JP2014167393A - Embedding plate for section observation sample - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an embedding plate and an embedding method for an observation sample in which the sample is easily embedded, there is no problem that the embedded sample is not easily peeled off, and a film thickness can be accurately measured, even if the sample is in a film shape.SOLUTION: An embedding plate for a flat plate-like section observation sample embedded with photocurable resin irradiated with light through a light transmission plate, on a mirror-like flat surface, comprises: an embedding plate body 2 having the mirror-like flat surface on which photocurable resin 7 is mounted; a spacer 5 for regulating a thickness of the photocurable resin mounted on the mirror-like flat surface of the embedding plate body; and a light transmission plate 6 mounted on the spacer, to the photocurable resin. A silicon sheet 10 is provided on the surface in contact with the photocurable resin of the embedding plate body and the light transmission plate.

Description

  The present invention relates to an embedding plate for a cross-sectional observation sample for embedding (embedding) a cross-sectional observation sample for cross-sectional observation with an optical microscope, a scanning electron microscope, a transmission electron microscope, or the like.

  There is a method of using an ultramicrotome (cross-section cutting machine) for cross-section preparation of an observation sample in cross-section observation of an observation sample that performs cross-section observation with an optical microscope, a scanning electron microscope, a transmission electron microscope, or the like. In preparing an observation sample with this ultramicrotome, a method for embedding the observation sample in a transparent resin is known in order to prevent the observation sample from being distorted by the impact of cutting or to facilitate handling. (Patent Document 1).

  The embedding plate is formed with a recess for accommodating the observation sample and enclosing it with a resin. For example, as a material-based sample embedding plate, a plate called a silicon embedding plate is used (Non-Patent Document 1).

  A silicon embedding plate is generally used as an embedding plate used for embedding a material-based sample, but there is a problem that the sample cannot be embedded horizontally. For example, when the sample is in the form of a film, the sample and the resin are placed in the concave part of the silicon embedding plate, and then the resin is often cured, the sample may tilt or curl in the resin. It is difficult to embed. In addition, when the sample sinks to the bottom, a portion where the sample is not covered with resin or a portion where the resin portion becomes thin and is not suitable for cutting is formed.

  In order to solve the above-mentioned problem, after the step of placing an unexposed photocurable resin on the mirror surface and the thickness of the photocurable resin are prescribed, light is irradiated to cure the photocurable resin. After the step of producing the resin chip and placing the observation sample on the resin chip in a state where the resin chip is placed on the mirror surface, the observation sample is covered with an unexposed photocurable resin. And a step of placing another resin chip, and irradiating light to the photocurable resin sandwiched between the resin chips to cure the photocurable resin to produce a sample holder in which the observation sample is sandwiched. There has been proposed a method including a process and a process of cutting the sample holder according to the purpose. However, there is a problem that the cured resin is difficult to peel off.

JP 2004-108303 A

Nissin EM Co., Ltd. NEM Catalog 2012, page 58

  To provide an embedding plate for a cross-sectional observation sample that enables easy measurement even when the sample is in the form of a film, and the embedded sample does not have a problem that it is difficult to peel off, and enables accurate film thickness measurement. There is.

As means for solving the above-mentioned problems, the invention according to claim 1 includes an embedding plate body having a mirror-like plane on which a photocurable resin is placed, and the mirror-like shape of the embedding plate body. A spacer for defining a thickness of a photocurable resin placed on a plane; and a light transmissive plate placed on the spacer, the light curable resin,
On the mirror-shaped plane, a flat plate-shaped cross-section observation sample embedding plate embedded with a photocurable resin irradiated with light through the light transmission plate,
An embedding plate for a cross-sectional observation sample, wherein a silicon layer is provided on the surface of the embedding plate main body and the light transmission plate in contact with the photocurable resin.

  The invention according to claim 2 is characterized in that the spacer is provided with a plurality of types having different thickness dimensions, and the thickness of the flat observation sample is 1 to 4 mm. It is an embedding board for cross-sectional observation samples of description.

  The invention according to claim 3 is the embedded plate for a cross-sectional observation sample according to claim 1 or 2, wherein the silicon layer is a silicon resin sheet.

  The sample can exist horizontally in the center of the resin, and the embedded sample can be easily peeled off from the embedding plate body or light transmission plate having a mirror-like flat surface. An embedding plate for a cross-sectional observation sample that can be measured with an accurate film thickness can be provided.

It is a section conceptual diagram showing composition of an embedding board for section observation samples of the present invention. It is a whole perspective conceptual diagram explaining the embedding board main body of this invention. It is a whole perspective conceptual diagram explaining the state which attached the spacer to the embedding board main body of this invention. It is a plane conceptual diagram explaining the embedding board main body of this invention. It is a plane conceptual diagram explaining the state which attached the spacer to the embedding board main body of this invention. It is a cross-sectional conceptual diagram explaining the embedding board main body of this invention. It is a cross-sectional conceptual diagram explaining the state which attached the spacer to the embedding board main body of this invention. It is a side surface conceptual diagram which shows the several spacer which is a spacer which consists of a metal plate, and differs in thickness mutually. It is a side surface conceptual diagram which shows a light transmissive board.

  DESCRIPTION OF EMBODIMENTS Hereinafter, embodiments for carrying out the present invention will be described in detail with reference to the drawings. FIG. 1 shows an embedding plate for a cross-sectional observation sample according to the present invention. An embedding plate main body 2 has a mirror surface 3, and a silicon layer 10 is provided on the surface thereof. A magnet 4 for fixing the spacer 5 is embedded in a part.

  The observation sample 8 is embedded with a photocurable resin 7, and after pressing the light transmitting plate 6 provided with a silicon sheet 10 on the surface from above, the photocurable resin 7 is cured by irradiation with visible light. Let

  FIG. 2 is an overall perspective conceptual diagram for explaining the embedding board main body 2 of the present invention, in which a silicon sheet 10 is attached to a mirror surface. The silicon sheet is notched so that the magnet comes out on the surface, and the silicon sheet and the magnet surface are the same height.

As shown in FIG. 3, a spacer 5 made of a metal plate is attached to the magnet 4. As shown in FIG. 8, different thicknesses of the metal plate serving as the spacer 5 are prepared and can be changed depending on the thickness of the sample and the application. The spacer 5 is attached to a magnet. For example, 400 series stainless steel may be used, or a magnet may be used.

  FIG. 4 is a plan view for explaining the embedding board main body of the present invention, showing the positional relationship of the magnets 3 for fixing the spacer 5, and FIG. 5 showing the state in which the spacer 5 is fixed.

  FIG. 6 is a cross-sectional view of the embedding board main body 2 of the invention, and shows that the silicon sheet 10 and the magnet 4 surface have the same height. FIG. 7 shows a state in which the spacer 5 made of a metal plate is attached. FIG. 9 shows a silicon sheet 10, and a magnet window 11 is provided so that the silicon sheet and the magnet surface have the same height.

  In the case of a cured resin made of a silicon-embedded plate, trimming with a razor or the like (scraping off the excess resin) took time and effort. Because it is plate-shaped, it can be easily cut off with scissors.

  In the case of an embedding plate in which the mirror surface 3 or glass is in direct contact with the photocurable resin 7, the cured resin is difficult to peel off from the embedding plate 1, and the cured resin may be cracked. Therefore, the cured embedding resin can be easily peeled off.

  The sample holder of the ultra-high resolution scanning electron microscope is a side entry method, and the sample size is limited to 5 mm in length and width, and the thickness is 2 mm. Since the thickness of the resin can be controlled if it is a cured resin, it can be used as a sample holder.

  Since the embedding plate 1 of the present invention is composed of the mirror surface 3, when the resin is reflected and the resin is cured by the light irradiator, the light that has passed through the sample and the light that has hit the periphery of the sample is reflected, and the resin is efficiently applied. It can be cured.

  An epoxy resin, a methacrylate resin, a styrene resin or the like is often used as an embedding resin for electron microscope observation. These resins have advantages such as easy slicing and resistance to electron beams, but thermosetting epoxy resins and methacrylate resins require 10 to 24 hours at 60 ° C. for complete curing. Even UV-polymerized styrene resins require 3 hours to cure under ultraviolet irradiation. If a visible light curable acrylic resin is used, the visible light curable acrylic resin is used for embedding in the present invention because it can be cured in 1 to 3 minutes under a light irradiator.

  The present invention is an embedding plate 1 in which a magnet 4 is embedded at both ends of a mirror and a silicon sheet 10 is attached to a mirror surface 3, and a metal plate is attached to both ends for use. The thickness of the metal plate used as the spacer 5 is different from each other and can be changed depending on the thickness of the sample and the application. The thickness of the spacer 5 becomes the thickness of the photo-curing resin 7, and in the normal case, the total thickness of the embedding resin is suitably 1 to 4 mm. The spacer 5 is attached to the magnet 4 and, for example, 400 series stainless steel is used.

  The embedding plate 1 may be a glass plate having a metallic luster or a glass plate having a normal reflection layer. As the silicon resin on the mirror surface, a transparent resin that transmits light is used. Although a film is used in addition to the embedding plate, a film that is thick to some extent and strong is good. For example, a PET film having a thickness of about 100 μm is used.

A procedure for preparing a sample for cross-sectional observation will be described with reference to the drawings. A spacer 4 having the same thickness as shown in FIG. 3 is attached to the magnet 4 embedded in the embedding plate body 2 having the silicon sheet 10 shown in FIG. Next, a few drops of acrylic resin is applied to the vicinity of the center of the embedding board main body 2, and a film as a sample is covered from above.
Further, after placing the light transmitting plate 6 and flattening the resin, the resin was cured in a light irradiator and peeled off from the embedding plate, thereby producing an observation 8.

  The cured resin is in contact with the silicon sheet 10 and the embedding resin can be easily peeled off.

DESCRIPTION OF SYMBOLS 1 ... Embedded board 2 ... Embedded board main body 3 ... Mirror surface 4 ... Magnet 5 ... Spacer 6 ... Light transmission board 7 ... Photocurable resin 8 ... Observation Sample 9 ... Final sample 10 ... Silicon sheet 11 ... Magnet window

Claims (3)

An embedding board body having a mirror-like plane on which the photocurable resin is placed; a spacer that defines the thickness of the photocurable resin placed on the mirror-like plane of the embedding board body; Mounted on the spacer, the light curable resin, and a light transmission plate,
On the mirror-shaped plane, a flat plate-shaped cross-section observation sample embedding plate embedded with a photocurable resin irradiated with light through the light transmission plate,
An embedded plate for a cross-sectional observation sample, wherein a silicon layer is provided on the surface of the embedded plate main body and the light transmitting plate in contact with the photocurable resin.   The embedded plate for a cross-sectional observation sample according to claim 1, wherein the spacer is provided with a plurality of types having different thickness dimensions, and the thickness of the flat observation sample is 1 to 4 mm.   The embedded plate for a cross-sectional observation sample according to claim 1, wherein the silicon layer is a silicon resin sheet.