JPS5979832A - Fabrication of specimen to be microscopically examined by two-stage replica method - Google Patents

Abstract

PURPOSE:To obtain a specimen to be microscopically examined faithful to an original specimen used in the examination due to an electron microscope within a short time, by such simple operation that metal In is pressed to the surface to be examined to fabricate one stage replica and a second replica is fabricated from said one stage replica by cellulose acetate. CONSTITUTION:Metal In is pressed to the surface to be examined of a rotary grinder by a hand presser and the uneveness of the specimen surface is transferred to In to obtain one stage replica. In the next step, 2-3 drops of acetone are dripped on the surface of said replica while a cellulose acetate film is adhered from above so as to exclude air bubbles and, after acetone is volatilized, said cellulose acetate film is peeled off to obtain a second stage replica. This second stage replica is fixed to the specimen stand of a scanning type electron microscope so as to upwardly direct the uneven surface thereof and, after a silver paste is applied to the periphery of the replica, gold is vapor deposited to the uneven surface to take a photograph while performing microscopic examination. By this method, the excellent two-stage replica is simply obtained within a short time. In addition, the one stage replica can be made preservable for a long time and can be used at a necessary time.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention particularly relates to a method for preparing a microscopic specimen using a two-stage replica method, which makes it easy and quick to prepare a microscopic specimen for a scanning electron microscope.

As is well known, scanning T4G microscopes are used in a wide range of fields because of their deep depth of focus, the ability to obtain immersive images, and the ability to use a wide variety of observation samples. .

By the way, the method for preparing a microscopic specimen for the scanning-type Oshi Microscope is as follows.
When the object to be observed is large, a general replica method using a cellulose acetate membrane is generally employed.

However, in the microscopic specimen obtained with this one-stage replica, the unevenness of the surface structure of the object to be observed is reversed, so it is difficult to grasp the surface structure of the object to be observed intuitively and three-dimensionally. It has the disadvantage of being extremely difficult. For this reason,
The two-stage replica method is preferable, but is it generally necessary to use the two-stage replica method? A method that perfectly transfers the subtle and minute irregularities on the surface of the original sample (#observation object) to the formed stone material.
- It is necessary to use a material that has both sufficient plasticity and sufficient rigidity to prevent the transferred regular irregularities from being deformed when the two-stage replica is obtained. An example of a material that meets these conditions is polymerizable acrylic fruit (I'#Tx), which is initially a liquid and then solidifies into a solid. The disadvantage is that it is cumbersome to operate and requires a long time to prepare the sample.

The present invention was made in view of the above circumstances, and provides a method for preparing a microscopic specimen using a two-stage replica method, which is easy to prepare, can be quickly made in general, and is particularly suitable when the original specimen is large. The purpose of the present invention is to provide a single-stage replica using metallic indium as the material for forming the replica.

The present invention will be described in detail below.

Here, a used rotary grindstone χ is selected as the original sample (object to be observed), a microscopic sample is prepared from this original sample by the method of the present invention and the conventional method, and the original sample itself is used as a microscopic sample and is subjected to a scanning electron microscope. The usefulness of the method of the present invention will be explained by examining the specimen and comparing the obtained micrographs. First, the procedure for preparing a specimen using the method of the present invention will be explained.

(11 indium (purity q9, 9*) *Press with a hand presser to form a smooth surface sound of about 1c+T12.

(Place the original sample on a smooth surface of indium metal 21 with a rotating grindstone, press it with a hand presser, and check the unevenness of the surface of the original sample.
It is transferred onto a metallic indium surface to create a single-stage replica.

(3) Apply acetate 772 to the uneven surface of the single-stage replica using a syringe, etc.
Add ~3 drops of acetic acid, then apply a cellulose membrane (thickness Q, 93 mm) of a suitable amount of acetic acid to the uneven surface, being careful not to introduce any air bubbles. Peel the cellulose sulfate film from the metal indium surface of the one-stage replica to create a two-stage replica.

(51) Apply double-sided adhesive tape to the sample stage for a scanning electron microscope, and firmly fix the uneven surface of the two-stage replica of cellulose acetate to soil, and then apply silver paste around the two-stage replica.

(6) Using ion sputtering, voltage 1zoov,'
G style 5~l QmA average? Deposit on the uneven surface of the two-stage replica for 4 minutes.

(7) Using a scanning electron microscope (Akashi PJr), examine the sample at a tilt angle of 45 degrees Celsius and an acceleration voltage of 15 KV, and take a micrograph.

Further, the procedure for creating a general replica using cellulose acetate is as follows.

(1) Add acetone to the observation surface of the rotating grindstone of the original sample.
~3 drops were added to the cellulose acetate membrane (thickness 0.08 mm).
) 'i Paste without creating any air bubbles, (2
) Thereafter, a microscope is similarly examined according to steps (4) to (71) according to the method of the present invention described above, and a microscopic photograph is taken.

Furthermore, is the original specimen itself examined using a rotating grindstone? Approximately 1cm
I cut it out into a corner, examined it as a specimen under a microscope, and photographed it.

The drawings are micrographs of microscopic specimens from replicas or original specimens prepared by the above-described method. Figures 1 to 5 are photographs of rotating grindstone samples, and the magnification of Figure 1 is 5.
0x, Figure 2 is 200x.

Figure 3 is 700x, Figure 4 is 2500x, and Figure 5 is 10,000x. Figures 6 to 10 are photographs of two-stage replicas made by the method of the present invention;
The figure shows a photograph of a general replica of metallic indium used as a specimen under a microscope, and Figures 16 to 20 are photographs of the conventional replica method using a cellulose acetate membrane. From the photographs in FIGS. 1 to 5, it can be seen that the original sample consists of a registration part with a pore structure and an abrasive drop-off part where abrasive, abrasive grains, and coating material remain. The rectangular abrasive grains (roughly half covered by the coating material) are partially missing, and there are pits of several μm and stair-like steps on the order of 1 μrn at the top of the abrasive grains. In the photographs of microscopic specimens obtained by the two-stage replica method of the present invention shown in Figures 6 to 10, there are parts where the pores of the resin and the shape of the coating material have been lost in relatively flat areas;
It lacks sharpness overall. However, the structure of the bits, steps, etc. where the abrasive grains wait appears almost the same as in the photograph from the original sample, and the uneven structure of the original sample is fully expressed as a whole. Furthermore, in the photographs of general replicas of indium shown in Figures 11 to 15 and the photographs of conventional general replicas of cellulose acetate shown in Figures 16 to 20, the surface structure is reversed, so it is difficult to understand the real image as an image. In particular, the part where the abrasive grains are inserted (recessed part) has many shadows Y and the shape χ is unclear. power)
Sh.

It can be seen that the one-stage cellulose acetate replica has a high degree of sharpness as a whole and reproduces the fine structure of the original sample.

As described above, the microscopic specimen obtained by the method of the present invention has a fine structure similar to that of the original specimen. Although there was a slight decrease in sharpness, the transfer was almost complete, and the culture rate was 20 (l Q~30
It can be seen that it can withstand observation up to 00x magnification. Therefore, the method of the present invention can replace the conventional two-stage replica method due to its operability.

Having explained the above, the method for preparing a speculum specimen using the two-stage replica method of the present invention is to create a one-stage replica by suppressing genus indium Y on the surface of the object to be observed, and from this one-stage replica. Since a two-stage replica is created using cellulose acetate, a single-stage replica can be created within a few minutes and in an extremely short time.The overall preparation time can be shortened, and the operation is simple and requires no skill. do not.

Well, one-tier replicas can be stored for a long time, and you can also freely increase the number of two-tier replicas depending on your peace of mind. Further, it has advantages such as being less subject to dimensional limitations χ of the object to be observed and having a wide range of applications.

[Brief explanation of the drawing]

The drawings are all scanning quadruple micrographs showing the fine structure of the coating surface of the rotary grindstone. Figures 1 to 5 are of the original sample, and Figures 6 to 10 are of the microscopic specimen of the present invention. Figures 11 to 15 are based on microscopic specimens of the preparation method, Figures 11 to 15 are one-stage replicas of disputed indium, and Figures 16 to 20 are one-stage replicas of cellulose acetate produced by Kojomai. Applicant: Showa Denko Co., Ltd.

Claims (1)

[Claims] Press a layer of poor metal indium onto the observation surface of the object to be observed, and reversely transfer the uneven surface of the observation surface to the metal indium surface.
A method for preparing a microscopic specimen using a two-stage replica method, which is characterized in that a one-stage replica of indium chloride is prepared, and then a two-stage replica is created from this one-stage replica using cellulose acetate.