JP2003185544A - Method for manufacturing microscope observation sample mount in porous body - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a microscope observation sample mount-manufacturing method having a short manufacturing time. <P>SOLUTION: In the method for mounting the microscope observation sample mount of a porous body, a cured resin is subjected to impregnation treatment to the pore section of the porous body by a vacuum impregnation method, a sample mount having a ring type before the curing resin is cured is rotated by a rotary pressurizing apparatus 1 for filling the cured resin into the pore section of the porous body by centrifugal force (1). In the microscope observation sample mount-manufacturing method of a porous body in 1 above, the cured resin is cured in approximately 15 minutes (2). <P>COPYRIGHT: (C)2003,JPO

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 a microscope observation sample mount of a porous body.

[0002]

2. Description of the Related Art For example, a member such as a turbine blade of a jet engine, a stator vane or an inner wall of a combustion chamber is provided with a ceramic thermal spray coating for imparting heat resistance.

The thermal spray coating portion is porous, and a microscope is used to inspect whether the porosity (void) rate, the amount of oxide, cracks, etc. are proper values. When performing a microscopic inspection, a sample mount for microscopic observation is usually manufactured by embedding a cut sample of a portion to be inspected of the above-mentioned component in a long-time curable resin such as epoxy resin.

When the observation surface of the above-mentioned sample mount for microscopic inspection is polished flat, the sprayed coating portion may fall off if there are pores (voids). Therefore, the sample is reinforced and erroneous analysis due to the dropout occurs. In order to prevent this, it is necessary to completely fill the pores on the observation surface (polished surface) with resin.

As a general method for filling the resin into the pores, a vacuum impregnation method using an epoxy resin that cures at room temperature and hardly shrinks after curing is performed.

FIG. 3 is a view for explaining an example of a method of manufacturing a sample mount for microscopic inspection by the above-mentioned vacuum impregnation method and a vacuum impregnation apparatus, in which a die ring 102 is put on a cut sample 101 placed on a support plate 100. , This mold ring 102
A curable epoxy resin 103 is injected into the inside.

The mold ring 102 is a disk-shaped ring holder 1
A plurality of them are arranged on the circumference of 04, and a vacuuming port 105 communicating with a vacuum pump is provided at the center of this ring holder 104.

The support plate 100 on which the plurality of mold rings 102 are arranged is installed on a vacuum container base 107 on which a bell-shaped vacuum container 106 is placed, and the ring holder 104 is a bell-shaped vacuum container. It is in a state that it completely fits inside 106.

The evacuation port 105 is connected to a suction pipe 109 which connects the base 107 of the vacuum container and the vacuum pump 108, and a desiccant 110 and glass wool 111 are provided in the suction pipe 109. A drier 112 and a vacuum gauge 113 filled with are provided. A valve 114 that can be opened to the atmospheric pressure is provided on the top of the vacuum container 106.

In the vacuum impregnating apparatus having the above structure, when the vacuum pump 108 is operated to obtain an appropriate degree of vacuum, the air in the pores existing in the sample is discharged and the pores are filled with the resin.

FIG. 4 (a, b) shows a sample mount in which the observation surface is polished after the resin is hardened by impregnating the pores with the resin in this way. It should be noted that FIG. 4a shows that the difference in hardness between the resin and the sample was reduced by adding an alumina filler to the resin, and polishing sag of the resin portion was suppressed, and FIG.

FIGS. 5 and 6 are micrographs of a sample obtained by impregnating the pores of the spray-coated portion with a curable epoxy resin in the vacuum impregnating apparatus as described above, and the pores are not filled with resin. This is an example of the remaining impregnation failure.

The upper part of FIGS. 5 and 6 is the surface side of the sample, and the magnifications of the photographs are 200 and 500, respectively.
Double.

As described above, the vacuum impregnation alone does not sufficiently impregnate the resin. Therefore, after the vacuum impregnation, the sample with the mold ring attached in the pressure chamber (not shown) having an air pressure of about 2 atm. It is practiced to place the mount so that all the pores are completely filled with resin.

7 and 8 are photomicrographs of a sample when pressure treatment (about 2 atm) is performed in addition to vacuum impregnation. FIG. 7 shows a magnification of 500 times, and FIG. 8 shows a magnification of 200 times. is there.

[0016]

It takes about 8 hours to cure the epoxy resin used in the conventional vacuum impregnation method.
Further, it requires one night (about 12 hours) until the pressurizing operation is completed, resulting in poor work efficiency and unusable for emergency inspection.

The present invention has been made to solve the above problems, and an object of the present invention is to provide a method of manufacturing a microscope observation sample mount which requires a short manufacturing time.

[0018]

As a means for solving the above-mentioned problems, a method for producing a microscope observation sample mount for a porous body according to claim 1 is a method for producing a microscope observation sample mount for a porous body, The pores of the porous body are impregnated with a curable resin by a vacuum impregnation method, and the sample mount before the curable resin is cured is rotated to fill the pores of the porous body with the curable resin by centrifugal force. The main point is to do.

According to a second aspect of the present invention, there is provided a microscope observation sample mount manufacturing method for a porous body, wherein the curable resin is cured in about 15 minutes. The gist is that it is a short-time curable resin.

[0020]

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below with reference to the drawings.

In place of the pressure operation after the vacuum impregnation as described above, the present invention is characterized in that the pressure is applied by the rotary pressure device described below.

FIG. 1 is a conceptual diagram of the rotary pressure device 1 described above. The rotary pressurizing device 1 includes a rotating shaft 2 extending in the vertical direction, and an arm 4 having a mount pedestal 3 at a lower end portion of the rotating shaft 2 in an upper end portion of the arm 4 in a plane including the rotating shaft 2. Is rotatably connected as a fulcrum 5.

The rotating shaft 2 can be driven to rotate at an appropriate rotation speed by a rotation driving means such as a motor (not shown).

In the rotary pressurizing device 1 having the above structure, the sample mount 6 with a mold ring in which the resin injected into the cut sample is uncured is placed on the mount pedestal 3 so that the observation surface is located above. When the rotary shaft 2 is rotationally driven by a rotary drive means (not shown) at an appropriate rotational speed, the arm 4 rotates together with the rotary shaft 2, and at the same time, as the rotational speed of the rotary shaft 2 increases, as shown in FIG. The arm gradually rotates in the horizontal direction, and the arm stops rotating at a position where the horizontal force acting on the arm 4 and the gravity acting on the arm 4 are balanced by the rotation.

Then, a large centrifugal force F acts on the sample mount 6 with the mold ring in which the injection resin placed on the mount pedestal 3 is uncured, and the resin is filled in the pores of the cut sample. become.

In the rotary pressurizing device 1, it is possible to pressurize to 2 atm or more used in the conventional pressurizing method in a short time (about several minutes).

Therefore, by using the rotary pressurizing device 1 described above, for example, a short-time curable acrylic resin (commercially available Durofix 2 or Citofix) which cures in 7 to 15 minutes can also be used. Is possible.

That is, vacuum impregnation is carried out in the vacuum impregnating apparatus as described above using a short-time curable acrylic resin, and the rotary pressurizing apparatus 1 is set before the acrylic resin is cured.
By applying the pressure, it is possible to reliably fill the porous pores with the resin in a short time.

Thereafter, the microscope observation sample mount can be manufactured in a short time by polishing the observation surface with a polishing device (not shown).

[0030]

According to the first aspect of the present invention, the pressure treatment after impregnation by the vacuum impregnation method is performed in a short time of about several minutes by utilizing the centrifugal force of the rotary pressure device. Can be manufactured in a short time.

According to the invention of claim 2, the pressure treatment after the impregnation by the vacuum impregnation method is performed in a short time of about several minutes by utilizing the centrifugal force by the rotary pressure device, and the impregnation by the vacuum impregnation method is performed. Since a short-time curable resin that cures in about 15 minutes is used as the resin used for the treatment, the microscope observation sample mount can be manufactured in an extremely short time.

[Brief description of drawings]

FIG. 1 is a conceptual diagram of a rotary pressure device according to the present invention.

FIG. 2 is a diagram showing an operating state of the rotary pressurizing device of FIG.

FIG. 3 is an example of a method and apparatus for manufacturing a sample mount for microscopic inspection by a conventional vacuum impregnation method.

FIG. 4 is an example of a sample mount in which an observation surface is polished after being impregnated with an epoxy resin by a vacuum impregnation device. Figure 4a shows the case with alumina filler and Figure 4b shows the case without filler.

FIG. 5 is a photomicrograph (magnification: 200) of a sample obtained by impregnating pores of a thermal spray coating portion with a curable epoxy resin only by vacuum impregnation treatment.

FIG. 6 is a micrograph (magnification: 500 times) of a sample in which a curable epoxy resin is impregnated into pores of a thermal spray coating portion only by vacuum impregnation treatment.

FIG. 7 is a micrograph of a sample in which a hardening epoxy resin is impregnated in a pore of a thermal spray coating portion by a vacuum impregnation treatment and a pressure treatment (about 2 atm) is performed (magnification: 5).
00 times).

FIG. 8 is a photomicrograph (magnification: 2) of a sample in which a curable epoxy resin is impregnated into the pores of the thermal spray coating portion by vacuum impregnation treatment and pressure treatment (about 2 atm) is performed.
00 times).

[Explanation of symbols]

1 rotary press 2 rotation axes 3 mount pedestal 4 arms 5 fulcrum 6 Sample mount

Claims (2)

[Claims] 1. A method for producing a sample mount for observing a porous body under a microscope, wherein a pore-shaped portion of the porous body is impregnated with a curable resin by a vacuum impregnation method, and the sample mount before the curable resin is cured is used. A method of manufacturing a microscope observation sample mount of a porous body, which comprises rotating to fill the pores of the porous body with the curable resin by centrifugal force. 2. The method for manufacturing a microscope observation sample mount for a porous body according to claim 1, wherein the curable resin is 15
A method for manufacturing a sample mount for microscopic observation of a porous body, which is a short-time curable resin that cures in about a minute.