JPH0921735A - Sample embedding body and production thereof - Google Patents

Abstract

PROBLEM TO BE SOLVED: To form an ultrathin cut piece suitable for quality inspection using a transmission microscope(TEM) efficiently while suppressing the delamination of a magnetic metal layer by adding fine particles to a resin for embedding a magnetic tape. SOLUTION: An epoxy resin is admixed with DDS and MNA at a specified ratio and stirred under normal temperature and then admixed with DMP and stirred. Subsequently, it is admixed with SiO2 powder (mean particle size; 0.01μm) by a very small quantity at a time and stirred to produce a dissolved embedding resin 4 containing fine particles. The dissolved resin 4 is poured into a molding die and the surface is flattened before being cured. A magnetic tape (sample) comprising a resin film (PET) layer 3a and a magnetic layer 3b of deposited metal is then mounted thereon with the magnetic layer 3b facing the resin 4. Finally, a resin 5 containing no fine particle of SiO2 is fed thereon and cured to form a sample embedding body. The magnetic layer 3b is not stripped off from the PET layer 3a or resin 4 at the time of dicing ultrathin cut pieces and an ultrathin cut piece (TEM sample) suitable for quality inspection can be obtained.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technique for producing a sample embedding body used for quality inspection by a transmission electron microscope (TEM), for example.

[0002]

Observation of a cut surface is one of the quality inspections for magnetic recording media. At the time of this inspection, a sample embedding body is produced in which the cut magnetic recording medium (sample) is embedded with resin. Then, an ultrathin section having a thickness of about several tens nm is cut out from this sample embedding body, and the cut surface is observed by TEM.

By the way, when an ultrathin section is cut out from a sample embedding body, the vapor-deposited metal magnetic layer of the sample is peeled off from the PET layer which is the support, or the metal magnetic layer is peeled off from the facing embedding resin. It often happens. Therefore, T
An ultrathin section suitable for quality inspection by EM cannot be obtained efficiently.

[0004]

[Means for Solving the Problems] In order to solve the above-mentioned problems, as a result of intensive studies, it was found that the metal magnetic layer was peeled off from the PET layer or the embedding resin. It has been found that a large shear force is generated between the layers when cutting out the slice. That is, since the sample embedding body has a structure in which a hard metal vapor deposition film is interposed between two soft layers of the embedding resin and the PET film, when cutting this, an excessive force is applied between the layers. It works.

Therefore, the present inventor thought that the above-mentioned drawbacks could be overcome by making the hardness of the resin facing the metal vapor deposition layer side and embedding the metal close to the hardness of the metal vapor deposition layer. Then, as a result of attempting to improve the resin hardness by various methods, it was found that the addition of a predetermined amount of fine particles appropriately increases the hardness of the resin and enables the sample embedded body to be satisfactorily cut. That is, if a resin containing fine particles is used, an excessive shearing force does not act between layers,
It has been found that peeling of the metal magnetic layer does not easily occur, and an ultrathin section suitable for quality inspection using a TEM can be efficiently obtained.

As a result of further research, it was found that even if a resin containing fine particles is provided only on the side of the sample facing the metal magnetic layer, it is possible to cut without peeling the metal magnetic layer. . The present invention has been made based on these findings, and by providing a sample embedding body which is unlikely to cause a defect in a sample when cutting out an ultrathin section, and which can efficiently obtain an ultrathin section suitable for quality inspection. is there.

The above object of the present invention is achieved by a sample embedding body in which a sample is embedded with a resin, wherein the resin contains fine particles. . A sample embedding body in which a sample on which a hard film is formed is embedded with a resin, wherein the resin provided on at least the side facing the hard film of the sample contains fine particles. Is achieved by the sample embedding medium.

A method for producing a sample embedding body in which a sample having a hard film formed thereon is embedded with a resin, wherein at least the side of the sample facing the hard film is
This is achieved by a method for producing a sample embedding body, which is characterized in that a resin containing fine particles is used. A method for producing a sample-embedded body in which a sample on which a hard film is formed is embedded with a resin, comprising a step of filling a mold with a resin containing fine particles to a predetermined height, and This is achieved by a method for producing a sample embedding body, which comprises a step of placing a hard film of the sample on a resin surface so as to face it, and a step of filling a resin on the sample.

The fine particles added to or contained in the resin may be either inorganic or organic. Examples of inorganic materials include silicon dioxide such as quartz and hydrous silicic acid, metal oxides such as aluminum oxide, chromium oxide and iron oxide, or metals such as manganese, iron and cobalt, carbon black and graphite. Fine powder can be used. Examples of organic compounds include plastics such as polyester, polyethylene and polypropylene, and other high melting point low molecular weight compounds. Of course, two or more kinds of substances may be mixed and used.

[0010]

1 to 5 show an embodiment of the present invention. FIG. 1 is a perspective view of a mold used for producing a sample embedding body, and FIG. 2 is a producing method of a sample embedding body. 3 is a sectional view of the prepared sample embedding body, and FIG. 5 is a reference diagram of an ultrathin section cutting step.

In each figure, reference numeral 1 denotes a mold made of silicon resin or the like, and an octagonal recess 2 is formed in the center. A magnetic tape (sample) 3 is composed of a resin (PET) film layer 3a as a support and a vapor-deposited metal magnetic layer 3b. The sample has a length of a few mm and a maximum width of 1
The one cut into a wedge shape of about mm is used.

A method for producing a sample embedding body using the mold 1 will be described below with reference to FIG. First, DDSA and MNA were added to the epoxy resin at a predetermined ratio, and the mixture was stirred at room temperature for 15 minutes.
Stir for 0 minutes. After 10 minutes, a small amount of SiO ₂ powder (average particle diameter 0.01 μm) is added while stirring. The mixture is further stirred for 10 minutes to obtain a resin embedding medium containing fine particles.

Next, the resin embedding agent 4 thus obtained is poured into the concave portion 2 of the mold 1 to about half its depth,
After the surface is flattened by a press, it is cured in a vacuum oven at 60 ° C. for about 10 hours. Then, the sample 3 is placed so that the metal magnetic layer 3b (indicated by diagonal lines in FIG. 2) is on the lower side, that is, the metal magnetic layer surface 3b faces the cured resin 4.

Then, a resin embedding medium 5 having the same components as the above resin embedding medium except that SiO ₂ powder was not added was poured into the mold 1, and the pressure was reduced to about 24 at 60 ° C. in a vacuum oven.
After the time-curing treatment, the mold 1 was taken out. FIG. 3 shows a cross section of the sample embedded body (first embodiment) thus produced. As can be seen from this figure, in the sample embedding body, the metal magnetic layer 3b of the sample 3 faces the resin 4 containing SiO ₂ particles, while the PET layer 3a faces the resin 5 containing no SiO ₂ particles. This prevents the metal magnetic layer 3b from peeling from the PET layer 3a and the resin 4 when cutting out an ultrathin section.

Table 1 shows the component amounts of the resin 4 and the resin 5. Table 1 Resin 4 Resin 5 Epoxy resin 20.3 ml 20.3 ml DDSA 12.5 ml 12.5 ml MNA 11.1 ml 11.1 ml DMP 0.88 g 0.88 g SiO ₂ 0.1 g No addition Next Embodiment 2 As a sample embedding medium, carbon black powder (average particle diameter 0.01 μm) was used instead of SiO ₂ . However, the manufacturing process is the same as in the first embodiment. Table 2 shows the component amounts of the resin 6 on the metal magnetic layer side and the resin 7 on the PET layer side.

Table 2 Resin 6 Resin 7 Epoxy resin 20.3 ml 20.3 ml DDSA 12.5 ml 12.5 ml MNA 11.1 ml 11.1 ml DMP 0.88 g 0.88 g carbon black 0.1 g FIG. 4 shows a cross section of the produced sample embedding body (second embodiment).

As can be seen from this figure, in the sample embedding body, the metal magnetic layer 3b of the sample 3 faces the resin 6 containing carbon black particles, while the PET layer 3a contains the resin 7 containing no carbon black particles. Therefore, the metal magnetic layer 3b is exposed to P when cutting out an ultrathin section.
The ET layer 3a and the resin 6 are prevented from peeling off. The sample embedding body F produced as described above is set in a cutting device (microtome) and an ultrathin section is cut out, but since the work content of this is conventionally known, only an outline thereof is given here. , FIG. 5 will be described.

First, in the prepared sample embedding body F, the side where the tip of the sample 3 is located is roughly shaved manually to form a truncated pyramid. However, the tip of the sample 3 is made to overlap the center of the truncated pyramid. The sample embedding body F whose tip is processed into a truncated pyramid shape is set in a cutting device. That is, the sample embedding body F is fixed to the segment arm 8, and the tip side is adjusted to 0.
Cut to about 5 mm square.

Subsequently, a diamond knife is installed in the cutting device, and the knife boat 1 of this diamond knife is installed.
Fill 0 with water. Then, the segment arm 8 is operated so that the tip of the sample embedding body F is brought into contact with the blade 11 so that the thickness is 50
Cut out ~ 70 nm ultrathin sections. After cutting out the required number of pieces in this way, an ultrathin section floating on the water surface without sinking is constructed by bonding eyelashes to the tip of the bamboo shaft 1
2 is used to collect in the center of the knife boat 10 for easy collection.

The ultrathin section is made of copper mesh sheet 13 (lattice size 170 μm) provided with a collodion film.
It is scooped up from the water surface, after which the ultrathin section is attached to a grid and moved to observation by TEM. Actually, ultrathin sections cut out from the sample embedding bodies of the first embodiment and the second embodiment were observed by TEM (H-7000 model manufactured by Hitachi, Ltd./accelerating voltage 100 kV). As a comparative example, the metal magnetic layer side and PET
A sample embedding body was prepared using a resin embedding agent containing the components shown in Table 3 on both layer sides, and an ultrathin section cut from this sample embedding body was observed.

Table 3 Metal magnetic layer side PET layer side Epoxy resin 20.3 ml 20.3 ml DDSA 12.5 ml 12.5 ml MNA 11.1 ml 11.1 ml DMP 0.88 g 0.88 g The results of the above observations are shown in Table 4. . However, in Table 4, the ultrathin section from each of the above three types of sample embedding bodies is shown.
Peeling occurred when cutting out one by one and observing the cross-sectional conditions, especially the boundary between the metal magnetic layer and the resin (boundary α) and the boundary between the metal magnetic layer and the PET layer (boundary β). It shows the number of things.

[0022] From this result, in the case where the resin embedding agent to which the fine particles were added was used on the side of the sample embedding body facing the metal magnetic layer, there was almost no peeling between the layers in the cut ultrathin section. , It can be seen that the one suitable for quality inspection by TEM is obtained with high probability. On the other hand, in the case of using only the resin embedding agent that does not contain fine particles, most of the samples are exfoliated between the layers, and there is a large proportion that cannot be used for quality inspection by TEM. I can't.

[0023]

EFFECTS OF THE INVENTION According to the present invention, it is possible to efficiently obtain an ultrathin section suitable for quality inspection because it is difficult for a sample to have a problem when cutting out an ultrathin section.

[Brief description of drawings]

FIG. 1 is a perspective view of a mold used for producing a sample embedding body.

FIG. 2 is a process diagram relating to the production of a sample embedded body.

FIG. 3 is a cross-sectional view of the produced sample embedding body (first embodiment).

FIG. 4 is a cross-sectional view of the produced sample embedding body (second embodiment).

FIG. 5 is a reference diagram of an ultrathin section cutting process.

[Explanation of symbols]

 1 type 2 concave part 3 magnetic tape (sample) 3a PET layer 3b evaporated metal magnetic layer 4 resin containing fine particles 5 resin not containing fine particles

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Katsumi Sasaki 2606 Akabane, Kaigai-cho, Haga-gun, Tochigi Prefecture

Claims (4)

[Claims] 1. A sample embedding body in which a sample is embedded with a resin, wherein the resin contains fine particles. 2. A sample embedding body obtained by embedding a sample on which a hard film is formed with a resin, wherein the resin provided at least on the side facing the hard film of the sample contains fine particles. A sample embedding body characterized by the above. 3. A method for producing a sample embedding body in which a sample on which a hard film is formed is embedded with a resin, wherein a resin containing fine particles is provided on at least a side of the sample facing the hard film. A method for producing a sample embedding body, which is characterized by being used. 4. A method for producing a sample embedding body in which a sample having a hard film formed thereon is embedded with a resin, which comprises a step of filling a mold with a resin containing fine particles to a predetermined height. A method for producing a sample embedding body, comprising: a step of placing a hard film of the sample on a filled resin surface so as to face it; and a step of filling a resin on the sample.