JPS5833150A - Manufacture of specimen observation of structure - Google Patents

Abstract

PURPOSE:To obtain a specimen for the observation of structure which can obtain an internal structure corresponding to a photo sensible structure, without the use of an electron ray diffraction which requires much labor, by a method wherein an etching is applied in the middle of electrolytic grinding of the specimen, and electrolytic grinding is applied to only one side. CONSTITUTION:A manufacturing process of specimen for the observation of structure consists of a sampling material setting process (a), a process (b) in the middle of electrolytic grinding, a completion (c) of electrolytic grinding and an etching (d). In a method used in this invention, an electrolytic grinding stops once at a time of the process (b) in the middle of electrolytic grinding to perform the etching (d) to expose a metalic structure, and then, an electrolytic grinding process starts again. During aforesaid process, only one side is ground by, for example, a jet electrolytic grinding method, and this allows to obtain an internal structure corresponding to a photo sensible structure. The use of said method permits to perform an easy operation to correspond to the photo sensible structure which requires a fairly well skill and much labor if a conventional electronic microscope observation is utilized.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a specimen for tissue observation using a scanning transmission electron microscope, which can be made to correspond to a tissue.

Conventionally, specimens for microstructure observation using a transmission electron microscope (hereinafter abbreviated as TEM) are mainly used for four-part microstructure observation.
It has been produced by electrolytic polishing to a thickness of about 1 .mu.m'l in a vacuum of 10"" Torr (about 10@-3 Pa) so that electron beams can pass through it.

However, in the observation using the microstructure observation specimen prepared by this method, since both sides are electrolytically polished, the microscopic structure (hereinafter abbreviated as "light microscopic structure") cannot be obtained as it is.
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Furthermore, when electron diffraction is used to determine the correspondence, it has the disadvantage of requiring extremely complicated procedures and skill. For example, in the light microstructure of δ-fulrite precipitated on austenitic stainless steel, by selecting a corrosive solution, the austenite in the matrix can corrode white and the δ-ferrite precipitate can corrode gray, making it easy to distinguish between the two. can do.

However, in the observation of TEMO structure and Orikansai test pieces,
As mentioned above, since both sides are electrolytically polished, it is not possible to clearly distinguish between the two, and therefore it is necessary to use electron diffraction to distinguish between the austenite and ferrite phases based on the difference in their crystal structures. The disadvantage of this method is that it requires experience and a lot of effort.

The purpose of the present invention is to obtain a test piece in which the correspondence between the internal structure of a TEM tissue observation test piece and the light microscope structure can be obtained without using such time-consuming electron diffraction.

(1) The present invention is characterized in that etching is performed during the electrolytic polishing of the test piece, and further electrolytic polishing is performed only on one side, and another object of the present invention is to obtain the above-mentioned test piece.

(2) It is characterized by etching the test piece after electrolytic polishing.

This is a method for producing a specimen for tissue observation.

In addition to normal transmission electron beam images, recent TEMs can now observe the internal structure of observation specimens while scanning the electron beam, and such electron microscopes can also be used as scanning electron microscopes. Observation of secondary electron beam images is also possible.

This type of electron microscope is a scanning transmission electron microscope (hereinafter referred to as 'ST').
(referred to as EM), and the present invention is particularly effective in this STEM.

The tissue observation specimen prepared by the method of the present invention is approximately 1
Because the thickness is only 1 μm, TEM observation is possible, and because the observation surface is etched, the correspondence with the light microscopic structure can be clearly seen using secondary electron beam images that are sensitive to surface conditions. There is.

The present invention will be explained below with reference to process diagrams.

FIG. 1 shows conventional method B1 method A1 according to the first invention of the present invention S according to method C according to the second invention of the present invention
The manufacturing process of TEM or a tissue observation test piece used for TEM is shown.

In addition, (a) is the sample material setting, (b) is during electrolytic polishing, (C
) shows the completion of electropolishing, (d) shows the etching, (e) shows the single-sided electropolishing, and (f) shows the completion of test piece preparation. In addition, 1 is a sample material for a thin plate-like structure observation specimen that also serves as an anode, 2 is a cathode for electrolytic polishing that is installed in pairs before and after the same sample material 1, 3 is an electrolytic polishing liquid, and 4 is a Engineering, Chi/Da liquid (corrosive liquid)
, 5 indicate etched surfaces, respectively. Conventional method B only performs electropolishing and does not perform etching as shown in step B, so it is not possible to distinguish the phase from the secondary electron beam image of the test piece, that is, to make it correspond to the light microscopic structure. .

On the other hand, in the first invention of the present application, that is, the method shown in step A, the electrolytic polishing is stopped once during the electrolytic polishing of the conventional method, etching is performed to present a metal structure, and then the electrolytic polishing is performed. The process of restarting is taken, but at this time 1
For example, by polishing only one side using a jet electrolytic polishing method, an internal structure corresponding to a light microscopic structure can be obtained. Similarly, the second invention of the present application.

That is, in the method shown in step C, by performing etching after completing electrolytic polishing using the conventional method, a specimen for microstructural observation can be prepared that allows an internal structure to be obtained that corresponds to the microscopic structure.

Hereinafter, the effects of using the above-described present invention will be described.

A martensitic 12SCr steel in which δ ferrite is precipitated was used as a sample material for a microstructural observation test piece, and the interior of the steel was observed. First, 12 tubes with a diameter of about 3 mm and a thickness of 0.1 to 0.5 ml were prepared in advance by high-speed force, ri, etc.
Load the 1Cr steel into the electrolytic polisher. Here, a 10% perchloric acid 90% alcohol solution was used as the electrolyte. after that.

Observation test pieces were prepared according to each step shown in FIG. 1. At this time, the corrosive liquid was Vilella reagent (100 m
1 alcohol, lf picric acid, 5m/! Hydrochloric acid) was used, and a jet electrolytic polishing method was used for two-sided electrolytic polishing. FIG. 2 is a photograph of a secondary electron image of a test piece prepared by a conventional method.

The test piece is only white and no metallic structure is observed.

Figure 3m, +21 is a photograph of a secondary electron beam image of a test piece prepared by the method of the first invention of the present application, which corresponds well to the optical M structure.

Figure 3 (3) is a photograph of a transmission electron beam image of the same test piece, showing the internal structure at the same position as Figure 3 (2). According to this, the transmission electron beam image clearly corresponds to the light microscopic structure.
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Similarly, FIG. 4 (+l, (21) is a photograph of a secondary electron beam image of a test piece prepared by the method of the second invention of the present application, which corresponds well to the light microscopic structure. 3) is a photograph of a transmission electron beam image of the same test piece.

It shows the internal structure at the same position as FIG. 4(2). Even when a specimen prepared by this method is used, its transmission electron beam image clearly corresponds to that of a light microscopic tissue.

As stated above, by using the method for preparing specimens for microstructural observation according to the present invention, it is now possible to very easily handle microstructures using light microscopy, which required considerable skill and effort in conventional electron microscopy. became. It goes without saying that the microstructure observation specimen prepared according to the present invention can also be used in a STEM or a scanning electron microscope equipped with a transmission electron beam detector.

[Brief explanation of drawings]

FIG. 1 shows the conventional method 2 of the first invention of the present application, t-51.
STEM or T by the method of the second invention of the present application
A flowchart that simply shows the method for preparing an EM structure observation specimen,
Figure 2 shows 5 specimens for microstructure observation prepared by the conventional method.
00x secondary electron beam image, Figure 3 is an electron micrograph of the microstructure observation specimen obtained by the method of the first invention of the present application, and +21 is 500x and 5000x, respectively.
The secondary electron beam image (3) in the same figure shows a 5000 times transmission electron beam image of the same field of view as (2) in the same figure. FIG. 4 is an electron microscope microstructure photograph of a microstructure observation specimen obtained by the method of the second invention of the present application, where +r3 and +21 are each 750
．． 5000x secondary electron beam image. Figure (3) shows a 5000x transmitted electron beam image of the same field of view as Figure (2). A: Process flow showing the method of the first invention of the present application B: Process flow of the conventional method C: Upstream flow showing the method of the second invention of the present application (a): Sample material setting (b): Electrolytic polishing Midway (C): End of electrolytic polishing (d): Enoching (e) - Single-sided electrolytic polishing 1: Sample material for tissue observation specimen (also serves as anode) 2: Cathode for electrolytic polishing 3: Electrolytic polishing solution 4: Etching solution 5: Etching liquid 6: Carbide 7: Delta ferrite No. 1 0) Akira 2 Mi (2) (3) Yasu 3 Nagi

Claims (2)

[Claims] (1) When preparing a specimen for electron microscopic structure observation,
A method for producing a composite fiber observation test piece, characterized by etching the test piece during electrolytic polishing and further electrolytically polishing only one side. (2) When preparing a specimen for electron microscope structure observation,
A method for preparing a specimen for microstructural observation, characterized by etching the specimen after electrolytic polishing.