Sample analysis method and sample analysis apparatus

Abstract

This invention provides a sample analysis method and apparatus that enable precise control of sample temperature over a wide temperature range and allow for in-situ analysis while filling the sample with hydrogen. [Solution] A method for analyzing a sample 1 made of metal, comprising: (a) placing the sample 1 inside a container 11 having an analysis window 11a and making the atmosphere inside the container 11 a hydrogen-containing gas with a pressure P of 1 to 2000 Pa; (b) plasma-generating the hydrogen-containing gas and bringing the plasma-generated hydrogen-containing gas into contact with the surface 1a of the sample 1; and (c) analyzing the surface 1a by injecting electromagnetic waves onto the surface 1a through the analysis window 11a.

Description

[Technical Field]

[0001] The present invention relates to a sample analysis method and a sample analysis apparatus. [Background Art]

[0002] In the development of high-strength steel, hydrogen embrittlement, in which strength and toughness are degraded by hydrogen, has become a major problem. However, the microstructural changes in materials related to hydrogen embrittlement have not been clarified, and in order to elucidate the mechanism of hydrogen embrittlement, it is desired to perform in-situ analysis on steel materials over time while introducing hydrogen into the steel. Specifically, it is desired to analyze over time the initiation site and propagation path of hydrogen embrittlement cracks, the formation of hydrides, the change in internal stress caused by hydrogen, the change in crystal structure caused by hydrogen, and the like.

[0003] For example, Patent Document 1 discloses a method of charging hydrogen by exposing a test piece to high-pressure hydrogen gas. Further, Patent Document 2 discloses a method of electrochemically charging hydrogen by immersing a steel material in an electrolytic solution. Furthermore, Patent Document 3 discloses a sample analysis method capable of analyzing a sample surface with high resolution over time using an electron beam apparatus while introducing hydrogen into the sample. [Prior Art Documents] [Patent Documents]

[0004] [Patent Document 1] Japanese Unexamined Patent Publication No. 2019-143228 [Patent Document 2] Japanese Unexamined Patent Publication No. 2020-30186 [Patent Document 3] Japanese Unexamined Patent Publication No. 2019-45409 [Patent Document 4] Japanese Patent Application No. 2023-202169 [Summary of the Invention] [Problems to be Solved by the Invention]

[0005] However, the method described in Patent Document 1 uses high-pressure hydrogen gas, which poses an explosion risk. Therefore, it requires large-scale equipment such as pressure vessels, gas compressors, and explosion-proof infrastructure, resulting in significant costs. Furthermore, analytical instruments such as microscopes are typically structurally unsuitable for use in high-pressure hydrogen gas.

[0006] Furthermore, although the method described in Patent Document 2 allows for efficient hydrogen filling, hydrogen bubbles are generated on the sample surface in the electrolyte, which may interfere with the analysis. In addition, corrosion of the sample surface by the electrolyte is also a concern.

[0007] The method described in Patent Document 3 involves observation using an electron microscope or the like. This method is not suitable for analyzing hydride formation or changes in internal stress due to hydrogen. Furthermore, its temporal resolution is not sufficiently high.

[0008] Against this backdrop, the inventors have so far developed a hydrogen filling method and hydrogen filling apparatus capable of filling a sample with hydrogen under atmospheric pressure, as well as a sample analysis method and sample analysis apparatus capable of analyzing the sample surface over time with high temporal resolution under atmospheric pressure while filling the sample with hydrogen (see Patent Document 4).

[0009] The method described in Patent Document 4 involves generating a hydrogen-containing gas into a low-temperature plasma under atmospheric pressure, and then bringing the low-temperature plasma-generated hydrogen-containing gas into contact with the sample under atmospheric pressure, thereby enabling the sample to be filled with hydrogen under atmospheric pressure.

[0010] However, in order to develop steels for use in high-temperature or low-temperature environments, it is also necessary to develop in-situ analysis that can control the temperature of the sample over a wide temperature range. In the method described in Patent Document 4, heat transfer occurs at the sample surface due to convection caused by hydrogen-containing gas, making it difficult to precisely control the temperature of the sample at extremely high or extremely low temperatures.

[0011] The present invention aims to provide a sample analysis method and sample analysis apparatus that enable precise control of the sample temperature over a wide temperature range and allow in-situ analysis while filling the sample with hydrogen. [Means for solving the problem]

[0012] This invention was made to solve the above problems, and its essence is the following sample analysis method and sample analysis apparatus.

[0013] (1) A method for analyzing a sample made of metal, (a) A step of placing the sample inside a container having an analysis window, and making the atmosphere inside the container a hydrogen-containing gas with a pressure P of 1 to 2000 Pa, (b) A step of plasmaizing the hydrogen-containing gas and bringing the plasmaized hydrogen-containing gas into contact with the surface of the sample, (c) The process of analyzing the surface by incidenting electromagnetic waves onto the surface and detecting the electromagnetic waves reflected from the surface outside the container through the analysis window, Sample analysis method.

[0014] (2) In step (c) above, the sample is analyzed by passing the reflected electromagnetic waves through an objective lens. The sample analysis method described in (1) above.

[0015] (3) In step (a) above, the sample is placed inside the container such that the distance L between the outer surface of the container of the analysis window and the surface is 40 mm or less. The sample analysis method described in (2) above.

[0016] (4) In step (b) above, an electrode is placed inside the container or the container itself is used as an electrode, and a DC voltage is applied between the electrode and the sample to generate a glow discharge between the electrode and the surface, thereby plasmaizing the hydrogen-containing gas, and the plasmaized hydrogen-containing gas is brought into contact with the surface of the sample. The sample analysis method described in (1) above.

[0017] (5) In the step (c), the sample is analyzed by causing the reflected electromagnetic wave to pass through an objective lens, The sample analysis method according to (4) above.

[0018] (6) In the step (a), the sample is placed inside the container such that a distance L between the outer surface of the container at the analysis window and said surface is 40 mm or less, The sample analysis method according to (5) above.

[0019] (7) A straight-line distance d from said surface to the farthest portion of said electrode when there is no obstacle therebetween is 15 to 500 mm, The sample analysis method according to (6) above.

[0020] (8) A product of the pressure P of the hydrogen-containing gas and the straight-line distance d is 10 3 to 10 5 Pa·mm, The sample analysis method according to (7) above.

[0021] (9) In the step (b), the plasmatized hydrogen-containing gas is brought into contact with said surface in a state where the temperature of said surface is controlled to a predetermined temperature, The sample analysis method according to any one of (1) to (8) above.

[0022] (10) The method further comprises (d) a step of applying a stress to the sample, The sample analysis method according to any one of (1) to (8) above.

[0023] (11) The method further comprises (d) a step of applying a stress to the sample, The sample analysis method according to (9) above.

[0024] (12) An analysis apparatus for a sample made of metal, comprising: a container having an analysis window and allowing the sample to be placed therein; and The container is equipped with an atmosphere adjustment unit that creates a hydrogen-containing gas atmosphere with a pressure P of 1 to 2000 Pa inside the container, A plasma generating unit that plasmaizes the hydrogen-containing gas and brings the plasma-generated hydrogen-containing gas into contact with the surface of the sample, The system includes an analysis unit that analyzes the surface by incidenting electromagnetic waves onto the surface and detecting the electromagnetic waves reflected from the surface through the analysis window outside the container. Sample analysis device.

[0025] (13) The analysis unit is a device that analyzes the sample by passing the reflected electromagnetic waves through an objective lens. The sample analysis apparatus described in (12) above.

[0026] (14) The sample can be placed inside the container such that the distance L between the outer surface of the container and the surface of the analysis window is 40 mm or less. The sample analysis apparatus described in (13) above.

[0027] (15) The plasma generating unit has an electrode installed inside the container or the container itself is an electrode, and applies a DC voltage between the electrode and the sample, generates a glow discharge between the electrode and the surface, thereby plasmaizing the hydrogen-containing gas, and brings the plasmaized hydrogen-containing gas into contact with the surface of the sample. The sample analysis apparatus described in (12) above.

[0028] (16) The analysis unit is a device that analyzes the sample by passing the reflected electromagnetic waves through an objective lens. The sample analysis apparatus described in (15) above.

[0029] (17) The sample can be placed inside the container such that the distance L between the outer surface of the container and the surface of the analysis window is 40 mm or less. The sample analysis apparatus described in (16) above.

[0030] (18) The straight-line distance d from the surface to the furthest part of the electrode, when there are no obstacles in between, is 15 to 500 mm. The sample analysis apparatus described in (17) above.

[0031] (19) Further comprising a temperature control unit that controls the temperature of the surface to a predetermined temperature, A sample analysis device as described in any of the above (12) to (18).

[0032] (20) Further comprising a stress loading section for applying stress to the sample, A sample analysis device as described in any of the above (12) to (18).

[0033] (21) Further comprising a stress loading section for applying stress to the sample, The sample analysis apparatus described in (19) above. [Effects of the Invention]

[0034] According to the present invention, precise control of the sample temperature is possible over a wide temperature range, and it becomes possible to analyze the sample surface in situ while filling the sample with hydrogen. [Brief explanation of the drawing]

[0035] [Figure 1] This figure shows a schematic configuration of a sample analysis device according to one embodiment of the present invention. [Figure 2] This figure shows a cross-section perpendicular to the normal direction on the normal side of the surface of the sample. [Figure 3] This figure shows a schematic configuration of a sample analysis device according to another embodiment of the present invention. [Figure 4] This figure shows a schematic configuration of a sample analysis device according to another embodiment of the present invention. [Figure 5] This figure shows a schematic configuration of a sample analysis device according to another embodiment of the present invention. [Figure 6] This is a diagram illustrating the dimensions and shape of the test specimen. [Figure 7]This is a diagram illustrating the dimensions and shape of a wedge. [Figure 8] These are optical microscope images of the test specimens before and after hydrogen filling. [Figure 9] This figure shows the schematic configuration of the sample analysis device used in the example. [Modes for carrying out the invention]

[0036] A sample analysis method and sample analysis apparatus according to embodiments of the present invention will be described with reference to Figures 1 to 5.

[0037] Figure 1 shows a schematic configuration of a sample analysis device 100 according to one embodiment of the present invention. The sample analysis device 100 is an analysis device for a sample 1 made of metal. The sample analysis device 100 comprises a container 11, an atmosphere adjustment unit 12, a plasma generation unit 13, and an analysis unit 14.

[0038] The container 11 has an analysis window 11a and is structured to allow the sample 1 to be placed inside. There are no particular restrictions on the material, shape, and dimensions of the container 11, but it must be able to maintain a high degree of vacuum inside.

[0039] The atmosphere adjustment unit 12 adjusts the atmosphere inside the container 11 to a hydrogen-containing gas atmosphere with a pressure P of 1 to 2000 Pa. In the configuration shown in Figure 1, the atmosphere adjustment unit 12 includes, but is not limited to, a mass flow controller 12a for supplying hydrogen-containing gas by adjusting the flow rate, a vacuum pump 12b for reducing the pressure inside the container 11, and a flow control valve 12c for adjusting the exhaust volume of the vacuum pump 12b. By setting the pressure P to 1 Pa or higher, it becomes possible to generate plasma inside the container 11. On the other hand, by setting the pressure P to a low pressure of 2000 Pa or less, the discharge current flowing through the sample 1 becomes smaller, suppressing heating of the sample 1 by plasma, and reducing heat transfer in the sample 1 by convection, making it possible to precisely control the sample temperature over a wide temperature range, for example, -200 to 1200°C.

[0040] As the hydrogen-containing gas, for example, a mixed gas of hydrogen and an inert gas (noble gas, nitrogen, carbon dioxide) can be used. More preferably, a mixed gas of helium and hydrogen is used. Using an inert gas other than helium may damage or alter the sample due to oxidation or sputtering. When using a mixed gas, the partial pressure of hydrogen in the mixed gas is preferably 1 Pa or higher. From the viewpoint of filling with as much hydrogen as possible at the lowest possible pressure, a pure hydrogen gas is preferred.

[0041] To stably fill sample 1 with hydrogen, it is preferable to continuously replace the hydrogen-containing gas inside container 11. The hydrogen-containing gas replacement flow rate Q is preferably 0.1 to 500 sccm. The replacement flow rate Q and pressure P are controlled by a mass flow controller 12a and a flow control valve 12c.

[0042] The plasma generation unit 13 converts hydrogen-containing gas into plasma and brings the plasma-converted hydrogen-containing gas into contact with the surface 1a of the sample 1. The hydrogen-containing gas is converted into plasma by DC discharge, AC discharge, high-frequency discharge, microwave discharge, etc. In the configuration shown in Figure 1, a pair of electrodes 13a and 13b are placed inside the container 11, and a DC voltage is applied so that electrodes 13a and 13b become the anode and the sample 1 becomes the cathode, generating a glow discharge between electrodes 13a and 13b and the sample 1 to convert the hydrogen-containing gas into plasma. By bringing the plasma-converted hydrogen-containing gas into contact with the surface 1a, it becomes possible to efficiently fill the sample 1 with hydrogen. Alternatively, a DC voltage may be applied so that electrodes 13a and 13b become the cathode and the sample 1 becomes the anode, or, although electrodes 13a and 13b are grounded in the configuration shown in Figure 1, the sample 1 may also be grounded.

[0043] In the configuration shown in Figure 1, a pair of electrodes 13a and 13b are placed inside the container 11, but this is not the only configuration. Figure 2 shows a cross-section perpendicular to the normal direction on the normal side of the surface 1a of the sample 1. As shown in Figure 2(a), four electrodes 13c, d, e, and 13f may be provided at 90° intervals, or as shown in Figure 2(b), a cylindrical electrode 13g may be used. Furthermore, as shown in Figure 2(c), the container itself may be used as electrode 13h.

[0044] In the configuration shown in Figure 1, the sample 1 and the DC power supply 13i are directly connected. However, as shown in Figure 3, the sample 1 may be placed on a conductive sample stage 11b, thereby indirectly connecting it to the DC power supply 13i via the sample stage 11b.

[0045] The analysis unit 14 analyzes the surface 1a by injecting electromagnetic waves (hereinafter referred to as "incident electromagnetic waves") onto the surface 1a and detecting the electromagnetic waves reflected from the surface 1a (hereinafter referred to as "reflected electromagnetic waves") outside the container 11 through the analysis window 11a. The incident electromagnetic waves may be injected from inside the container 11 or from outside the container 11 through the analysis window 11a. Furthermore, the reflected electromagnetic waves include electromagnetic waves scattered by the surface 1a after the incident electromagnetic waves are injected, and electromagnetic waves diffracted by the surface 1a.

[0046] In the configuration shown in Figure 1, the analysis unit 14 is an optical microscope, using visible light as the incident and reflected electromagnetic waves. Since the outside of the container 11 is under atmospheric pressure, the optical microscope and the like can be easily installed and used, and through the analysis window 11a, it becomes possible to perform in-situ analysis over time with high temporal resolution, for example, of the process by which hydrogen embrittlement occurs.

[0047] If the analysis unit 14 is a device that analyzes the sample 1 by passing reflected electromagnetic waves, such as an optical microscope, through an objective lens, it is desirable to place the analysis unit 14 as close as possible to the surface 1a of the sample 1, taking into account the working distance of the objective lens. Therefore, it is preferable to place the sample 1 inside the container 11 such that the distance L between the outer surface 11c of the container 11 of the analysis window 11a and the surface 1a is 40 mm or less.

[0048] However, when the distance L is reduced, the distance between the electrode and the sample usually also decreases, making it difficult to secure a large area of ​​surface 1a that can generate a glow discharge and be analyzed. Therefore, as a result of the inventors' investigation into electrode arrangement, it is preferable to arrange the electrodes so that the normal direction of surface 1a and the normal direction of electrodes 13a and 13b are approximately perpendicular to each other, as shown in Figure 1, and to set the straight-line distance d from surface 1a to the furthest point of electrodes 13a and 13b in the absence of obstacles between them to 15 to 500 mm.

[0049] By setting the linear distance d to 15 mm or more, it becomes possible to stably generate glow discharge between electrodes 13a,b and sample 1, and to secure a wide area of ​​surface 1a that can be analyzed. On the other hand, if the linear distance d exceeds 500 mm, it becomes difficult to keep the distance L below 40 mm.

[0050] Similarly, in order to stably generate a glow discharge between electrodes 13a,b and sample 1, the product of the hydrogen-containing gas pressure P and the linear distance d should be 10 3 ~10 5 It is preferable to use Pa·mm. If the product of the pressure P and the linear distance d is within the above range, it becomes possible to stably generate a glow discharge, for example, when using a typical DC power supply with a maximum voltage of 5kV.

[0051] The analysis unit 14 is not limited to an optical microscope, but may also be various analysis devices that emit electromagnetic waves, such as a laser microscope, a micro-Raman spectrometer, a micro-FT-IR, or an X-ray diffraction device.

[0052] Figure 4 shows a schematic configuration of a sample analysis device 100 according to another embodiment of the present invention. In the configuration shown in Figure 4, the sample analysis device 100 further includes a temperature control unit 15. The temperature control unit 15 controls the temperature of the surface 1a of the sample 1 to a predetermined temperature. For example, it is possible to maintain the temperature of the surface 1a at a high temperature or at a low temperature. As described above, in the sample analysis device 100, the inside of the container 11 can be kept at a low pressure, so that the heat transfer in the sample 1 due to convection is reduced. As a result, the temperature control unit 15 can precisely control the temperature of the surface 1a over a wide temperature range, for example, -200 to 1200°C.

[0053] Figure 5 shows a schematic configuration of a sample analysis device 100 according to another embodiment of the present invention. In the configuration shown in Figure 5, the sample analysis device 100 further comprises a stress loading unit 16. The stress loading unit 16 applies stress to the sample 1. The type of stress applied to the sample 1 is not particularly limited and may be any of tensile stress, compressive stress, bending stress, torsional stress, or shear stress.

[0054] Furthermore, the sample analysis device 100 may also include both a temperature control unit 15 and a stress loading unit 16.

[0055] In the above description, there are no particular restrictions on the type of sample as long as it is a metal, and examples include carbon steel, alloy steel, stainless steel, Ni-based alloys, Al alloys, Ti alloys, etc. In particular, carbon steel has a large hydrogen diffusion coefficient and is difficult to maintain in a hydrogen-filled state for a long period of time. For this reason, the sample analysis method and sample analysis apparatus according to the present invention can be suitably used when carbon steel is the target.

[0056] Furthermore, there are no particular restrictions on the shape of the sample; for example, it may be plate-shaped, cylindrical, or even in the shape of an actual product (e.g., bolt-shaped). There are also no particular restrictions on the dimensions of the sample, as long as it can be installed within the container. Suitable materials for the electrode and sample stage include copper, silver, aluminum, iron, stainless steel, etc., which have good conductivity.

[0057] The present invention will be described more specifically below with reference to examples, but the present invention is not limited to these examples. [Examples]

[0058] JIS-SCM435 steel (tensile strength 1892 MPa) was used as the sample. A test specimen with the dimensions and shape shown in Figure 6 was taken from this sample, and a wedge with the dimensions and shape shown in Figure 7 was inserted into the notch to introduce the pre-crack shown in Figure 8(a). The wedge was held in place while inserted into the test specimen, and a constant strain was applied to the specimen.

[0059] Subsequently, sample 1 was placed inside the sample analysis apparatus 100 shown in Figure 9. After creating a vacuum inside container 11 using the vacuum pump 12b, hydrogen gas was continuously supplied at a displacement flow rate of 2 sccm by the mass flow controller 12a and flow control valve 12c, maintaining the pressure inside container 1 at 100 Pa. Then, under the conditions of a discharge current of 3 mA and an applied voltage of 310 V, a glow discharge was generated between sample 1 and electrodes 13a and 13b to plasmaize the hydrogen gas. Here, container 11 was made of stainless steel, and as shown in Figure 9, container 11 itself served as electrode 13h. By bringing the plasmaized hydrogen gas into contact with the surface 1a of sample 1, hydrogen was filled into the sample, and in-situ observation was performed using an optical microscope in that state.

[0060] As a result, as shown in Figures 8(b) to 8(h), it was possible to observe how cracks propagate due to hydrogen embrittlement. The numbers in the upper right corner of each figure in Figure 8 indicate the time from the start of discharge. By using the sample analysis device of this embodiment, it was possible to induce cracks due to hydrogen embrittlement and analyze their behavior in situ with high temporal resolution. [Industrial applicability]

[0061] According to the present invention, precise control of the sample temperature is possible over a wide temperature range, and it becomes possible to analyze the sample surface in situ while filling the sample with hydrogen. [Explanation of Symbols]

[0062] 1. Sample 1a.Surface 11. Container 11a. Analysis window 11b. Sample stage 11c. 12. Atmosphere Adjustment Unit 12a. Mass flow controller 12b. Vacuum pump 12c. Flow control valve 13. Plasma generation unit 13a-h. Electrode 13i.DC power supply 14.Analysis Department 15. Temperature Control Unit 16. Stress Loading Section 100. Sample analysis device

Claims

1. A method for analyzing a sample made of metal, (a) A step of placing the sample inside a container having an analysis window, and making the atmosphere inside the container a hydrogen-containing gas with a pressure P of 1 to 2000 Pa, (b) A step of plasmaizing the hydrogen-containing gas and bringing the plasmaized hydrogen-containing gas into contact with the surface of the sample, (c) The process of analyzing the surface by incidenting electromagnetic waves onto the surface and detecting the electromagnetic waves reflected from the surface outside the container through the analysis window, Sample analysis method.

2. In step (c) above, the sample is analyzed by passing the reflected electromagnetic waves through an objective lens. The sample analysis method according to claim 1.

3. In step (a) above, the sample is placed inside the container such that the distance L between the outer surface of the container of the analysis window and the surface is 40 mm or less. The sample analysis method according to claim 2.

4. In step (b) above, an electrode is placed inside the container, or the container itself is used as an electrode, and a DC voltage is applied between the electrode and the sample to generate a glow discharge between the electrode and the surface, thereby plasmaizing the hydrogen-containing gas, and the plasmaized hydrogen-containing gas is brought into contact with the surface of the sample. The sample analysis method according to claim 1.

5. In step (c) above, the sample is analyzed by passing the reflected electromagnetic waves through an objective lens. The sample analysis method according to claim 4.

6. In step (a) above, the sample is placed inside the container such that the distance L between the outer surface of the container of the analysis window and the surface is 40 mm or less. The sample analysis method according to claim 5.

7. The straight-line distance d from the surface to the furthest point of the electrode, when there are no obstacles in between, is 15 to 500 mm. The sample analysis method according to claim 6.

8. The product of the pressure P and the straight-line distance d of the hydrogen-containing gas is 10 ３ ~10 ５ It is Pa·mm. The sample analysis method according to claim 7.

9. In step (b) above, while the surface temperature is controlled to a predetermined temperature, the plasma-generated hydrogen-containing gas is brought into contact with the surface. A sample analysis method according to any one of claims 1 to 8.

10. (d) Further comprising the step of applying stress to the sample, A sample analysis method according to any one of claims 1 to 8.

11. (d) Further comprising the step of applying stress to the sample, The sample analysis method according to claim 9.

12. An analytical apparatus for samples made of metal, A container having an analysis window and capable of holding the sample inside, The container is equipped with an atmosphere adjustment unit that creates a hydrogen-containing gas atmosphere with a pressure P of 1 to 2000 Pa inside the container, A plasma generating unit that plasmaizes the hydrogen-containing gas and brings the plasma-generated hydrogen-containing gas into contact with the surface of the sample, The system includes an analysis unit that analyzes the surface by incidenting electromagnetic waves onto the surface and detecting the electromagnetic waves reflected from the surface through the analysis window outside the container. Sample analysis device.

13. The aforementioned analysis unit is a device that analyzes the sample by passing the reflected electromagnetic waves through an objective lens. The sample analysis apparatus according to claim 12.

14. The sample can be placed inside the container such that the distance L between the outer surface of the container and the surface of the analysis window is 40 mm or less. The sample analysis apparatus according to claim 13.

15. The plasma generating unit has an electrode installed inside the container, or the container itself is used as an electrode, and applies a DC voltage between the electrode and the sample, generating a glow discharge between the electrode and the surface to plasmaize the hydrogen-containing gas, and brings the plasmaized hydrogen-containing gas into contact with the surface of the sample. The sample analysis apparatus according to claim 12.

16. The aforementioned analysis unit is a device that analyzes the sample by passing the reflected electromagnetic waves through an objective lens. The sample analysis apparatus according to claim 15.

17. The sample can be placed inside the container such that the distance L between the outer surface of the container and the surface of the analysis window is 40 mm or less. The sample analysis apparatus according to claim 16.

18. The straight-line distance d from the surface to the furthest point of the electrode, in the absence of any obstacles in between, is 15 to 500 mm. The sample analysis apparatus according to claim 17.

19. The system further includes a temperature control unit that controls the temperature of the surface to a predetermined temperature. A sample analysis apparatus according to any one of claims 12 to 18.

20. The system further comprises a stress loading section for applying stress to the aforementioned sample. A sample analysis apparatus according to any one of claims 12 to 18.

21. The system further comprises a stress loading section for applying stress to the aforementioned sample. The sample analysis apparatus according to claim 19.

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