JPH0528511Y2 - - Google Patents

Description

[Detailed Description of the Invention] (Field of Industrial Application) The present invention relates to a sample for interface analysis of materials such as various metal materials, ceramic materials, and electronic materials where the interface state affects the original function of the material.

(Conventional technology) In recent years, the properties required for materials, regardless of whether they are structural or functional materials, have become increasingly sophisticated, and when manufacturing materials, delicate control of conditions is required. I'm getting used to it. The internal state of the material changes in response to slight changes in manufacturing conditions, but atoms contained in discontinuous areas, such as phase boundaries and grain boundaries, tend to segregate and precipitate, which can affect the material properties. The material itself often changes, generally tending to deteriorate the material properties.

Because these phenomena usually occur in an extremely narrow region of less than μm across the boundary, elemental analysis is performed using physical analysis equipment with specific functions. Examples include Auger electron spectroscopy (AES), secondary ion mass spectrometry (SIMS), X-ray photoelectron spectroscopy (XPS), and ultraviolet electron spectroscopy (UPS).

As the area to be analyzed is extremely narrow, a method is often adopted in which the test specimen is broken at the interface and measured in a two-dimensional area for the purpose of more accurate measurement. Moreover, in this case, a device for breaking the test piece in order to prevent the fracture surface to be measured from being contaminated is disclosed, for example, in Japanese Utility Model Publication No. 55-20371 and Japanese Patent Application Laid-Open No.
As shown in Japanese Patent Publication No. 50-105188, Japanese Patent Publication No. 57-37102, etc., 10 ^-8 Torr as well as the analyzer.
Equipped in a high vacuum chamber.

On the other hand, when breaking a test piece, it is necessary to apply stress to the test piece, and it is essential to break brittlely so that the sample after breaking does not undergo deformation due to stress loading. For this purpose, notches are often introduced into the specimen or cooled to low temperatures.

(Problem that the invention aims to solve) When breaking a test piece in a vacuum chamber as described above, normally one end of the test piece is fixed to a holder and stress is applied to the test piece to cause it to break. The test piece on the end side was scattered and only the half fixed to the holder remained, so the fractured surface of this half piece was observed and analyzed.

However, there is no guarantee that the measurable fracture surface and the free end fracture surface left in the vacuum chamber have the same amount and state of the element to be measured. In fact, these analytical methods often result in large variations in the measured values, and although the cause is not necessarily clear, one concern is that, for example, the element to be measured is not equally distributed on both sides of the fracture surface. It is possible that there is no such phenomenon. Therefore, in order to accurately grasp the state before rupture, it is essential to measure the states of both opposing fracture surfaces, but this method requires complicated equipment and is difficult to implement.

(Means for solving the problem) The present invention solves the above problems and makes it easy to measure both sides of the fracture. The present invention relates to a test piece for double-sided fracture analysis, characterized in that a connecting body having strength enough to withstand the applied stress at the time of fracture is provided on the sample on both sides of the sample.

The present invention will be explained below with reference to the drawings. Figure 1a is a side view of the test piece of the present invention, b is a plan view, and 1 is a test piece.
2 is a notch provided in the center. Furthermore, holes 3, 3 are bored on both sides of the notch 2 in this test piece 1, and a connecting body 4 is inserted into the holes. 5 is the connected body 4
This is a trench in which the material is buried. 2 and 3 are side views showing the breaking operation, and 6 is a holder, 7 is a hammer that applies stress to the free end of the specimen 1, and 8 is an analyzer. Note that the connecting body 4 can be made of any wire, plate, hinge, or the like. However, when breaking the sample, the sample is often cooled to a low temperature, and the material needs to be one that will not break brittle. Further, it is necessary to plastically deform or rotate with a small applied stress upon fracture, and it is also necessary to have enough rigidity to allow the fracture surfaces 9, 9 to face and be fixed to the analyzer 8.

Therefore, as shown in FIG. 2, one end of the test piece of the present invention is fixed in a holder 6 in a vacuum chamber (not shown), and when an impact is applied to the other end (free end) with a hammer 7, the test piece 1 moves into the notch. 2, but since it is connected by the connecting body 4, the free end is rotated by 180° as shown in FIG. 3, and both fracture surfaces 9, 9 face the analyzer 8. Therefore, it is possible to measure both fresh fracture surfaces immediately after fracture.

(Example) Next, an example of the present invention will be shown.

As a sample, we prepared an alloy of iron with 0.09 at.
A specimen with a diameter of 3.3 mm was prepared. Furthermore, a hole was drilled in the sample with the notch in between, and a 0.6 mm copper wire was inserted into the hole.

The sample was placed in the vacuum chamber of the Auger electron spectrometer, one end was fixed with a holder, and after cooling to -100℃, the free end was ruptured by impact with a hammer, and both fractured surfaces were aligned. The amount of phosphorus present at the grain interface was measured.

FIG. 4 shows the results of 10 sets, in which the shaded values are the measured values of the fracture surface on the side fixed with the holder, and the others are the measured values of the fracture surface on the free end side.

In some cases, as in the case of No. 10, the amount of phosphorus on both fracture surfaces remains almost unchanged, but in general, the amount of phosphorus on both surfaces differs greatly, and in measurement examples, there are even cases where there is a 50% difference. Is recognized. The amount of phosphorus present in the grain boundaries at the measurement location is the sum of the amount on both sides of the fracture surface, but this is not equal to the value obtained by measuring the amount of phosphorus on one side and multiplying it by two. Therefore, it is clear that in order to perform accurate interface analysis, it is necessary to measure both sides of the fractured sample.

(Effects of the invention) As explained above, unlike conventional specimens, the specimen on the free end side is not scattered when it breaks and is parallel to the specimen on the fixed end side, so observation and analysis of the fracture surface can be carried out. can be done accurately and the effect is extremely large.

[Brief explanation of the drawing]

Fig. 1 a is a side view of the test piece of the present invention, b is a plan view, Fig. 2 is a side view showing the state during the breaking operation, Fig. 3 is a side view showing the state after breaking, and Fig. 4 is the test piece according to the present invention. It is a graph showing an example of measurement results of phosphorus. 1... Test piece, 2... Notch, 3... Hole, 4...
...Connector, 5...Groove, 6...Holder, 7...Hammer, 8...Analyzer.

Claims (1)

[Scope of utility model registration request] In a test piece in which an impact load stress is applied to the free end of a test piece with one end fixed in the sample bending direction and the test piece ruptures, the surface of the test piece on the opposite side of the test piece to which the load stress is applied is placed at the time of breakage. A test piece for fractured double-sided analysis, characterized in that it is provided with a connecting body that has strength to withstand applied stress, and is bendable so that both fractured specimens are connected at the time of fracture and their fractured surfaces face in the same direction. .