Analysis sample

By embedding conductive samples and conductors in resin and polishing specific surfaces for electrolytic etching, the analytical sample preparation process is streamlined, addressing the time-consuming nature of existing methods.

JP2025085951APending Publication Date: 2025-06-06AISAN IND CO LTD
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Patent Information

Application Number
JP2023199674
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2023-11-27
Publication Date
2025-06-06

AI Technical Summary

Technical Problem

The existing process for preparing analytical samples for electrolytic etching is time-consuming due to the need to wind and fix lead wires around conductive samples before molding, and to create holes for wire extraction in the molding die.

Method used

The analytical sample is formed by embedding a conductive sample and a conductor in resin, with the observation surface polished for electrolytic etching and the electrode surface formed by polishing away from the observation surface, allowing for easy preparation of the sample.

Benefits of technology

This approach simplifies the preparation of analytical samples for electrolytic etching by allowing the observation and electrode surfaces to be formed through polishing, reducing the time and complexity of the process.

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Abstract

To facilitate formation of an analysis sample for electrolytic etching.SOLUTION: An analysis sample is a molding article 10f molded to have a predetermined size from a conductive sample 12 and a resin 15 in which the sample 12 is embedded. A part of the molding article 10f is polished so as to form an observation surface 12k from which the sample 12 is exposed, and the observation surface 12k can be electrolytically etched. In the molding article 10f, an electrode plane 12e of the sample 12 to which an electrode 25 for electrolytic etching can be abutted is formed by polishing a position separated from the observation surface 12k of the sample 12.SELECTED DRAWING: Figure 1
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Description

[Technical field]

[0001] The present technology relates to an analytical sample which is a molded product of a predetermined size made of a conductive sample and a resin in which the sample is embedded, and which has an exposed observation surface of the sample formed by polishing a portion of the molded product, and which is configured so that the observation surface can be electrolytically etched. [Background technology]

[0002] The technology relating to the above-mentioned analytical sample is described in Patent Document 1. As shown in FIG. 7, the analytical sample 100 described in Patent Document 1 is a molded product 101 formed to a predetermined size from a conductive sample 102 and a resin 104 in which the sample 102 is embedded. The lower surface of the analytical sample 100 (molded product 101) is polished with a polishing machine (not shown), thereby exposing a part of the sample 102 to form an observation surface 102s. The observation surface 102s of the analytical sample 100 is subjected to an electrolytic etching process to enable observation of the observation surface 102s.

[0003] In the electrolytic etching process, as shown in FIG. 7, the analysis sample 100 is immersed in a solution (not shown) of an electrolytic etching device. A negative electrode 105m of the electrolytic etching device is disposed at a position facing the observation surface 102s of the analysis sample 100 through the solution. A lead wire 105r is wound and fixed around the center of the sample 102, and the lead wire 105r is drawn out above the resin 104 of the molded product 101 and connected to the positive electrode of the electrolytic etching device. When a voltage is applied between the positive electrode and the negative electrode 105m of the electrolytic etching device, a current flows through the solution to the observation surface 102s of the sample 102, and electrolytic etching of the observation surface 102s of the sample 102 is performed. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] Japanese Patent Publication No. 8-271677 Summary of the Invention [Problem to be solved by the invention]

[0005] For the above-mentioned analytical sample 100, a step prior to molding of the molded product 101, i.e., before embedding the sample 102 in the resin 104, is required to wind and fix the lead wire 105r around the center of the sample 102. Furthermore, in order to pull out the lead wire 105r to the outside of a molding die (not shown) for the resin 104, it is necessary to process a hole or the like for pulling out the lead wire 105r in the molding die. For this reason, molding the analytical sample for electrolytic etching is time-consuming.

[0006] The present technology has been made to solve the above problems, and the problem that the present invention aims to solve is to make it possible to easily form an analytical sample for electrolytic etching. [Means for solving the problem]

[0007] The above-mentioned problems are solved by each technique. The first technique is an analytical sample that is a molded product formed to a predetermined size from a conductive sample and a resin in which the sample is embedded, and an exposed observation surface of the sample is formed by polishing a part of the molded product, and the observation surface is configured to be electrolytically etchable, and the molded product is polished at a position away from the observation surface of the sample to form an electrode surface of the sample that is configured to be able to abut against an electrode for electrolytic etching.

[0008] According to the first technique, the electrode surface of the sample that the electrode for electrolytic etching comes into contact with can be formed by polishing a position of the molded product away from the observation surface of the sample. That is, the observation surface and the electrode surface of the sample can be formed by polishing two places of a molded product formed to a predetermined size from a sample and a resin in which the sample is embedded. This makes it easy to create an analytical sample for electrolytic etching.

[0009] The second technique is an analytical sample that is a molded product of a predetermined size made of a resin in which a conductive sample and a conductor electrically connected to the sample are embedded, and an exposed observation surface of the sample is formed by polishing a part of the molded product, and the observation surface is configured to be electrolytically etched, and an electrode surface of the conductor that is configured to be able to abut against an electrode for electrolytic etching is formed by polishing a position of the molded product away from the observation surface of the sample. Therefore, by polishing two places of the molded product, the observation surface and the electrode surface of the sample can be formed, and an analytical sample for electrolytic etching can be easily prepared. Effect of the Invention

[0010] The present technology facilitates preparation of analytical samples for electrolytic etching. [Brief description of the drawings]

[0011] [Figure 1] FIG. 2 is a schematic vertical cross-sectional view showing a state in which an observation surface of an analysis sample according to the first embodiment of the present invention is subjected to an electrolytic etching treatment. [Diagram 2] 5A to 5C are schematic vertical cross-sectional views showing a molding process for forming a molded product for forming the analytical sample. [Diagram 3] FIG. 2 is a schematic vertical cross-sectional view showing a state at the start of a process of forming an electrode surface of the sample in the analysis sample (molded product). [Figure 4] FIG. 4 is a schematic vertical cross-sectional view showing the end state of the electrode surface formation process of the analysis sample (molded product). [Diagram 5] 3 is a schematic vertical sectional view showing a step of forming an observation surface of the sample in the analysis sample (molded product). FIG. [Figure 6] FIG. 4 is a schematic vertical sectional view showing a modified example of the analysis sample. [Figure 7] FIG. 1 is a schematic vertical cross-sectional view showing a state in which an observation surface of a conventional analytical sample is subjected to electrolytic etching treatment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0012] [Embodiment 1] An analysis sample 10 according to a first embodiment of the present invention will be described below with reference to Figures 1 to 6. The analysis sample 10 according to this embodiment is formed into a predetermined size from a conductive sample 12 and a resin 15 in which the sample 12 is embedded, and is configured so that an observation surface 12k of the sample 12 exposed by polishing can be electrolytically etched.

[0013] <About analytical sample 10> As shown in Fig. 1, the analytical sample 10 is formed into a columnar shape of a predetermined size from a conductive sample 12 and a resin 15 in which the sample 12 is embedded in the center. One axial end (upper surface) of the analytical sample 10 is polished to expose the upper surface of the sample 12, forming an electrode surface 12e. The other axial end (lower surface) of the analytical sample 10 is polished to expose the lower surface of the sample 12, forming an observation surface 12k. The sample 12 may be made of a material that can be processed by electrolytic etching, such as non-ferrous material such as aluminum or stainless steel. The resin 15 may be made of, for example, epoxy resin.

[0014] <About the electrolytic etching device 20> 1, the electrolytic etching device 20 is a device for electrolytically etching the observation surface 12k of the sample 12 of the analytical sample 10. The electrolytic etching device 20 includes a container 23 for storing a solution 21 for electrolytic etching, a positive electrode 25 installed so as to abut against the electrode surface 12e of the analytical sample 10 (sample 12) stored in the container 23, and a negative electrode 27 installed so as to face the observation surface 12k of the analytical sample 10 (sample 12) via the solution 21. The electrolytic etching device 20 also includes a power supply device 28 for supplying power for electrolytic etching to the observation surface 12k of the sample 12 via the positive electrode 25 and the negative electrode 27.

[0015] That is, when the power supply 28 of the electrolytic etching device 20 is operated and a voltage is applied between the positive electrode 25 and the negative electrode 27, a current flows between the observation surface 12k of the sample 12 and the negative electrode 27 via the solution 21, and the observation surface 12k is electrolytically etched. If the sample 12 is, for example, aluminum, a hydrofluoric acid solution is used as the solution. If the sample 12 is, for example, stainless steel, an oxalic acid solution is used as the solution.

[0016] <Procedure for forming analytical sample 10> First, as shown in Fig. 2, the sample 12 is set in the center of a mold container 31 of a predetermined size with the observation surface 12k side facing down. In this state, a predetermined amount of two types of liquid epoxy resin 15 (hereinafter referred to as resin 15) is poured into the mold container 31. Then, after the resin 15 hardens, the molded body of the resin 15, etc. is taken out of the mold container 31, and the molded product 10f is completed. In this state, the lower surface side (the observation surface 12k side) of the molded product 10f is molded in an almost flat state.

[0017] 3, the molded product 10f is set on the arm 32 of the grinder 30 with the flat lower surface (observation surface 12k side) facing up. As described above, the observation surface side of the molded product 10f is almost flat, so that the observation surface 12k side of the molded product 10f can be pressed well by the arm 32.

[0018] In this state, the polishing disk 34 of the polisher 30 rotates, and the uneven upper surface side of the molded product 10f is polished to be horizontal, as shown in Figures 3 and 4. That is, the upper surface 12e of the sample 12 becomes exposed from the resin 15 in a state where the upper surface of the resin 15 in the molded product 10f and the upper surface 12e of the sample 12 are continuous with each other. Then, the exposed upper surface 12e of the sample 12 is used as the electrode surface 12e with which the positive electrode 25 of the electrolytic etching device 20 comes into contact.

[0019] Next, as shown in Fig. 5, the molded product 10f is set on the arm 32 of the grinder 30 with the upper surface side (electrode surface 12e side) facing up. In this state, the grinding disk 34 of the grinder 30 rotates, and the lower surface side (observation surface 12k side) of the molded product 10f, which is in a substantially flat state, is polished horizontally. That is, the observation surface 12k of the sample 12 is polished so as to be completely exposed from the resin 15. Then, the lower surface 12k of the sample 12 becomes the observation surface 12k to be electrolytically etched. In this state, the molding of the analysis sample 10 is completed.

[0020] <Regarding the correspondence between the terms used in this embodiment and the terms related to the present invention> The electrode surface 12e on the upper surface side of the analytical sample 10 corresponds to the electrode surface of the sample of the present invention. Moreover, the positive electrode 25 of the electrolytic etching device 20 corresponds to the electrode for electrolytic etching.

[0021] <Advantages of the analytical sample 10 according to this embodiment> According to the analysis sample 10 of this embodiment, the electrode surface 12e of the sample 12 with which the positive electrode 25 (electrode for electrolytic etching) of the electrolytic etching device 20 abuts can be formed by polishing a position of the molded product 10f away from the observation surface 12k of the sample 12. That is, the observation surface 12k and the electrode surface 12e of the sample 12 can be formed by polishing two places of the molded product 10f, which is formed to a predetermined size from the sample 12 and the resin 15 in which the sample 12 is embedded. Therefore, the analysis sample 10 for electrolytic etching can be easily prepared.

[0022] <Change Example 1> Here, the present invention is not limited to the above embodiment, and modifications are possible within the scope of the present invention. For example, in this embodiment, the upper surface side of the molded product 10f is polished by a polishing machine 30 to form the electrode surface 12e of the sample 12, and the positive electrode 25 of the electrolytic etching device 20 is abutted against the electrode surface 12e. However, as shown in FIG. 6, it is also possible to form the molded product 10f by embedding the sample 12 and the conductor 13 electrically connected to the sample 12 via a conductive tape 13t in the resin 15. In this case, the lower surface side of the molded product 10f is polished to form the observation surface 12k of the sample 12, and the upper surface side of the molded product 10f is polished to form the electrode surface 13e of the conductor 13, thereby making it possible to prepare an analysis sample 10 for electrolytic etching. [Explanation of symbols]

[0023] 10. Analytical sample 10f...molded product 12. Sample 12k... Observation surface 12e Electrode surface (electrode surface of sample) 13 Conductor 13e Electrode surface (electrode surface of conductor) 15...Resin 20. Electrolytic etching equipment 21...solution 25 Positive electrode (electrode for electrolytic etching) 27...Negative electrode 30...polishing machine 34... Grinding disc (grinding machine)

Claims

1. An analytical sample comprising a molded product having a predetermined size made of a conductive sample and a resin in which the sample is embedded, the molded product being polished to form an exposed observation surface of the sample, the observation surface being configured to be capable of being electrolytically etched, An analytical sample in which the molded product has an electrode surface of the sample that is configured to be able to contact an electrode for electrolytic etching by polishing a position away from the observation surface of the sample.

2. An analytical sample comprising a molded product having a predetermined size made of a conductive sample and a resin in which a conductor electrically connected to the sample is embedded, the molded product being polished to form an exposed observation surface of the sample, the observation surface being configured to be capable of being electrolytically etched, An analytical sample in which the molded product has an electrode surface of the conductor formed by polishing a position away from the observation surface of the sample so that an electrode for electrolytic etching can be abutted against the electrode.

Citation Information

Patent Citations

  • Formation method for metallographic testpiece by electrolytic etching of metallographic sample

    JP1996271677A