JPH06273294A - Manufacture of embedded sample for observing structure - Google Patents

Abstract

PURPOSE:To provide a method for manufacturing an embedded sample for observing the structure which prevents the generation of the gap between a sample and a resin for embedding and permits the observation of the edge surface exposed outside up to the edge part free from fault. CONSTITUTION:A method for manufacturing an embedded sample 7 for observing the structure in which the inner peripheral surface and outer peripheral surface of a metal sample 1 having the outer peripheral surface, inner peripheral surface and an edge surface are embedded into a resin, and the edge surface of the metal sample 1 is supplied for observing the structure includes a process for closely attaching a thermosetting resin 4 on the outer peripheral surface of the metal sample 1 and a process for closely attaching an inside hardened body 6 which can be hardened at the normal temperature and is free from the contraction performance, on the inner peripheral surface of the metal sample 1.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing an embedded sample for observing a structure, and more specifically, a embedded sample for observing a structure in which a metal sample is embedded in a resin and an end face of the metal sample is exposed. The present invention relates to a method for manufacturing an embedded sample for tissue observation, which can be manufactured without forming a gap between a peripheral surface and a cured resin in a space surrounded by an inner peripheral surface.

[0002]

2. Description of the Related Art Usually, for example, when observing the structure of a metal sample formed in a tubular shape, the end surface of the metal sample is changed in order to clarify the structure to be observed. A so-called mirror finish for polishing is carried out.

At this time, from the viewpoint of securely holding the metal sample during polishing, polishing the tissue surface with high flatness, and not damaging the edge of the metal sample during polishing, etc. The sample is embedded in the resin.

When the metal sample to be observed is tubular and the end face structure in the radial direction is to be observed, it is necessary to fill and harden the resin not only on the outer peripheral surface side but also on the entire inner peripheral surface side of the metal sample. is there.

Therefore, a conventional example of a method for manufacturing such a textured embedded sample is described below.

First, as shown in FIG. 13, a metal sample 21 made of a metal tube having a circular radial cross-section is put on the inner bottom of a molding container 20 having an open upper part, and then FIG.
As shown in, the outer peripheral surface and the inner peripheral surface side of the metal sample 21 are filled with powder of thermosetting resin powder. At this time,
The thermosetting resin powder is carefully fed into the molding container 20 so that the upper surface of the thermosetting resin powder is substantially level with the end surface of the metal sample.

Next, the inside of the molding container 20 is kept at a high temperature and pressure to thermally cure the thermosetting resin powder.

Thereafter, the metal sample 21 in which the hardened resin is loaded in the space surrounded by the inner peripheral surface of the metal sample 21 and the hardened resin is attached to the outer peripheral surface of the metal sample 21 is taken out from the molding container 20. By polishing the end surface of the metal sample 21 into a mirror surface, the embedded sample 30 for tissue observation shown in FIGS. 15 and 16 is obtained.

However, the embedded sample 30 for tissue observation obtained by the above-mentioned manufacturing method has the following problems.

That is, when the above-mentioned thermosetting resin powder is thermoset, the thermosetting resin 22 on the outer peripheral surface side of the metal sample 21 contracts due to contraction, but adheres to the outer peripheral surface of the metal sample 21. On the inner peripheral surface side, conversely, due to contraction of the thermosetting resin 22, as shown in FIGS. 15 and 16, there is a small amount between the inner peripheral surface of the metal sample 21 and the outer periphery of the thermosetting resin 22. A gap 23 is created.

When such a gap 23 is formed, polishing water, etching liquid, or the like penetrates into the gap 23 at the stage of polishing the end surface of the embedded sample 30 for tissue observation into a mirror surface. Etc. do not easily dry and are therefore not removed, so that the polishing water or the etching solution seeps out while observing the structure of the metal sample 21. As a result, the observation of the structure of the metal sample 21 cannot be performed accurately.

Further, when the end surface of the metal sample 21 filled with the cured resin is mirror-polished, a warp occurs at the end of the metal sample 21 facing the gap 23, and the warp is peeled off during the finish polishing to remove the metal sample. 21 scratches the tissue surface to be observed,
Again, it becomes difficult to perform accurate tissue observation.

Further, a metal sample 21 filled with a cured resin
When the end surface of the metal sample 21 is polished to a mirror surface, damage such as chipping or cracking of the end portion facing the gap 23 in the metal sample 21 occurs, and if a crack or the like is to be observed from the surface of the texture of the metal sample 21, it is fatal. Will be a serious defect.

Therefore, according to the present invention, there is no gap between the sample and the resin for embedding, and the end face exposed to the outside can be used for observation up to the end without defects. It is an object of the present invention to provide a method for manufacturing an embedded sample for tissue observation.

[0015]

The invention according to claim 1 for solving the above-mentioned problems is characterized in that it has an outer peripheral surface, an inner peripheral surface and an end surface and is hardened to the outside of the outer peripheral surface of a metal sample arranged in a container. Step of filling a thermosetting resin and curing the same, and second step of filling a space surrounded by an inner peripheral surface of the metal sample with a room temperature curable resin which is non-shrinkable upon curing and curing the resin The method for producing an embedded sample for observing a tissue according to claim 2, wherein the metal sample has a tubular shape.
The method for manufacturing an embedded sample for tissue observation according to claim 3, wherein the invention according to claim 3 is the embedded sample for tissue observation according to claim 1, wherein the second step is performed after the first step. It is a manufacturing method, and the invention according to claim 4 is
The method for producing a tissue observation embedded sample according to claim 3, which is a first step of filling a curable resin and curing the resin in a state where an opening portion opened by an end surface of the metal sample is closed.

[0016]

According to the method of manufacturing an embedded sample for observing a structure of claim 1, the outer periphery of the metal sample can be formed without simultaneously forming a cured body of a curable resin on the outer peripheral surface side and the inner peripheral surface side of the metal sample. The formation of the hardened body of the curable resin on the surface side and the formation of the hardened body of the curable resin on the inner peripheral surface side of the metal sample are performed independently, and the inner peripheral surface side of the metal sample does not undergo curing. Since the shrinkable room temperature curable resin is cured, no gap is generated between the cured body cured on the inner peripheral surface side of the metal sample and the inner peripheral surface of the metal sample.

According to the method for manufacturing an embedded sample for observing a tissue according to claim 2, since the shape of the metal sample is tubular, it is possible to easily perform positioning when arranging it in the molding container. Remarkably good.

According to the method for manufacturing an embedded sample for observing a structure of claim 3, after the hardened body of the curable resin is formed on the outer peripheral surface side of the metal container, it is room temperature curable on the inner peripheral surface side of the metal container. Since the cured product of the resin is formed, it is not deformed by heating when the cured product of the room temperature curable resin is formed, and therefore the gap between the inner peripheral surface of the metal container and the cured product of the room temperature curable resin is more reliably eliminated. The embedded sample for texture observation is manufactured.

According to the method for manufacturing an embedded sample for observing a structure of claim 4, when the curable resin is supplied to the outer peripheral surface side of the metal sample, the opening opened by the end face of the metal sample is closed. Therefore, there is no concern that the curable resin will enter the inner peripheral surface side of the metal sample, and the operation of supplying the curable resin will be facilitated.

[0020]

The method of the present invention will be described in detail below.

First, as shown in FIG. 1, a metal sample 1 made of a metal tube having a circular radial cross-section is put on the inner bottom of a molding container 2 having an open upper part, and then as shown in FIG. In addition, the upper end surface and the inner peripheral surface of the metal sample 1 are shielded by the lid 3 having the flat plate portion 3a covering the entire upper end surface of the metal sample 1 and the projection 3b protruding downward from the flat plate portion 3a. At the same time, the curable resin 4a is filled between the outer peripheral surface of the metal sample 1 in the molding container 2 and the inner wall of the molding container 2. At this time, the supply amount of the curable resin 4a is set to the metal sample 1
It is preferable to adjust the upper surface of the curable resin 4a supplied into the gap between the outer peripheral surface of the metal sample 1 and the inner wall of the molding container 2 so as not to rise above the end surface of the metal sample 1.

Here, the curable resin is not particularly limited as long as it is a resin which is cured by heat, radiation, light, a curing agent, etc., and examples thereof include diallyl phthalate resin, thermosetting aromatic polyimide, bismaleimide type polyimide, An epoxy resin, a phenol resin, etc. can be mentioned. Among these, diallyl phthalate resin is preferable. The form of the curable resin to be supplied is not particularly limited, and curable resin powder, curable resin pellets, liquid curable resin, and the like can be used as appropriate.

Next, the molding container 2 is heated and pressurized to cure the curable resin 4a.

At this time, even if the curable resin 4a shrinks by heat, the object of the present invention is not impaired. Since the thermosetting resin contracts during curing, the cured body and the outer peripheral surface of the metal sample 1 are in close contact with each other, and no gap is generated.

After that, the metal sample 1 having the outer hardened body 4 integrally bonded on the outer peripheral surface side is taken out from the molding container 2 together with the lid body 3, cooled, and then the lid body 3 is removed, as shown in FIG. Thus, the metal sample 1 in which the outer hardened body 4 is in close contact with the outer peripheral surface side of the metal sample 1 is obtained.

The inner peripheral surface of the metal sample 1 exposed by removing the lid 3 without taking out the metal sample 1 having the outer hardened body 4 integrally bonded to the outer peripheral surface side together with the lid 3 from the molding container 2. A room temperature curable resin 6a may be filled in the space surrounded by the space as described below.

Next, the metal sample 1 having the outer hardened body 4 adhered to the outer peripheral surface is placed on the jig 5 as shown in FIG. 4, and the room temperature curable resin 6a is placed on the inner peripheral surface of the metal sample 1. To fill. In this state, the room temperature curable resin 6a is cured at room temperature. When the room temperature curable resin 6a is filled, it is desirable that the outer cured body 4 and the metal sample 1 be sufficiently cooled. Sufficient cooling is sufficient if it is cooled to room temperature, but if sufficient cooling is performed when the room temperature curable resin 6a is filled, expansion, carbonization, bubble generation, etc. of the cured body 4 will occur. You don't have to come.

Here, the room temperature curable resin in the present invention may be any resin that cures at room temperature and does not shrink when cured. In addition, the above-mentioned "normal temperature" usually means room temperature, and it means that slight heating may be performed as long as the object of the present invention is not impaired. In the present invention, heating from room temperature to about 10 ° C. is allowed even if it is said that heating is performed at room temperature. Further, the term "non-shrinkability" means that the "shrinkability" upon curing is small as long as the object of the present invention is not impaired. Epoxy resin and the like can be cited as a preferred example of the non-shrinkable room temperature curable resin for curing in the present invention.

After being hardened as described above, the outer hardened body 4 is formed on the outer peripheral surface of the metal sample 1 as shown in FIGS.
Embedded in the inner periphery of the metal sample 1 and the inner cured body 6 of the room temperature curable resin is closely adhered to the inner periphery of the metal sample 1 without a gap. A sample 7 can be obtained.

According to such a manufacturing method, the metal sample 1
There is no gap on the outer peripheral surface and the inner peripheral surface, and polishing water or etching liquid enters the gap 12 in the polishing step as in the conventional example, warpage occurs, and further, there is no chip or crack at the end. This can be prevented from occurring, and the entire end surface of the metal sample 1 can be used for observation up to the end without defects.

In place of the lid 3 that covers the entire upper end surface of the metal sample 1, a disc-shaped lid 8 as shown in FIG.
Alternatively, as shown in FIG. 8, a flat plate portion 9a that covers the entire upper end surface of the metal sample 1 and a projecting portion that projects downward from the flat plate portion 9a and that extends to the vicinity of the other end surface of the metal sample 1 It is also possible to use the lid 9 having 9b.

Next, another embodiment method of the present invention will be described with reference to FIGS.

First, as shown in FIG. 9, the metal sample 1
Is placed on the jig 11, and on the inner peripheral surface side of the metal sample 1,
A room temperature curable resin 6a which is room temperature curable and has no shrinkage is filled. In this state, the room temperature curable resin 6a is cured at room temperature to form the inner cured body 6 on the inner peripheral surface of the metal sample 1. Since the room temperature curable resin 6a is non-shrinkable, the inner hardened body 6 is formed in close contact with the inner peripheral surface of the metal sample 1.

Next, as shown in FIG. 10, the metal sample 1 on which the inner hardened body 6 is formed in close contact is placed on the inner bottom portion of the molding container 2 having an open upper part, and the inner wall of the molding container 2 and the metal. A curable resin 4a is filled between the outer peripheral surface of the sample 1. In this case, the amount of the curable resin 4a to be filled is such that the upper surface of the curable resin 4a supplied between the inner wall of the molding container 2 and the outer peripheral surface of the metal sample 1 exceeds the end surface of the metal sample 1. Alternatively, as shown in FIG. 11, filling may be performed until the end surface of the metal sample 1 and the upper surface of the inner hardened body 6 are hidden.

In any case, the filled curable resin 4a
Cure. In this case, the curable resin 4a is preferably cured at room temperature by radiation, light or a curing agent. When the curable resin 4a is cured by heating,
This is because the inner hardened body 6 may be altered, deteriorated, or deformed.

The curable resin 4a was filled until the upper surface of the inner hardened body 6 was hidden, and when the hardened resin 4a was cured, the metal sample 1 integrally joined with the outer hardened body 4 was taken out from the molding container 2, After cooling, as shown in FIG. 11, a position slightly lower than the end surface of the metal sample 1 is horizontally cut together with the outer hardened body 4 and the inner hardened body 6 so that as shown in FIG. Similarly to the case shown in FIGS. 5 and 6, the outer hardened body 4 shrinks and adheres to the outer peripheral surface of the metal sample 1 by heat, and the inner peripheral surface of the metal sample 1 has
It is possible to obtain the embedded sample 7A for texture observation, in which the inside cured body 6 that is curable at room temperature and has no shrinkage is in close contact without a gap.

The embedding sample 7A for tissue observation can also exhibit the same operational effects as the embedding sample 7 for tissue observation.

Next, a concrete experimental example will be shown.

(Experimental example) Diameter 30 mm, length 15 mm,
And a stainless steel pipe with a wall thickness of 3 mm is placed in the forming chamber of a forming device (Aeropress MPO-520 manufactured by Refinetech), and a stainless steel disc with a thickness of 2.5 mm and a diameter of 30 mm is fitted exactly on the upper end opening of the steel pipe. Placed in. Then, the molding chamber was filled with diallyl phthalate resin powder (manufactured by Refinetech) until the filling depth of the diallyl phthalate resin powder reached the upper end surface of the stainless steel pipe. Then 140 ℃
While heating to 3, the pressure was increased to 3 atm, and heat curing was performed for 7 minutes.

After heat curing, the molding chamber is cooled, and after reaching the room temperature at room temperature, the interior space of the stainless steel pipe is filled with epoxy resin (made by Konishi Bond, quick curing epoxy quick menter) and kept at room temperature. Cured.

After the room temperature curing, the stainless steel pipe with the cured product integrally fixed was taken out from the molding chamber, the diallyl phthalate cured product, the stainless steel pipe and the epoxy resin cured product were horizontally cut, and the exposed end surface of the stainless steel pipe was observed. No gap was observed between the inner peripheral surface of the stainless steel pipe and the cured epoxy resin.

The present invention is not limited to the above-described embodiments, but various modifications can be made within the scope of the gist thereof.

[0043]

According to the present invention described in detail above, the following effects are obtained.

According to the first aspect of the present invention, the curable resin shrinks and adheres to the outer peripheral surface of the metal sample when it cures, and the inner peripheral surface of the metal sample contracts at room temperature with curability. The non-resistive resin will cure without gaps,
As a result, there is no gap between the outer peripheral surface and the inner peripheral surface of the metal sample, and the entire end surface of the metal sample can be used for observation up to the end without defects and for the structure observation embedded sample. It is possible to provide a method for producing an embedded sample for observing a tissue capable of obtaining the above.

According to the second aspect of the present invention, since the tubular metal sample is used, the positioning of the metal sample during curing is easy and the manufacturing operation is simple.

According to the third aspect of the present invention, the curable resin is first cured on the outer peripheral surface of the metal sample, and then the room temperature curable and non-shrinkable resin is cured on the inner peripheral surface of the metal sample. Therefore, a thermosetting resin can be adopted as the curable resin to be cured on the outer peripheral surface, and the type of curable resin is not limited. Further, since the room temperature is adopted as the thermal condition for curing the resin in the inner peripheral surface, it is possible to prevent the already cured outer cured body from thermal deterioration, deterioration, bubble generation and the like.

According to the invention of claim 4, claim 3
In the method described in (1), since the upper end opening of the metal sample is closed by the lid member, when supplying the curable resin, it is necessary to pay attention so that the interior space of the metal sample is not filled with the curable resin. In addition, the filling operation of the curable resin is easy and simple.

[Brief description of drawings]

FIG. 1 is a cross-sectional view showing a manufacturing process in an embodiment of a method for manufacturing an embedded sample for texture observation according to the present invention.

FIG. 2 is a cross-sectional view showing the manufacturing process of the method of this embodiment.

FIG. 3 is a perspective view showing a manufacturing process of the method of the present embodiment.

FIG. 4 is a cross-sectional view showing a manufacturing process of the method of the present embodiment.

FIG. 5 is a perspective view of an embedded sample for tissue observation obtained by the method of this example.

FIG. 6 is a cross-sectional view of an embedded sample for tissue observation obtained by the method of this example.

FIG. 7 is a perspective view showing another example of the lid body used in the method of the present embodiment.

FIG. 8 is a perspective view showing still another example of the lid body used in the method of the present embodiment.

FIG. 9 is a cross-sectional view showing a manufacturing process in another embodiment of the method for manufacturing a textured embedded sample of the present invention.

FIG. 10 is a cross-sectional view showing a manufacturing process in a method of another embodiment.

FIG. 11 is a cross-sectional view showing a manufacturing process in a method according to another embodiment.

FIG. 12 is a cross-sectional view of a tissue observation embedded sample obtained by another example method.

FIG. 13 is a cross-sectional view showing a manufacturing process of a conventional manufacturing method.

FIG. 14 is a cross-sectional view showing a manufacturing process of a conventional manufacturing method.

FIG. 15 is a perspective view of a tissue observation embedded sample obtained by a conventional manufacturing method.

FIG. 16 is a cross-sectional view of a tissue observation embedded sample obtained by a conventional manufacturing method.

[Explanation of symbols]

 1 Metal Sample 2 Molded Container 3 Lid 4 Thermosetting Resin 5 Jig 6 Resin 7 Embedded Sample for Tissue Observation

Claims (4)

[Claims] 1. A first step of filling a curable resin outside an outer peripheral surface of a metal sample having an outer peripheral surface, an inner peripheral surface and an end surface and arranged in a container and curing the resin, and an inner peripheral surface of the metal sample. And a second step of filling a non-shrinkable room temperature curable resin into the space surrounded by the surface and curing the resin. 2. The method for producing a tissue observation embedded sample according to claim 1, wherein the metal sample has a tubular shape. 3. The method for manufacturing an embedded sample for tissue observation according to claim 1, wherein the second step is performed after the first step. 4. The method for producing a tissue observation embedded sample according to claim 3, which is a first step of filling a curable resin and curing the resin in a state in which an opening opened by an end surface of the metal sample is closed. .