JPH08271677A - Formation method for metallographic testpiece by electrolytic etching of metallographic sample - Google Patents

Abstract

PURPOSE: To drastically shorten formation work time for forming a metallographic testpiece for metallography test by electrolysis etching of metallographic sample, reduce labor man power and difficulty, and completely eliminate failure undesirable accidents of the metallographic sample. CONSTITUTION: In a metallographic sample 14 contained in a cylinder 11 of a press machine 10 together with an electric insulating resin material 16, an electric conductive lead wire 15 placed in conductive state in an advance to a non-metal observation surface 14b is extracted out of a path for leading out 17a of a press plate 17. The press machine 10 is operated in this state under heating condition and press formation is performed between a piston 13 and the press plate 17. The metallographic testpiece 18 from which hardened resin 18a a conductive lead wire 15 for conducting to the metallography sample 14 from the cylinder 11 is extracted is taken out. If the conductive lead wire 15 is connected to a power source provided with electrode for operation after polishing the metallographic observation surface 14a of metallographic sample 14, then electrolysis etching can be performed by using etching liquid.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a metallic phase sample such as a fuel cladding tube or a plate constituting a PWR fuel assembly or a metallic phase sample such as a plate, and a pair of electrodes for a metallic phase observing surface which is a section thereof. The present invention relates to a method for forming a metal phase test body obtained by embedding the metal phase sample in an electrically insulating resin material in order to perform a metal phase test that corrodes by electrolytic etching by using an etching solution. .

[0002]

2. Description of the Related Art Conventionally, in order to form a metallic phase test body for this kind of electrolytic etching, first, a press machine 1 as shown in FIG. 4 (a) is used, and its cylinder 1a has an exterior heater 2
The metal phase sample 3 is placed on the piston 1b fitted in the cylinder 1a so as to be movable up and down from below in the example shown in FIG. Insulating resin material 4
Is supplied from the upper end opening 1c of the cylinder 1a, and the upper end opening 1c is closed by the pressing lid 1d.

Next, the heater 2 is energized, and the piston 1b is moved upward by the external force F under the heating condition of the electrically insulating resin material 4, and the pressing lid 1d is moved downward by the external force F. The press machine 1 is operated while maintaining the pressed state by ′, and thereby the metal-phase test molded body 5 shown in FIG. 4B is obtained. Therefore, the metal-phase test molded body 5 is the heater 2 of the electrically insulating resin material 4.
The cured resin portion 5a obtained by press molding under the heating condition of 1 and the metal phase sample 3 embedded in the cured resin portion 5a. Then, the metallic phase observation surface 3a in the metallic phase sample 3
Is exposed on the one surface 5b of the cured resin portion 5a, and the metallic phase observation surface 3a is polished by a polishing machine at a proper time.

Further, in order to form the metallic phase test body A shown in FIG. 6 which can be subjected to electrolytic etching, the embedded metallic phase sample 3 in the above metallic phase test molding 5 is formed.
For the electrolytic etching shown in FIG. 6, one electrode 7a connected to the power source 6 is brought into contact with the upper end surface 3b side, which is the non-gold phase observation surface, and the metal phase observation surface 3a is , The other electrode 7b is brought into contact with the other via the etching solution, but in order to connect the one electrode 7a to the upper end surface 3b side, processing as shown in FIGS. 5A, 5B and 5C is performed. The work will continue.

That is, one electrode 7 as shown in FIG.
In order to provide a, on the other surface 5c of the cured resin portion 5a,
The drill 8 shown in FIG. 5B is used to form the electrode hole 5d shown in FIG. 5C.
The positioning work is performed depending on where on the other surface 5c should be set. Then, if the electrode hole 5d is formed by the drill 8 with the tip position 5e as the axis, one rod-shaped electrode 7a is fitted into the electrode hole 5d, and the one electrode 7a The tip portion of the gold phase sample 3 is pressed against the upper end surface 3b side of the gold phase sample 3 to secure the conduction state.

[0006]

In the conventional method for forming a metallurgical phase test body described above, since the cured resin portion 5a of the metallurgical phase test molding 5 is actually colored and opaque, a drill is used. Positioning work for selecting the tip position 5e of 8 becomes considerably difficult, and if there is an error in this, sufficient electrical contact between the one electrode 7a and the metal sample 3 cannot be guaranteed. become.

Further, even when the electrode hole 5d is drilled by the drill 8 as described above, the tip portion of the drill 8 cannot be directly viewed, so that the drilling depth becomes excessive and the metal phase sample 3 There is also a high possibility of scratching the gold phase observation surface 3a.

Therefore, in order to eliminate the above defects,
It is conceivable that the conductive resin material may be used instead of the electrically insulating resin material, and the work of forming an electrode hole or fitting one of the electrodes into the hole may be unnecessary. If such a conductive resin material is used, not only a considerable time is required to perform electrolytic etching, but also the current value required for this must be increased. . Further, there is a problem that the range of electrolytic etching is limited with respect to the current value per unit area on the gold phase observation surface.

The present invention, like the above-mentioned conventional method, has a difficulty in the positioning work caused by the drilling work with a drill, a drawback such as damage to the observation surface of the metal phase, and an electrolytic etching caused by the use of a conductive resin material. He is trying to solve various problems such as inefficient work.

Therefore, in the present invention, for the metal phase sample,
The conductive lead wire appropriately attached in advance is led out to the outside from the lead-out passageway in the separately prepared pressing plate, and in this state, molding by the press machine in the conventional method is performed. Then, the purpose is to be able to complete the formation of the metallic phase test body without performing a step such as perforation after the molding.

[0011]

In order to achieve the above object, the present invention provides a conductive lead wire in advance in the cylinder of a press machine so as to be electrically connected to the non-metal phase observing surface. And the electrically insulating resin material coexist, and the conductive lead wire is pulled out from the lead-out passageway of the pressure plate closed and covered with the electrically insulating resin material. Every time, the press machine is operated under heating conditions in this state, and by the piston and the pressing plate,
From the one surface of the cured resin portion made of the electrically insulating resin material, the conductive lead wire is led out, and the other surface is molded into a metal phase test body in which a metal phase observation surface of the metal phase sample is exposed. A method for forming a metal-phase test body by electrolytic etching of a metal-phase sample, characterized in that the metal-phase test body taken out from the press is polished on the metal-phase observation surface. Trying to.

In the method according to claim 2, since the conductive lead wire according to claim 1 is attached to the non-gold phase observation surface of the gold phase sample so as to be in a conductive state, the conductive lead wire is connected to the non gold phase. The content is that the wrapping is fastened on the observation surface.

[0013]

The electrically insulating resin material is press-molded together with the metallic phase sample under heating conditions using a pressing machine as in the conventional method, but in the present invention, a simple metallic phase sample is used as the electrically insulating resin material. Instead of burying it in the mold and molding it, a conductive lead wire is previously attached to the metal phase sample so as to be in a conductive state, and the conductive lead wire is attached to the electrically insulating resin material of the pressing plate. After being led out to the outside from the lead-out passage, press molding is performed. Therefore, at the time of press molding, the press molding can be performed without the substantially melted electrically insulating resin material being unintentionally washed away from the lead-out gap passage.

After the press molding, the molded product is taken out of the press and the pressing plate is removed, whereby the final object of the metal phase test before polishing is obtained. A conductive lead wire derived from one surface of the cured resin portion is connected to one terminal of a power source, and an electrode provided on the other terminal of the power source performs electrolytic etching on the metal phase observing surface of the metal phase test body. be able to.

[0015]

EXAMPLE A method for forming a metallic phase test article according to the present invention will be described below with reference to FIGS. 1 and 2. FIG.
The press machine 10 itself shown in Fig. 4 is substantially the same as that shown in Fig. 4 (a), and its cylinder 11 has the heater 1
The piston heated by 2 and fitted in the cylinder 11 so as to be movable up and down from the lower end port 11a side thereof is shown in FIG.
11b shows the upper end opening of the cylinder 11.

Here, on the upper surface 13a of the above-mentioned piston 13, a required metal phase sample 14 such as a pipe or a rod is provided.
Is placed in the same manner as in the conventional method described above, with the metallic phase observation surface 14a facing downward.
In advance, the conductive lead wire 15 having a required length is attached to the non-gold phase observation surface 14b so as to be in a conductive state.

Here, for the conductive lead wire 15, for example, a bare copper wire or the like can be used.
Although it may be done in any way, in the illustrated example, the conductive lead wire 15 is fastened around the non-gold phase observation surface 14b, which is the cylindrical peripheral side surface of the gold phase sample 14, so as to be fastened.
In order to secure the fastening state, the conductive lead wire 15 may be twisted or solder may be used.

Further, similarly to the conventional method, the powdery electrically insulating resin material 16 made of bakelite, dialerstallate, plastic or the like is provided on the upper surface 13a of the piston 13 from the upper end opening 11b of the cylinder 11. The metal phase sample 14 is charged and embedded in this, but in the present invention, at this time, the conductive lead wire 15 is pulled out from the electrically insulating resin material 16 and provided on a pressing plate 17 prepared separately. It is led out to the outside through the lead-out passageway 17a. The lead-out clearance passage 17a shown in FIG. 1 is formed by a through hole formed in the center of the pressing plate 17, and in FIG. 17b is provided in advance, and is led out to the outside through the lead-out gap passage 17a between this and the inner peripheral surface of the cylinder 11. Here, the lead-out passageways 17a shown in FIG. 1 are formed separately.

Here, the pressing plate 17 is closed and mounted on the upper surface side of the electrically insulating resin material 16, but the pressing plate 17 may be fitted in the cylinder 11 as shown in the illustrated example. Further, it may be mounted on the upper end opening 11b of the cylinder 11 like the pressing lid 1d in FIG.

When the lead-out passageway 17a is too large, the electrically insulating resin material 16 melted from the lead-out passageway 17a during press working by the press machine 10 described later. However, if the diameter of the pressing plate 17 is 30 mm in FIG.
It is desirable that the through holes have a diameter of about mm.

When the above preparation is completed, the heater 12 is energized and the cylinder 11 is cooled to 100% as in the conventional method.
The external force F is applied to the piston 13 while heating it up to about 200 ° C.
And the pressing plate 17 is held in a pressed state by the external force F ′, and press working is carried out by a usual method. When the press molding is completed by this, a press product on which the pressing plate 17 is mounted is obtained from the inside of the cylinder 11 as shown in FIG. 1B, and the pressing plate 17 is removed from the press product to cure the press product. Resin part 18
A metallic phase test body 18 in which the metallic phase sample 14 is embedded in a is obtained.

As shown in FIG. 3, the metal phase test body 18 pressed in this way has the one surface 18b which is the upper surface in the drawing of the cured resin portion 18a obtained from the electrically insulating resin material 16, as clearly shown in FIG. From the above, the conductive lead wire 15 is led out, and the gold phase observation surface 14a of the metal phase sample 14 on the other surface 18c which is the lower surface is exposed.
The gold-phase observing surface 14a is polished by a conventional method as is known, and electrolytic etching is performed.

In order to perform electrolytic etching using the metal phase test body 18 obtained according to the present invention as described above, a known power source 19 prepared separately is used, and one terminal thereof has the above-mentioned cured resin portion. The conductive lead wire 15 led out from 18a is connected. As a result, one electrode for electrolytic etching is connected to the non-gold phase observation surface 14b of the gold phase sample 14, and therefore, the other electrode 20 connected to the other terminal of the power source 19 and the gold phase sample 14 are connected. Electrolytic etching can be performed by using the etching liquid applied to the gold phase observation surface 14a.

[0024]

EFFECTS OF THE INVENTION Since the present invention can be carried out as described above, a conductive lead wire is lead out from a metal phase sample in advance, and the lead wire is brought out from the lead-out passageway of the pressing plate and pressed. Since the press working is carried out by a machine, the desired metal phase test body can be immediately obtained by the press molding. Therefore, the work of attaching the electrode with a drill as in the conventional method is completely unnecessary,
It is possible to eliminate the above-mentioned problems such as the positioning work of the drill and the damage on the observation surface of the metallic phase. Further, it is possible to solve the problems that the electrolytic etching requires a long time and the current value needs to be increased as in the method using the conductive insulating resin material.

[Brief description of drawings]

FIG. 1 (a) is a vertical cross-sectional front view showing a state before press working of a press used for carrying out the method for forming a metal phase test body according to the present invention, and FIG. 1 (b) is the press. It is a perspective view showing a state where a molded product obtained by operating the machine is taken out.

FIG. 2 is a schematic plan view showing another embodiment of the press machine in FIG.

FIG. 3 is an overall configuration explanatory diagram when electrolytic etching is performed on a metal phase sample using a metal phase test body which is a pressed product obtained by carrying out the present invention.

FIG. 4 (a) is a vertical cross-sectional front view showing a state before the press working of a press used to carry out the conventional method for forming a single metal phase test body, and FIG. FIG. 3 is a perspective view of a metal-phase-test molded body molded by.

5 is a view showing a working procedure for forming one electrode of a metal phase sample for the metal body for a metal phase test of FIG. 4;
(A) is a front view showing a molded body for metal phase test in which a drill has been positioned, (b) is a front view showing a state in which an electrode hole is drilled by a notched drill, (c) FIG. 4 is a vertical cross-sectional front view showing a metal-phase test molded body after perforating the electrode hole.

6 is an overall configuration explanatory view of a state in which electrolytic etching of a gold phase sample is about to be performed by a metal phase test body obtained by fitting one electrode into an electrode hole in FIG.

[Explanation of symbols]

 10 Press Machine 11 Cylinder 13 Piston 14 Gold Phase Sample 14a Gold Phase Observation Surface 14b Non-Gold Phase Observation Surface 15 Conductive Lead Wire 16 Electrically Insulating Resin Material 17 Pressing Plate 17a Lead-out Passage Path 18 Metal Phase Testing Body 18a Curing Resin part 18b One surface 18c Other surface

Claims (2)

[Claims] 1. A metal phase sample in which a conductive lead wire is attached in advance to a non-metal phase observation surface in a cylinder of a press machine to coexist with an electrically insulating resin material, and the conductivity The lead wire is pulled out from the lead-out passageway of the pressure plate closed and covered with the electrically insulating resin material, and the press machine is operated under heating condition in this state, and the piston and the above-mentioned pressure plate. With the above, the above-mentioned conductive lead wire is led out from one surface of the cured resin portion made of the above-mentioned electrically insulating resin material, and the metal phase observation surface of the metal phase sample is exposed on the other surface. And forming a metal-phase test body by electrolytic etching of a metal-phase sample, characterized in that the metal-phase test body taken out from the press was polished on the metal-phase observation surface. Method. 2. A conductive lead wire is attached to the non-gold phase observation surface of the gold phase sample so as to be in a conductive state, so that the conductive lead wire is wound and fastened on the non gold phase observation surface. The method for forming a gold phase test body by electrolytic etching of the gold phase sample according to claim 1.