, the grid can be removed from the tweezers and scraped off at a predetermined position of the grid. If the upper end of the tweezers 4 sandwiching the grid 5 and the grid 5 are difficult to be separated from each other, it is often possible to take the tip of the grid 5 by placing it flat on the sample holder 3 as it is. It can also be scraped off as described.

After the grid 5 and the tweezers 4 are separated from each other, when the projection 1c protruding from the bottom of the hole is lowered and the instrument is slowly removed from the sample holder 3, the sample attached to the grid seems to block the hole 3c. Can be accommodated in the recess 3d and can be made stationary. Finally, the grid 5 is fixed to the bottom surface of the recess 3d with the grid fixing jig 6 (FIG. 3C).
Through the above steps, the grid can be more securely attached to a predetermined position above the through hole 3c without damaging the grid 5.

FIG. 4 is a schematic process diagram of the method for removing the thin grid 5 for an electron microscope according to the present invention.
FIG. 4A shows a state in which the grid 5 is accommodated in the recess 3 d of the sample holder 3. In the removing method of the present invention, the jig 6 for fixing the grid 5 is first removed from the sample holder 3. In a state where the grid 5 is not fixed, the protrusion 1c at the tip of the grid installation auxiliary instrument 1 protrudes from the bottom surface of the transmission electron hole 3c of the sample holder 3 toward the top surface, and the flat grid 5 is slightly lifted (FIG. 4 ( b)). Since the diameter of the grid 5 is larger than the diameter of the cylindrical protrusion 3c, the end of the grid 5 protrudes beyond the circle of the protrusion 1c. Furthermore, since there is a slight gap between the grid 5 and the hole surface of the sample holder 3, the tip of the tweezers 4 can be easily caught under the frame portion of the grid 5, and the grid 5 can be sandwiched.

In the case of a semicircular grid, the flat grid frame and the cylindrical projection contact each other, but the thickness of the sample flake is sufficiently smaller than the thickness of the grid frame, so that even if it contacts, it will not be damaged. After gripping and lifting the end of the grid 5 with the tweezers 4, the protrusion 1 c protruding from the bottom of the through hole 3 c is lowered, and the auxiliary instrument 1 is slowly removed from the sample holder 3 (FIG. 4C).
Through the above steps, the observation sample can be collected in a state of being placed on the thin slice grid 5 for an electron microscope without deforming or flying the grid 5 or dropping it from the sample holder hole 3c.

  Next, the structure and the like of the auxiliary device according to the present invention will be described with reference to FIGS.

  As for the shape of the minute protrusion part 1c with which the front-end | tip of the grid installation auxiliary tool based on this invention is equipped, it is desirable that it is the cylindrical protrusion 7a shown in FIG. In the case of an elongated shape such as a cone or a needle, the grid may be damaged or the sample may be damaged by coming into contact with the sample piece attached to the grid. Further, in the case of a cube or a rectangular parallelepiped, there is a risk of damaging the grid or the sample adhering to the grid because the portion is sharp at 90 °. The diameter of the cylinder is not limited as long as it can be inserted into the transmission electron hole of the sample holder. If the diameter exceeds 2.0 mm, it is difficult to insert the sample holder into the electron transmission hole of the sample holder. On the other hand, if the diameter of the circle is less than 1.0 mm, it may deviate from the center of the transmission electron hole and protrude from the end. The part may be damaged.

  Further, the shape of the protrusion of the auxiliary device may be a cylindrical shape as shown in the right view of FIG. In the case of the cylinder 7b, it is desirable that the thickness of the cylinder frame is such that the grid frame is stably placed flat when the grid is placed. If the grid material is not damaged or deformed in the cylinder frame part, the cylinder cylinder The thickness of the frame is not particularly specified, but preferably the frame thickness is 0.5 mm or more.

The height of the column or cylinder is preferably about 0.5 mm to 3 mm. The thickness d of the sample holder 3 is about 0.8 mm, and the thickness t of the central recess 3d is even thinner, about 0.1 to 0.3 mm (see FIG. 3B). The height obtained by subtracting this is the height protruding from the holder hole of the protrusion. If the height of the protrusion is higher than 3.0 mm, the grid will be inclined and the grid bottom will become unstable because it is arcuate, and it may fall down to the surroundings. There is danger. In addition, when the grid is unexpectedly detached from the tweezers and dropped onto the sample holder, if the projection height is high, there is a risk that the grid will hit the projection and jump to other parts. However, if the protruding height is low, it stays still without bouncing.

  The auxiliary device 1 according to the present invention is preferably extended in a plate shape, and can be stably fixed when it comes into contact with the sample holder. Further, as shown in FIG. 6, there is a method in which the size is set to the same size as the recessed portion of the sample holder 3 without being formed into a plate shape, and the sample holder 3 is used by being placed on the base 9. A shape that is larger than the tip of the sample holder and has a handle connected to the protrusion is easier to use. Moreover, even if it is the shape bent diagonally, it becomes easy to hold by hand (refer FIG. 7). This becomes the auxiliary device 10 having a shape in which two plates bent into a “he” shape are connected. If the bending angles are the same and they are connected in the opposite direction, both ends will be parallel and handling will be easier.

  The tip of the auxiliary instrument 1, 10 that touches the sample holder is an antistatic material that is less likely to generate static electricity, and is preferably a material that does not transfer or break components to the sample holder due to volatile gas or contact. Any material can be used as long as it satisfies the requirements, and any material such as a polymer material, a metal material, or a ceramic material may be used. Static electricity may repel the grid foil, and when charged with static electricity, it may attract dirt and fine dust. In addition, since the sample holder is placed in an ultra-high vacuum, the sample holder must be kept free from contamination as much as possible. If it is, there is a risk of secondary contamination due to contact. As a method of handling the tip of the sample holder, it is desirable to periodically clean the instrument, in particular, with a solvent such as ethanol or asahicrine so that the most advanced part is not directly touched by hand and does not get sebum or dirt.

  After the FIB processing, the end of the semicircular grid with the observation sample attached to a predetermined site was pinched with tweezers and held on the grid installation position of the transmission electron microscope holder. In order to place the grid in place, the tweezers were lowered to the grid installation planned position and the tip was opened, but the tip of the tweezers and the grid adhered to each other due to static electricity. Became dragged.

  Therefore, the tweezers were once closed, and the auxiliary instrument of the present invention was installed below the tip of the sample holder. The auxiliary tool used was made of Ti, had a total length of about 8 cm including the handle from the tip, and a width of about 1 cm. The projection at the tip was about 1.8 mm in diameter and about 2.0 mm in height. Insert the protrusion of the auxiliary tool into the hole of the sample holder from below, bring the tweezers holding the grid from above, and open the tweezers again at a position where the grid slightly touches the protrusions. Distant. When the auxiliary instrument was pulled down from the sample holder, the grid stopped at a predetermined position so as to block the electron transmission hole. Thereafter, a fixing jig was fitted from above the grid, and the mounting of the grid was completed.

  An attempt was made to place the semicircular grid after FIB processing at a predetermined position on the sample holder, but one side of the end of the semicircle was partially out of the hole frame of the sample holder, and the grid was slightly tilted It became. If the position is corrected with tweezers or the like from above in this state, the grid may be flipped. Therefore, the projection of the auxiliary tool was inserted from below the sample holder hole, and the grid was lifted from the hole. After that, when the auxiliary device is inserted and the auxiliary device is moved away from the grid end hole frame and the auxiliary device protrusion is removed from the hole, the grid fits in the hole frame and prevents the downward drop. I was able to correct the position. After that, the jig for fixing the grid was put on and the installation of the grid was finished.

After the TEM observation, the jig for fixing the grid of the sample holder was removed, the auxiliary instrument was pushed below the sample holder, and the protrusion of the auxiliary instrument was inserted from the hole under the grid. Since the semicircular grid was lifted upward from the hole, the portion of the grid frame that protruded from the protrusion was grasped with tweezers, and the semicircular grid was collected. The grid could be recovered without failure.

1 ... Grid installation aid (plate)
DESCRIPTION OF SYMBOLS 1a ... Holding part 1b ... Holding part side surface 1c ... Protrusion 2 ... Grid 2a ... Mesh frame 2b ... Grid main-body part 2c ... Grid main-body part 3 ... Transmission electron microscope Sample holder 3c ・ ・ hole (through hole)
3d..Concavity 4 ... tweezers 5 ... grid 6 ... transmission electron microscope sample holder 7 ... protrusion projection 7a ... cylinder projection surface 7b ... cylinder support cylinder Projection frame 7c ... Auxiliary tool cylindrical projection hole 8 ... Grid placement aid 9 ... Transmission electron microscope sample holder base 10 ... Grid placement aid d ... Sample holder plate Thickness t ... Thickness of the recess in the sample holder

Claims (5)

A method of attaching a grid holding an observation thin sample to a predetermined position of an electron beam transmitting through-hole provided in a transmission electron microscope sample holder,
A step of inserting the protrusion of the grid installation auxiliary instrument having a columnar protrusion at the end of the plate-like base material upward from below the through hole; and
Placing the grid on the upper surface of the columnar protrusion protruding from the through hole; and
Mounting the grid to the sample holder for a transmission electron microscope, the method comprising: lowering the grid installation auxiliary tool, extracting the protrusion from the through hole, and retaining the grid in a predetermined position in the through hole. Method. A method of removing a grid for holding an observation thin piece sample held at a predetermined position of an electron beam transmission through-hole from a transmission electron microscope sample holder,
A step of lifting the grid by inserting the protrusions of the grid-installing auxiliary instrument having columnar protrusions at the end of the plate-like base material upward from below the through holes; and
A step of grasping the edge of the lifted grid and removing it from the sample holder; and a step of lowering the grid installation auxiliary device, extracting the protrusion from the through hole, and removing the auxiliary device. How to remove the grid from the transmission electron microscope sample holder.   2. The grid attachment to the transmission electron microscope sample holder according to claim 1, wherein the plate-like substrate has a shape in which two plate-like substrates having a flat plate shape or a “h” shape are connected. Method.   The transmission electron microscope according to claim 1, wherein the columnar protrusion has a height in a range of 0.5 mm to 3.0 mm and a diameter in a range of 1.0 mm to 2.0 mm. How to attach the grid to the sample holder.   The transmission electron microscope according to claim 2, wherein the columnar protrusion has a height in a range of 0.5 mm to 3.0 mm and a diameter in a range of 1.0 mm to 2.0 mm. To remove the grid from the specimen holder.