JP2013061192A - Embedding plate and embedding method of sample for cross-sectional observation - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable cross section exposing of a sample for observation to be accurately performed and the sample to be measured with accurate film thickness, and to provide an embedding plate and an embedding method allowing processing of the sample for observation such as cutting out to be easily performed.SOLUTION: An embedding plate comprises: an embedding plate body 2 having a planar mirror plane 2A on which a photocurable resin is mounted; a spacer 3A mounted on the mirror plane 2A of the embedding plate body 2; and a light transmission plate 4 mounted on the spacer 3A and regulating the thickness of the photocurable resin. The photocurable resin 5 is mounted on the mirror plane 2A, and is irradiated with visible light to be cured after regulating the thickness of the photocurable resin 5, and a resin chip 5A is manufactured. Then, a sample for observation is mounted on the resin chip 5A, and after the sample for observation is covered by an unexposed photocurable resin, another resin chip is mounted thereon to manufacture a primary sample and this primary sample is cut in accordance with a purpose.

Description

  The present invention relates to an embedding plate for embedding (embedding) a cross-section observation sample (hereinafter referred to as an observation sample) for cross-section observation with an optical microscope, a scanning electron microscope, a transmission electron microscope, etc., with a resin, It relates to the embedding method.

  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 of 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. (For example, refer to 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 (for example, see Non-Patent Document 1) is used.

JP 2004-108303 A

Nissin EM Co., Ltd. NEW Catalog page 54

  However, the above-described embedding method has a problem that the observation sample cannot be embedded horizontally in the recess of the embedding plate. That is, when the observation sample is in the form of a film, if the observation sample and the resin are placed in the recess of the silicon embedding plate and then the resin is cured, the observation sample is tilted or bent (curled) in the resin. It was difficult to embed horizontally with high accuracy. In addition, when the observation sample is placed in the recessed portion of the embedding plate and the resin is put in, a portion where the observation sample is not covered with the resin or a portion where the resin portion becomes thin may occur. Thus, if the resin adheres unevenly to the observation sample, it becomes unsuitable for cutting with an ultramicrotome. In particular, when film thickness is measured from cross-sectional observation, it is necessary to cut a horizontally held object, so it is important to embed an observation sample horizontally with high accuracy.

  The present invention has been made in view of the above-mentioned problems, and can perform cross-sectioning of an observation sample with high accuracy and measure with an accurate film thickness, and can also be used for cutting an observation sample. An object is to provide an embedding plate and an embedding method for an observation sample that can be easily processed.

In order to solve the above-described problems and achieve the object, an aspect of the present invention is an embedding plate for a cross-sectional observation sample, and an embedding plate main body having a plane on which a photocurable resin is placed, A spacer placed on the plane of the embedding plate main body, and a light transmission plate placed on the spacer and defining the thickness of the photocurable resin. The observation sample can be embedded with a plurality of flat resin chips made of a photo-curable resin irradiated with light.
As said aspect, it is preferable that several types from which a thickness dimension mutually differs are provided as a spacer.
As said aspect, it is preferable that the plane of an embedding board main body is a mirror surface when light-irradiating a photocurable resin.
As said aspect, it is preferable that the embedding board main body embeds a magnet so that it may become flush | planar with a plane, and the spacer is formed with the metal.

  Another aspect of the present invention is a method for embedding a sample for cross-sectional observation, in which a step of placing an unexposed photocurable resin on a mirror surface and the thickness of the photocurable resin are defined. Thereafter, the step of irradiating light to cure the photocurable resin to produce a resin chip, and placing the observation sample on the resin chip with the resin chip placed on the mirror surface, After covering the observation sample with a photocurable resin for exposure, placing the other resin chip, and irradiating the photocurable resin sandwiched between the resin chips with light to cure the photocurable resin. And a step of producing a sample holder in which the observation sample is sandwiched, and a step of cutting the sample holder in accordance with the purpose.

  According to the present invention, the observation sample can be accurately cross-sectioned, and can be measured with an accurate film thickness, and the observation sample can be easily cut out and embedded in the observation sample. A plate and embedding method can be realized.

FIG. 1 is a perspective view showing an embedding plate for a cross-sectional observation sample according to an embodiment of the present invention. FIG. 2 is a perspective view showing an embedding plate, a metal plate, and a transparent resin film of the cross-sectional observation sample according to the embodiment of the present invention. FIGS. 3A to 3C are side views showing a plurality of metal plates having different thicknesses, which are metal plates used in the embedding method of the present embodiment. FIG. 4 is an explanatory cross-sectional view showing a state in which a metal plate is adsorbed to the embedding plate in the embedding method of the cross-section observation sample according to the present embodiment. FIG. 5 is an explanatory cross-sectional view showing a state where a resin is potted on an embedding plate in the method for embedding a sample for cross-sectional observation according to the present embodiment. FIG. 6 is an explanatory cross-sectional view showing a process of placing a light transmitting plate on a resin and irradiating light in the method for embedding a sample for cross-sectional observation according to the present embodiment. FIG. 7 is a perspective view showing a resin chip molded in the method for embedding a cross-sectional observation sample according to the present embodiment. FIG. 8 is an explanatory cross-sectional view showing a state where the observation sample is placed on the resin chip and the resin is potted in the method for embedding the cross-sectional observation sample according to the present embodiment. FIG. 9 is an explanatory cross-sectional view showing a state in which an observation sample is sandwiched between resin chips in the method for embedding a cross-sectional observation sample according to the present embodiment. FIG. 10 is a perspective view showing a sample in which an observation sample is sandwiched between resin chips in the method for embedding a cross-sectional observation sample according to the present embodiment. FIG. 11 is a perspective view showing a state in which a sample is processed in the method for embedding a specimen for cross-sectional observation according to the present embodiment.

An embedding plate for a cross-sectional observation sample according to the present invention includes an embedding plate body having a plane on which a photocurable resin is placed, a spacer placed on the plane of the embedding plate body, and a spacer. A plurality of plate-shaped resin chips made of a photocurable resin that is light-irradiated through a light transmitting plate on a plane. In addition to the feature that the observation sample can be embedded, the following modifications are possible.
In other words, the spacers may be provided with a plurality of types having different thickness dimensions. The plane may be a mirror surface that reflects light. Further, the embedding plate body can be configured such that the magnet is embedded so as to be flush with the flat surface, and the spacer is formed of metal.

  The aspect of the method for embedding a sample for cross-sectional observation according to the present invention includes a step of placing an unexposed photocurable resin on a mirror surface and a thickness of the photocurable resin, and then irradiating with light. A step of producing a resin chip by curing the photo-curable resin, and with the resin chip placed on a mirror surface, an observation sample is placed on the resin chip, and an unexposed photo-curable resin is placed on the mirror chip. After the observation sample is covered with, a step of placing another resin chip, and the photocurable resin sandwiched between these resin chips is irradiated with light to cure the photocurable resin, and the observation sample is sandwiched. And a step of producing the sample holder (primary sample) and a step of cutting the sample holder according to the purpose to form a final sample.

Below, the detail of the embedding board and embedding method of the sample for cross-sectional observation which concerns on embodiment of this invention is demonstrated based on drawing.
As shown in FIG. 1 and FIG. 2, an embedding plate 1 for a cross-sectional observation sample according to the present embodiment includes an embedding plate body 2 having a planar mirror surface 2A on which a photocurable resin is placed, A spacer 3A placed on the mirror surface 2A of the embedding plate main body 2 and a light transmission plate 4 placed on the spacer 3A and defining the thickness of the photocurable resin are provided.

  In this Embodiment, the embedding board main body 2 is formed with the metal plate. The upper surface of the embedded plate body 2 is finished to the mirror surface 2A. In the present embodiment, the embedding plate body 2 is made of a metal plate, but a glass plate may be used as long as it is a plate-like body having a mirror surface 2A. Moreover, you may produce 2 A of mirror surfaces by the plating process with respect to the surface of the board which consists of material which does not have light reflectivity.

  Moreover, as shown in FIG. 1, the elongate magnet 2B is embed | buried so that the mirror surface 2A may become flush with the mirror surface 2A along the longitudinal direction in the width direction both sides part of the mirror surface 2A of the embedding board main body 2. As shown in FIG. The spacer 3A is formed of a metal made of a ferromagnetic material attracted to the magnet 2B, for example, 400 series stainless steel. As shown to (a)-(c) of FIG. 3, it is preferable to provide spacers 3B and 3C having different thicknesses in addition to the spacer 3A having a small thickness. The material of the spacers 3B and 3C is the same as that of the spacer 3A. These spacers 3A, 3B, and 3C are arbitrarily selected and used according to the thickness and application of the observation sample to be produced.

A light transmission plate 4 made of a transparent resin film is arranged on the pair of spacers 3A adsorbed to the magnet 2B on the mirror surface 2A of the embedding plate main body 2. The light transmission plate 4 has a thickness with a certain degree of stiffness. In addition, the thickness of the light transmission plate 4 is appropriately changed depending on the resin as the constituent material. In the present embodiment, a PET (polyethylene terephthalate) film having a thickness of about 100 μm is used as the light transmission plate 4.
The embedding plate 1 composed of such a plurality of members is observed with a plurality of plate-like resin chips made of a photocurable resin irradiated with light through the light transmission plate 4 on the mirror surface 2A, as described later. The sample can be embedded.

Next, a method for embedding a cross-sectional observation sample according to an embodiment of the present invention will be described with reference to FIGS.
First, an observation sample 6 is prepared by cutting a sample for cross-sectional observation into a strip shape or a triangular wedge shape depending on the purpose of observation.
Then, as shown in FIG. 4, spacers 3 </ b> A are adsorbed and arranged on the magnets 2 </ b> B on the mirror surface 2 </ b> A of the embedding plate body 2. In the present embodiment, since the arrangement of the spacer 3A is substantially determined by the magnet 2B, the spacer 3A can be stably arranged at substantially the same position every time the cross-sectional observation sample is manufactured.

  Next, as shown in FIG. 5, a predetermined amount (several drops) of a photocurable resin 5 is potted (resin pile) at the center of the mirror surface 2 </ b> A sandwiched between the spacers 3 </ b> A. In general, epoxy resin, methacrylate resin, styrene resin or the like is used as an embedding resin for electron microscope observation. These resins have advantages such as being easy to cut thinly and being strong against electron beams. Among these, thermopolymerizable epoxy resins and methacrylate resins require 10 to 24 hours at 60 ° C. for complete curing. Also, UV-polymerized styrene resins require 3 hours for curing under ultraviolet irradiation. Therefore, in this embodiment, a visible light curable acrylic resin is used. Since this visible light curable acrylic resin can be cured in about 1 to 3 minutes under a light irradiator, the embedding process can be performed efficiently.

  Then, after potting the unexposed photocurable resin 5, by placing the light transmitting plate 4 on the photocurable resin 5 and flattening the photocurable resin 5 as shown in FIG. The thickness of the photocurable resin 5 is defined (defined by the thickness of the spacer 3A). At this time, since the light transmission plate 4 has a predetermined rigidity, the light transmission plate 4 can be disposed horizontally when placed so as to be horizontally mounted on the pair of spacers 3A. For this reason, it becomes possible to form the upper and lower surfaces of the resin chip 5A formed between the mirror surface 2A and the light transmission plate 4 in parallel planes. Thereafter, as shown in FIG. 6, the resin chip 5 </ b> A is formed by irradiating the photocurable resin 5 with visible light through the light transmission plate 4 and curing the resin, and then the resin chip 5 </ b> A is formed as shown in FIG. 7. Remove from the mirror surface 2A. In the present embodiment, two such resin chips 5A are produced.

Next, as shown in FIG. 8, one resin chip 5A is placed on the mirror surface 2A of the embedding plate body 2, and the observation sample 6 is placed on the resin chip 5A. Potting. The photocurable resin 7 can be the same resin as the photocurable resin 5. Then, as shown in FIG. 9, another resin chip 5 </ b> A is placed so as to cover the observation sample 6 potted with the photocurable resin 7. And the photocurable resin 7 is hardened by irradiating visible light similarly to the above.
Then, as shown in FIG. 10, a disk-shaped primary sample as a sample holder can be formed, and the final sample 8 is cut by, for example, a scissors along the cutting line indicated by C1 to C4, for example. Can be produced.

According to the above embodiment, since the observation sample 6 is embedded between the flat resin chips 5A, the observation sample 6 can exist horizontally in the center of the resin. For this reason, after taking out the cross section of the sample 6 for observation, it can measure with an exact film thickness.
As in the past, for example, in the case of a cured resin made of a silicon-embedded plate, trimming with a razor or the like (removal of excess resin) took time and effort, but it was produced by the present invention. Since the primary sample can be formed into a thin plate shape, it can be easily cut out with scissors or the like.

In general, the sample holder of the ultra-high resolution scanning electron microscope is a side entry method, and the sample size is limited to a height of 5 mm and a thickness of 2 mm. Therefore, although it was too large for the silicon-embedded plate, the thickness of the resin layer in the final sample 8 can be controlled by the thickness of the resin chip 5A to be manufactured in the observation sample of the present embodiment. It can be produced in a size corresponding to the sample holder of the ultrahigh resolution scanning electron microscope.
Furthermore, since the embedding plate 1 of the present embodiment reflects light at the mirror surface 2A, when 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, which is efficient. There is an advantage that the resin can be cured.

(Other embodiments)
Although the embodiment has been described above, it should not be understood that the description and the drawings constituting a part of the disclosure of the embodiment limit the present invention. From this disclosure, various alternative embodiments, examples and operational techniques will be apparent to those skilled in the art.
For example, in the above embodiment, a visible light curable acrylic resin is used as the photocurable resin 5, but an ultraviolet curable resin may be used. Moreover, in the said embodiment, although the plane of the embedding board main body 2 was made into the mirror surface 2A, if the photocurable resin 5 is fully photosensitized and hardening reaction advances, it may not be a mirror surface.

Moreover, in the said embodiment, although the light transmissive plate 4 was comprised with the PET film, you may use the resin film or glass plate which has a light transmittance.
Furthermore, in the above embodiment, when another resin chip 5A is further stacked, the light transmission plate 4 is not used. However, for example, by selecting the spacer 3B, the observation sample 6 is sandwiched between the resin chips 5A. The light transmitting plate 4 can be pressed against the upper surface of the upper resin chip 5A so as to be stabilized, and flatness can be further ensured.

DESCRIPTION OF SYMBOLS 1 Embedding board 2 Embedding board main body 2A Mirror surface 3A, 3B, 3C Spacer 4 Light transmission board 5,7 Photocurable resin 5A Resin chip 6 Sample for observation 8 Final sample

Claims (5)

An embedding board body having a plane on which the photocurable resin is placed, a spacer placed on the plane of the embedding board body, and a thickness of the photocurable resin placed on the spacer A light transmissive plate that regulates,
An embedment plate for a cross-sectional observation sample, characterized in that the observation sample can be embedded with a plurality of flat resin chips made of a photocurable resin irradiated with light through the light transmission plate on the plane. .   The embedded plate for a sample for cross-sectional observation according to claim 1, wherein the spacer is provided with a plurality of types having different thickness dimensions.   The embedding plate for a cross-sectional observation sample according to claim 1 or 2, wherein the plane is a mirror surface.   The cross-sectional observation according to any one of claims 1 to 3, wherein a magnet is embedded in the embedded plate body so as to be flush with the flat surface, and the spacer is formed of metal. Sample embedding plate. Placing a non-exposed photocurable resin on the mirror surface;
After prescribing the thickness of the photocurable resin, irradiating light to cure the photocurable resin and producing a resin chip;
With the resin chip placed on the mirror surface, place an observation sample on the resin chip, cover the observation sample with an unexposed photocurable resin, and then place another resin chip. A step of placing;
Irradiating the photocurable resin sandwiched between the resin chips with light to cure the photocurable resin to produce a sample holder in which the observation sample is sandwiched; and
Cutting the sample holder according to the purpose;
A method for embedding a sample for cross-sectional observation, comprising:

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