Sample analysis method and sample analysis device

Abstract

The invention relates to a sample analysis method and a sample analysis apparatus, which can analyze the internal state of a sample with high precision. In a first X-direction cutting step following the first Z-direction cutting step, the load applied to the cutting blade in the X direction is measured while cutting the sample in the X direction. In a second X-direction cutting step following the second Z-direction cutting step, the load applied to the cutting blade in the X direction is measured while the sample is cut in the X direction. In the first second Z-direction cutting step, the sample is cut to a position lower in the Z direction than the cutting position in the first X-direction cutting step. In the second Z-direction cutting step after the second time, the sample is cut to a position closer to the lower part in the Z direction than the cutting position in the second X-direction cutting step performed immediately before. The internal state of the sample is analyzed on the basis of the X-direction load measured in the first and second X-direction cutting steps.

Description

Technical Field

[0001] The present invention relates to a specimen analysis method and a specimen analysis device for analyzing the internal state of a specimen. Background Art

[0002] In a lithium battery, if the component distribution inside the electrode is uneven, the performance will deteriorate. Patent Document 1 discloses a method of analyzing the internal state of an electrode using a cutting device.

[0003] Patent Document 1: Japanese Patent Laid-Open Publication No. 2022-137005 Summary of the Invention

[0004] -Technical Problem to be Solved-

[0005] In recent years, there has been a desire to analyze the internal state of a specimen with higher precision.

[0006] An object of the present invention is to provide a specimen analysis method and a specimen analysis device capable of analyzing the internal state of a specimen with high precision.

[0007] -Technical Solution for Solving the Technical Problem-

[0008] To achieve the above object, the specimen analysis method according to the present invention is a specimen analysis method for analyzing the internal state of a specimen using a cutting device. The cutting device includes a cutting edge, a specimen stage, and a drive unit. The specimen stage fixes the specimen, and the drive unit moves the cutting edge relative to the specimen stage. The cutting edge and the specimen stage can move relative to each other in the X direction, the Y direction, and the Z direction. The X direction and the Y direction are parallel to the surface of the specimen and orthogonal to each other, and the Z direction is perpendicular to the surface of the specimen.

[0009] The sample analysis method according to the present invention includes a first Z-direction cutting process, a first X-direction cutting process, a second Z-direction cutting process, and a second X-direction cutting process. In the first Z-direction cutting process, the cutting edge is relatively moved with respect to the sample stage in the downward direction in the Z direction, or in the downward direction in the Z direction and the forward direction in the X direction, thereby performing cutting starting from the surface of the sample. After the first Z-direction cutting process, immediately in the first X-direction cutting process, while relatively moving the cutting edge with respect to the sample stage in the forward direction in the X direction to cut the sample, the load in the X direction applied to the cutting edge is measured. After the first X-direction cutting process, in the second Z-direction cutting process, the cutting edge is relatively moved with respect to the sample stage in the downward direction in the Z direction, or in the downward direction in the Z direction and the forward direction in the X direction, thereby cutting the sample. After the second Z-direction cutting process, immediately in the second X-direction cutting process, while relatively moving the cutting edge with respect to the sample stage in the forward direction in the X direction to cut the sample, the load in the X direction applied to the cutting edge is measured.

[0010] The second Z-direction cutting process and the second X-direction cutting process are each performed at least once. In the first second Z-direction cutting process, the sample is cut until the cutting edge reaches a position closer to the lower side in the Z direction than the cutting position of the first X-direction cutting process. In the second and subsequent second Z-direction cutting processes, the sample is cut until a position closer to the lower side in the Z direction than the cutting position of the immediately preceding second X-direction cutting process.

[0011] The sample analysis method according to the present invention further includes an analysis process, in which the internal state of the sample is analyzed based on the load in the X direction measured in the first X-direction cutting process and the second X-direction cutting process.

[0012] According to the sample analysis method according to the present invention described above, since the cutting edge is relatively moved in the X direction with respect to the sample while cutting in the first X-direction cutting process and the second X-direction cutting process, and the load in the X direction applied to the cutting edge is measured, the load in the X direction at different depths (Z-direction positions) in the sample can be obtained with high precision. Therefore, the internal state of the sample can be analyzed three-dimensionally and with high precision using the measured value of the load in the X direction.

[0013] In the sample analysis method according to the present invention, it may also be that in each of the first X-direction cutting process and the second X-direction cutting process, the cutting ranges in the X direction and the Y direction include the same area. In this way, the state of a specific three-dimensional area inside the sample can be analyzed with high precision using the load measurement value in the X direction.

[0014] In the sample analysis method according to the present invention, it may also be that in the case of performing the second Z-direction cutting process once, the second Z-direction cutting process is performed starting from the cutting surface of the first Z-direction cutting process or the first X-direction cutting process; in the case of performing the second Z-direction cutting process two or more times, the subsequently performed second Z-direction cutting process is performed starting from the cutting surface of the immediately preceding second Z-direction cutting process or the second X-direction cutting process. In this way, compared with the case of starting cutting from the sample surface in each second Z-direction cutting process, the cutting distance is shorter, so the time required for analysis can be significantly shortened.

[0015] In the sample analysis method according to the present invention, it may also be that the analysis process includes a first analysis process and a second analysis process. In the first analysis process, the average value of the loads in the X direction measured in the same specific section in the X direction in the first X-direction cutting process and the second X-direction cutting process is obtained. In the second analysis process, the internal state of the sample is analyzed by comparing the average values of the loads in the X direction obtained in the first analysis process with each other. In this way, the internal state of the sample can be analyzed with higher precision using the average values of the loads in the X direction at different depths (Z-direction positions) of the sample.

[0016] In the sample analysis method according to the present invention, it may also be that the sample is an electrode for a battery. In this way, the internal state of the battery electrode can be analyzed three-dimensionally and with high precision.

[0017] The sample analysis device according to the present invention is a sample analysis device for analyzing the internal state of a sample, and includes a cutting edge, a sample stage, a driving unit, a control unit, and an analysis unit. The sample stage fixes the sample, the driving unit moves the cutting edge relative to the sample stage, the control unit controls the driving of the driving unit, and the analysis unit analyzes the internal state of the sample. The cutting edge and the sample stage can move relative to each other in the X direction, the Y direction, and the Z direction. The X direction and the Y direction are parallel to the surface of the sample and orthogonal to each other, and the Z direction is perpendicular to the surface of the sample.

[0018] The control unit incorporates a first command, a second command, a third command, and a fourth command. The first command causes a first Z-direction cutting process to be performed. In the first Z-direction cutting process, the cutting edge is relatively moved with respect to the sample stage in the downward direction in the Z-direction, or in the downward direction in the Z-direction and the forward direction in the X-direction, thereby performing cutting starting from the surface of the sample. The second command causes a first X-direction cutting process to be performed immediately after the first Z-direction cutting process. In the first X-direction cutting process, while relatively moving the cutting edge with respect to the sample stage in the forward direction in the X-direction to cut the sample, the load in the X-direction applied to the cutting edge is measured. The third command causes a second Z-direction cutting process to be performed at least once after the first X-direction cutting process. In the second Z-direction cutting process, the sample is cut by relatively moving the cutting edge with respect to the sample stage in the downward direction in the Z-direction, or in the downward direction in the Z-direction and the forward direction in the X-direction. The fourth command causes a second X-direction cutting process to be performed at least once immediately after the second Z-direction cutting process. In the second X-direction cutting process, while relatively moving the cutting edge with respect to the sample stage in the forward direction in the X-direction to cut the sample, the load in the X-direction applied to the cutting edge is measured.

[0019] The third command includes the following command. Under this command, in the first second Z-direction cutting process, the sample is cut until a position closer to the lower side in the Z-direction than the cutting position of the first X-direction cutting process. In the second and subsequent second Z-direction cutting processes, the sample is cut until a position closer to the lower side in the Z-direction than the cutting position of the second X-direction cutting process immediately before the implementation.

[0020] The analysis unit analyzes the internal state of the sample based on the load in the X-direction measured in the first X-direction cutting process and the second X-direction cutting process.

[0021] In the sample analysis device according to the present invention described above, since the cutting edge is relatively moved in the X-direction with respect to the sample while cutting in the first X-direction cutting process and the second X-direction cutting process, and the load in the X-direction applied to the cutting edge is measured, the load in the X-direction at different depths (Z-direction positions) in the sample can be obtained with high precision. Therefore, the internal state of the sample can be analyzed three-dimensionally and with high precision using the measured value of the load in the X-direction.

[0022] -Effects of the Invention-

[0023] According to the present invention, it is possible to provide a sample analysis method and a sample analysis apparatus capable of analyzing the internal state of a sample with high accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is a sectional structure diagram of the sample analysis apparatus according to the embodiment;

[0025] Figure 2 is a partial perspective view of the sample analysis apparatus according to the embodiment;

[0026] Figure 3 is a diagram for explaining the moving direction of the cutting edge in the sample analysis method according to the embodiment;

[0027] Figure 4 is a diagram schematically illustrating an example of the sample analysis method according to the embodiment;

[0028] Figure 5 shows Figure 4 a diagram of the cutting ranges in the X direction and the Y direction in the sample analysis method shown;

[0029] Figure 6 shows Figure 4 a diagram of the load (horizontal load) in the X direction measured in the sample analysis method shown.

[0030] -SYMBOL DESCRIPTION-

[0031] 1 - Sample analysis apparatus; 2 - Cutting edge; 3 - Sample; 4 - Sample stage; 10 - Main body portion; 11 - Cutting edge support portion; 12 - Driving unit (X-direction moving motor); 13 - X-direction thread cutting rod; 14 - Support table; 15 - X-direction displacement meter; 16 - X-direction sliding member; 17 - X-direction guide shaft; 18 - Driving unit (Z-direction moving motor); 19 - Connecting portion; 20 - Z-direction thread cutting rod; 21 - Nut; 22 - Z-direction displacement meter; 23 - Z-direction guide shaft; 24 - Z-direction sliding member; 25 - Z-direction pressure detector; 26 - X-direction pressure detection sliding member; 27 - Y-direction sliding member; 28 - Y-direction guide shaft; 29 - X-direction pressure detector; 30 - Main body support portion; 31 - Driving unit (Y-direction moving motor); 32 - Y-direction thread cutting rod; 35 - X-direction pressure detection guide shaft; 36 - X-direction inclination adjustment unit; 37 - Y-direction inclination adjustment unit; 38 - XY-direction position adjustment member; 40 - Control portion; 41 - Input interface; 42 - First output interface; 43 - Second output interface. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0032] (Embodiment)

[0033] Hereinafter, a sample analysis method according to an embodiment and a sample analysis apparatus capable of implementing the sample analysis method will be described with reference to the accompanying drawings.

[0034] <Sample Analysis Apparatus>

[0035] Figure 1 is a cross-sectional structure diagram of the sample analysis apparatus according to the present embodiment, Figure 2 is a partial perspective view of the sample analysis apparatus according to the present embodiment.

[0036] As Figure 1 , Figure 2 shown, the sample analysis apparatus 1 according to the present embodiment includes a cutting edge 2, a sample stage 4, drive units 12, 18, 31, and a control unit 40. Among them, the sample stage 4 fixes the sample 3, and the drive units 12, 18, 31 move the cutting edge 2 relative to the sample stage 4, and the control unit 40 controls the operation of the drive units 12, 18, 31.

[0037] The cutting edge 2 and the sample stage 4 can move relative to each other in the X direction, the Y direction, and the Z direction, respectively. Among them, the X direction and the Y direction are parallel to the surface of the sample 3 and orthogonal to each other, and the Z direction is perpendicular to the surface of the sample 3. Figure 3 is a diagram for explaining the direction in which the cutting edge 2 moves relative to the sample stage 4. In the present embodiment, the cutting edge 2 can move relative to the sample stage 4 along Figure 3 the three-axis directions shown, that is, it can move relative to the sample stage 4 along the cutting direction of the cutting edge 2, that is, the X direction, the Y direction (the width direction of the cutting edge 2) orthogonal to the X direction, and the Z direction perpendicular to the surface of the sample 3. It should be noted that the forward direction and the backward direction in the X direction are respectively referred to as the “+X direction” and the “−X direction”, and the downward direction and the upward direction in the Z direction are respectively referred to as the “+Z direction” and the “−Z direction”.

[0038] The cutting edge 2 is supported on the cutting-edge support portion 11, and the cutting-edge support portion 11 is held on the main body portion 10. The cutting edge 2 can move in the X direction (the extending direction of the cutting line) together with the main body portion 10 and the cutting-edge support portion 11 by a driving unit (X-direction moving motor) 12, and the driving unit (X-direction moving motor) 12 is disposed on the opposite side of the cutting edge 2 across the main body portion 10. The X-direction moving motor 12 is disposed on the main body support portion 30 via a support table 14. The main body portion 10 is disposed on the X-direction guide shaft 17 on the main body support portion 30 via an X-direction sliding member 16 so as to be movable in the X direction on the main body support portion 30. The X-direction moving motor 12 moves the main body portion 10 and the X-direction sliding member 16 in the X direction by an X-direction lead screw 13. An X-direction displacement gauge 15 is disposed on the X-direction guide shaft 17, and the X-direction displacement gauge 15 is used to measure the X-direction displacement (X-direction moving distance) of the cutting edge 2. As the X-direction displacement gauge 15, for example, a laser displacement gauge, a micrometer, etc. are used.

[0039] The cutting edge 2 can move in the Z direction (the direction perpendicular to the surface of the specimen 3) together with the cutting-edge support portion 11 by a driving unit (Z-direction moving motor) 18 disposed above the cutting-edge support portion 11. The Z-direction moving motor 18 is supported on the main body portion 10 via a connecting portion 19. The Z-direction moving motor 18 moves a nut 21 provided on the side surface of the main body portion 10 in the Z direction by a Z-direction lead screw 20, and the nut 21 moves the cutting edge 2 and the cutting-edge support portion 11 in the Z direction. A Z-direction displacement gauge 22 is disposed on the main body portion 10, and the Z-direction displacement gauge 22 is used to measure the Z-direction displacement of the nut 21, that is, the Z-direction displacement (Z-direction moving distance) of the cutting edge 2. As the Z-direction displacement gauge 22, for example, a contact displacement gauge such as a scale type, a micrometer, etc. are used. The nut 21 is disposed on the Z-direction guide shaft 23 on the side surface of the main body portion 10 via a Z-direction sliding member 24 so as to be movable in the Z direction on the side surface of the main body portion 10. A Z-direction pressure detector 25 is disposed on the cutting-edge support portion 11, and the Z-direction pressure detector 25 is used to measure the pressure (Z-direction pressure) applied to the specimen 3 from the cutting edge 2 in the Z direction.

[0040] The specimen stage 4 is provided on the main body support portion 30. Between the specimen stage 4 and the main body support portion 30, there are, in order from above, a slide member 26 for X-direction pressure detection, a guide shaft 35 for X-direction pressure detection, an X-direction tilt adjustment unit 36, a Y-direction tilt adjustment unit 37, an XY-direction position adjustment member 38, a slide member 27 for Y-direction, and a guide shaft 28 for Y-direction. In addition, the slide member 26 for X-direction pressure detection is a member for transmitting the load applied from the cutting edge 2 during cutting to the X-direction pressure detector 29, and slides along the guide shaft 35 for X-direction pressure detection according to the load applied from the cutting edge 2. The X-direction tilt adjustment unit 36 is a member for rotating the specimen fixing surface of the specimen stage 4 in the X direction (the rotation axis extends along the Y direction). Specifically, a micrometer can be used as the X-direction tilt adjustment unit 36. The Y-direction tilt adjustment unit 37 is a member for rotating the specimen fixing surface of the specimen stage 4 in the Y direction (the rotation axis extends along the X direction). Specifically, a micrometer can be used as the Y-direction tilt adjustment unit 37. The XY-direction position adjustment member 38 is a member for manually moving the specimen stage 4 before the start of automatic cutting to arrange the specimen stage 4 at the cutting start position. The specimen stage 4 is provided on the guide shaft 28 for Y-direction on the main body support portion 30 in such a manner that it can move along the Y direction on the main body support portion 30 together with the slide member 26 for X-direction pressure detection, the guide shaft 35 for X-direction pressure detection, the X-direction tilt adjustment unit 36, the Y-direction tilt adjustment unit 37, and the XY-direction position adjustment member 38, with the slide member 27 for Y-direction interposed therebetween. An X-direction pressure detector 29 is provided on the guide shaft 35 for X-direction pressure detection, and this X-direction pressure detector 29 is for measuring the pressure (X-direction pressure) applied to the specimen 3 from the cutting edge 2 in the X direction.

[0041] The specimen stage 4 can move in the Y direction by a drive unit (Y-direction moving motor) 31 disposed on one side in the Y direction of the slide member 27 for Y-direction. The Y-direction moving motor 31 moves the specimen stage 4 and the slide member 27 for Y-direction together in the Y direction through a Y-direction lead screw 32.

[0042] In the specimen analysis device 1 of the present embodiment, the operations of the X-direction moving motor 12, the Z-direction moving motor 18, and the Y-direction moving motor 31 are automatically controlled, for example, by a control unit 40 including a computer such as a personal computer. The control unit 40 reads in the information detected by the X-direction displacement meter 15, the X-direction pressure detector 29, the Z-direction displacement meter 22, and the Z-direction pressure detector 25 through an input interface 41, and based on this information, controls the operations of the X-direction moving motor 12 and the Z-direction moving motor 18 through a first output interface 42, and controls the operation of the Y-direction moving motor 31 through a second output interface 43.

[0043] Regarding the Y-direction displacement (Y-direction movement distance) of the cutting edge 2, the control unit 40 can use the drive command sent to the Y-direction movement motor 31, i.e., the movement distance, or alternatively, a Y-direction displacement gauge for measuring the Y-direction movement distance can be provided and the information detected by this displacement gauge can be used. Additionally, regarding the X-direction displacement (X-direction movement distance) of the cutting edge 2, the control unit 40 can also use the drive command sent to the X-direction movement motor 12, i.e., the movement distance, instead of the information detected by the X-direction displacement gauge 15; regarding the Z-direction displacement (Z-direction movement distance) of the cutting edge 2, the control unit 40 can also use the drive command sent to the Z-direction movement motor 18, i.e., the movement distance, instead of the information detected by the Z-direction displacement gauge 22. However, when cutting the specimen 3, due to the reaction force received by the cutting edge 2 from the specimen 3 and the like, there may be a deviation in the movement distance. Therefore, in order to cut the specimen 3 with high precision, regarding the X-direction movement distance and the Z-direction movement distance, it is preferable to perform cutting while precisely monitoring the actual movement distance by means of a displacement gauge.

[0044] In the control unit 40, each function is implemented by a computer executing a program. The computer includes a processor that operates according to the program, a memory that stores data required for executing the program, etc. as the main hardware components. Regarding the processor, as long as it can implement the functions by executing the program, its type is not limited. For example, it can also be composed of one or more electronic circuits including a semiconductor integrated circuit (IC, Integrated Circuit) or a large-scale integrated circuit (LSI, Large Scale Integration). The program and data are recorded in a non-temporary recording medium such as a computer-readable read-only memory (ROM, Read-Only Memory), an optical disc, or a hard disk drive. The program and data can be pre-stored in the recording medium or supplied to the recording medium via a wide area network including the Internet, etc.

[0045] The first instruction, the second instruction, the third instruction, and the fourth instruction are programmed in the control unit 40. The first instruction causes the first Z-direction cutting process to be performed. In this first Z-direction cutting process, the cutting edge 2 is relatively moved downward in the Z direction or downward in the Z direction and forward in the X direction with respect to the specimen stage 4, thereby cutting starting from the surface of the specimen 3. The second instruction causes the first X-direction cutting process to be performed immediately after the first Z-direction cutting process. In this first X-direction cutting process, while cutting the specimen 3 by relatively moving the cutting edge 2 forward in the X direction with respect to the specimen stage 4, the load in the X direction applied to the cutting edge 2 is measured. The third instruction causes the second Z-direction cutting process to be performed at least once after the first X-direction cutting process. In this second Z-direction cutting process, the specimen 3 is cut by relatively moving the cutting edge 2 downward in the Z direction or downward in the Z direction and forward in the X direction with respect to the specimen stage 4. The fourth instruction causes the second X-direction cutting process to be performed at least once immediately after the second Z-direction cutting process. In this second X-direction cutting process, while cutting the specimen 3 by relatively moving the cutting edge 2 forward in the X direction with respect to the specimen stage 4, the load in the X direction applied to the cutting edge 2 is measured.

[0046] It should be noted that the third instruction includes the following instruction. Under this instruction, in the first second Z-direction cutting process, the specimen 3 is cut until a position lower in the Z direction closer to the cutting position of the first X-direction cutting process. In the second and subsequent second Z-direction cutting processes, the specimen 3 is cut until a position lower in the Z direction closer to the cutting position of the immediately preceding second X-direction cutting process.

[0047] The specimen analysis device 1 of the present embodiment analyzes the internal state of the specimen 3. Specifically, in the specimen analysis device 1 shown in Figure 1 and Figure 2 , the control unit 40 includes an analysis unit. This analysis unit analyzes the internal state of the specimen 3 based on the load in the X direction measured in the first X-direction cutting process and the second X-direction cutting process. However, it is not limited to this, and an analysis unit may be separately provided separately from the control unit 40. For example, the analysis unit may be constituted by another computer connected to the control unit 40 via a network. The specimen analysis device 1 other than the analysis unit is a cutting device for cutting the specimen 3.

[0048] In addition, in Figure 1 and Figure 2In the sample analysis apparatus 1 shown, as the drive unit for relatively moving the cutting edge 2 and the sample stage 4, an X-direction moving motor 12 for moving the cutting edge 2 in the X direction, a Z-direction moving motor 18 for moving the cutting edge 2 in the Z direction, and a Y-direction moving motor 31 for moving the sample stage 4 in the Y direction are used. However, as long as the cutting edge 2 and the sample stage 4 can relatively move in at least the three axial directions of the X direction, Y direction, and Z direction, either the cutting edge 2 or the sample stage 4 can move.

[0049] <Sample Analysis Method>

[0050] Next, an explanation will be given of the sample analysis method of the present embodiment using the Figure 1 and Figure 2 sample analysis apparatus 1 shown.

[0051] In the sample analysis method of the present embodiment, first, a step (A) of fixing the sample 3 to the sample stage 4 is performed. For example, the sample stage 4 is composed of a box-shaped body having a sample attracting portion (attracting hole) on the upper surface for placing the sample 3, and an attracting tube (not shown) is connected to the side portion of the box-shaped body, and the attracting tube can also be connected to a vacuum pump (not shown). Therefore, by operating the vacuum pump, the sample 3 can be attracted downward on the sample stage 4, and thus the sample 3 can be fixed to the sample stage 4. Instead of the fixing method described above, the sample 3 can also be fixed to the sample stage 4 by a chemical fixing method using an adhesive, a hot melt adhesive, etc., or a physical fixing method using bolts, etc. However, from the viewpoints of fixing accuracy and ease of operation, the above-described attracting and fixing method is preferred.

[0052] Next, a step (B) of measuring the inclination of the surface of the sample 3 is performed. The step (B) can be implemented by using, for example, a indenter in contact with the surface of the sample 3, a Z-direction displacement meter 22 and a Z-direction pressure detector 25 in the sample analysis apparatus 1 as the inclination measurement unit. Specifically, the indenter is installed on the cutting edge support portion 11 instead of the cutting edge 2, while bringing the indenter into contact with the sample 3, the indenter is moved in a state where a certain load is applied using the Z-direction pressure detector 25, and the displacement of the indenter is continuously detected using the Z-direction displacement meter 22. Thereby, the height information of the surface of the sample 3 can be obtained, and thus the inclination of the surface of the sample 3 can be measured. In addition, at a plurality of positions on the surface of the sample 3, the indenter can be pressed against the surface of the sample 3 to a certain height position using the Z-direction displacement meter 22, and the load received by the indenter at this time can be detected by the Z-direction pressure detector 25. Thereby, the loads received at a certain height position can be compared at a plurality of points, and thus the inclination of the surface of the sample 3 can be measured.

[0053] It should be noted that when performing tilt measurement, it is preferable to move the indenter at least in two directions, namely the X direction and the Y direction, for tilt measurement. To further improve the tilt measurement accuracy, it is more preferable to move the indenter in three directions, namely the X direction, the Y direction, and the tilt direction (for example, a direction intersecting the X direction at 45°), for tilt measurement. The tip shape of the indenter for tilt measurement preferably has a curved surface so as not to damage the specimen 3 when the indenter contacts the specimen 3. To further improve the tilt measurement accuracy, the tip shape of the indenter is more preferably spherical.

[0054] Next, a process (C) of adjusting the tilt of the surface of the specimen 3 is performed. For example, a micrometer (i.e., the X-direction tilt adjustment unit 36) that rotates the specimen fixing surface of the specimen stage 4 in the X direction (the rotation axis extends along the Y direction) and a micrometer (i.e., the Y-direction tilt adjustment unit 37) that rotates the specimen fixing surface of the specimen stage 4 in the Y direction (the rotation axis extends along the X direction) can be used to adjust the angle of the specimen 3. Alternatively, an actuator or other tilt adjustment unit can be used instead of the micrometer. After performing the process (C), the tilt measurement of the process (B) can be performed again to confirm that the surface of the specimen 3 is close to horizontal.

[0055] After performing the above processes (A), (B), and (C), a cutting operation (the first Z-direction cutting process, the first X-direction cutting process, the second Z-direction cutting process, and the second X-direction cutting process) by the cutting edge 2 of the specimen analysis device 1 (cutting device) is started. When starting the cutting operation, the operator can also preset various cutting conditions such as the number of cutting times to the control unit 40, so as to automatically perform the cutting operation.

[0056] As the cutting conditions, the range of the three-dimensional region to be analyzed in the specimen 3 can be set, for example, to 5 μm to 1000 μm in the Z direction and 500 μm to 20000 μm in the X direction. The range in the Y direction can also be set to 0.05 mm to 4.0 mm according to the width of the cutting edge 2.

[0057] As conditions for the first Z-direction cutting process and the second Z-direction cutting process, for example, the +Z-direction cutting distance can be set to 1 μm to 100 μm, and the +Z-direction cutting speed can be set to 0.1 μm / s to 50 μm / s. Since the +Z-direction cutting distance is the difference between the measurement depth of the previous X-direction load and the measurement depth of the subsequent X-direction load, if the +Z-direction cutting distance is reduced, the analysis accuracy becomes higher. On the other hand, if the +Z-direction cutting distance is increased, the measurement time becomes shorter. Therefore, the +Z-direction cutting distance can be set considering the balance between the two. The +Z-direction cutting distance can also be different in each Z-direction cutting process. For example, after initially increasing the +Z-direction cutting distance for cutting, the +Z-direction cutting distance can be reduced to perform a detailed analysis of a specified Z-direction range. In addition, when cutting in the +Z direction and the +X direction in the first Z-direction cutting process and the second Z-direction cutting process, for example, the +X-direction cutting distance can be set to 500 μm to 20,000 μm, and the +X-direction cutting speed can be set to 1 μm / s to 1000 μm / s.

[0058] As conditions for the first X-direction cutting process and the second X-direction cutting process, for example, the +X-direction cutting distance can be set to 500 μm to 20,000 μm, and the +X-direction cutting speed can be set to 1 μm / s to 1000 μm / s. Here, based on the setting of the +X-direction cutting distance in the first X-direction cutting process and the second X-direction cutting process, the setting in the X direction of the "range of the three-dimensional region to be analyzed in Specimen 3" described above is performed.

[0059] It is also possible to select a load cell for measuring the load in the X direction applied to the cutting edge 2 in the first X-direction cutting process and the second X-direction cutting process according to the measured load (horizontal load Fh). For example, if the horizontal load Fh is 0.1 N or less, a load cell with a rated capacity of 5 N can be selected. If the horizontal load Fh exceeds 0.1 N and is less than 20 N, a load cell with a rated capacity of 20 N can be selected. If the horizontal load Fh is 20 N or more, a load cell with a rated capacity of 100 N can be selected. Since the smaller the rated capacity of the load cell, the better the resolution of the load cell, for general specimen analysis, a load cell with a rated capacity of 20 N can be selected. For the analysis of electrodes of lithium-ion batteries, etc., a load cell with a rated capacity of 5 N can be selected. For the analysis of metals, a load cell with a rated capacity of 100 N can be selected.

[0060] [First Z-direction cutting process]

[0061] In the first Z-direction cutting process, the control unit 40 drives the X-direction movement motor 12 and the Z-direction movement motor 18 to move the cutting edge 2 in the +Z direction (the downward direction in the Z direction) or in the +Z direction and the +X direction (the forward direction in the X direction), thereby starting cutting from the surface of the specimen 3.

[0062] Specifically, at the stage when the specimen stage 4 on which the specimen 3 is fixed is arranged at the cutting start position, the cutting edge 2 is separated from the specimen 3 in the Z direction. Therefore, first, the control unit 40 drives the Z-direction movement motor 18 to move the cutting edge 2 in the downward direction in the Z direction so that the cutting edge 2 contacts the cutting start position on the surface of the specimen 3. This contact operation can also be manually performed by providing, for example, a unit that allows the cutting edge 2 to move arbitrarily in the Z direction. In addition, regarding the confirmation of the contact between the specimen 3 and the cutting edge 2, for example, the Z-direction pressure detector 25 can be used to confirm the contact between the specimen 3 and the cutting edge 2, or the specimen 3 and the cutting edge 2 can be photographed with a camera or the like and magnified and displayed on a personal computer or the like, and the operator can visually confirm the distance between the specimen 3 and the cutting edge 2 while performing the contact confirmation between the specimen 3 and the cutting edge 2.

[0063] Next, the control unit 40 drives the X-direction movement motor 12 and the Z-direction movement motor 18 to move the cutting edge 2 in the +Z direction (or the +Z direction and the +X direction) until the cutting edge 2 reaches the set position (+Z-direction cutting distance and +X-direction cutting distance). At this time, the X-direction pressure detector 29 and the Z-direction pressure detector 25 can also be used to detect the X-direction pressure and the Z-direction pressure of the cutting edge 2. In this way, since the cutting condition can be monitored, it is possible to know whether the cutting condition deviates from the set value of the cutting operation due to the influence caused by the hardness of the specimen 3 or the like. In the case of a non-negligible deviation, the cutting operation can also be interrupted and the processes (B) and (C) can be performed again.

[0064] [First X-direction cutting process]

[0065] After the first Z-direction cutting process is performed, immediately in the first X-direction cutting process, while the control unit 40 only drives the X-direction moving motor 12 to move the cutting edge 2 in the +X direction until the cutting edge 2 reaches the set position (+X-direction cutting distance), thereby cutting the specimen 3, the load applied to the cutting edge 2 in the X direction is measured. An X-direction pressure detector 29 can also be used for measuring the load in the X direction. At this time, although the cutting operation is performed without displacing the cutting edge 2 in the Z direction, a tilt of within ±2°, preferably within ±1° in the Z direction, of the cutting direction with respect to the X direction caused by, for example, the tilt of the surface of the specimen 3 or the moving accuracy of the cutting edge 2 is allowed. It should be noted that in the first X-direction cutting process, it is not necessary to cut to the +X-direction end of the specimen 3.

[0066] In the present embodiment, after the first X-direction cutting process, the control unit 40 may drive the Z-direction moving motor 18 to move the cutting edge 2 in the -Z direction (the upward direction in the Z direction). In this way, when the first X-direction cutting process ends and the cutting edge 2 is moved in the -X direction (the backward direction in the X direction) to the start position of the second Z-direction cutting process described later, contact between the cutting edge 2 and the cutting surface of the specimen 3 formed in the first X-direction cutting process can be prevented. At this time, it may also be that the control unit 40 drives the X-direction moving motor 12 and the Z-direction moving motor 18 together to move the cutting edge 2 in the -Z direction and the +X direction, thereby cutting a slice from the specimen 3.

[0067] Next, the control unit 40 drives the X-direction moving motor 12 to move the cutting edge 2 in the -X direction until the cutting edge 2 returns to the start position of the second Z-direction cutting process. Here, in order to shorten the cutting time, the moving speed of the cutting edge 2 in the -X direction (return speed) may be made greater than the moving speed of the cutting edge 2 in the first X-direction cutting process (+X-direction cutting speed). In addition, when the cutting edge 2 returns to the start position of the second Z-direction cutting process, the return moving speed may be reduced immediately before this start position, that is, immediately before the stop position of the cutting edge 2. In this way, displacement of the cutting edge 2 caused by suddenly stopping the cutting edge 2 from the state of moving in the -X direction at high speed can be prevented.

[0068] [Second Z-direction cutting process]

[0069] In the second Z-direction cutting process, the control unit 40 drives the X-direction movement motor 12 and the Z-direction movement motor 18 to move the cutting edge 2 in the +Z direction, or in the +Z direction and the +X direction, until the cutting edge 2 reaches the set position (+Z-direction cutting distance and +X-direction cutting distance), thereby cutting the specimen 3. At this time, the X-direction pressure detector 29 and the Z-direction pressure detector 25 can also be used to detect the X-direction pressure and the Z-direction pressure of the cutting edge 2. In this way, since the cutting condition can be monitored, it is possible to know whether the cutting condition deviates from the set value of the cutting operation due to the influence caused by the hardness of the specimen 3 or the like. In the case where an unignorable deviation occurs, the cutting operation can also be interrupted and the processes (B) and (C) can be performed again.

[0070] It should be noted that in the case where the cutting edge 2 and the specimen 3 are in a separated state in the Z direction at the start time of the second Z-direction cutting process, the control unit 40 needs to drive the Z-direction movement motor 18 to move the cutting edge 2 in the +Z direction so that the cutting edge 2 contacts the specimen 3. This contact operation can also be manually performed by providing, for example, a unit that allows the cutting edge 2 to move arbitrarily in the Z direction. In addition, regarding the confirmation of the contact between the specimen 3 and the cutting edge 2, for example, the Z-direction pressure detector 25 can be used to confirm the contact between the specimen 3 and the cutting edge 2, or the specimen 3 and the cutting edge 2 can be photographed with a camera or the like and enlarged and displayed on a personal computer or the like, and the operator can visually confirm the distance between the specimen 3 and the cutting edge 2 while performing the contact confirmation between the specimen 3 and the cutting edge 2.

[0071] [Second X-direction cutting process]

[0072] After the second Z-direction cutting process is implemented, immediately in the second X-direction cutting process, while the control unit 40 only drives the X-direction movement motor 12 to move the cutting edge 2 in the +X direction until the cutting edge 2 reaches the set position (+X-direction cutting distance), thereby cutting the specimen 3, the load applied to the cutting edge 2 in the X direction is measured. The X-direction pressure detector 29 can also be used for the measurement of the load in the X direction. At this time, although the cutting operation is performed without displacing the cutting edge 2 in the Z direction, a tilt of the cutting direction with respect to the X direction within ±2°, preferably within ±1° in the Z direction, caused by the tilt of the surface of the specimen 3 or the movement accuracy of the cutting edge 2 is allowed. It should be noted that in the second X-direction cutting process, it is not necessary to cut to the +X-direction end of the specimen 3.

[0073] In the present embodiment, after the second X-direction cutting process, the control unit 40 may drive the Z-direction moving motor 18 to move the cutting edge 2 in the -Z direction (the upward direction in the Z direction). In this way, when the second X-direction cutting process ends and the cutting edge 2 is moved in the -X direction to the start position of the next second Z-direction cutting process, it is possible to prevent the cutting edge 2 from contacting the cutting surface of the specimen 3 formed in the second X-direction cutting process. At this time, it may also be that the control unit 40 drives the X-direction moving motor 12 and the Z-direction moving motor 18 together to move the cutting edge 2 in the -Z direction and the +X direction, thereby cutting a slice from the specimen 3.

[0074] Next, the control unit 40 drives the X-direction moving motor 12 to move the cutting edge 2 in the -X direction until the cutting edge 2 returns to the start position of the next second Z-direction cutting process. Here, in order to shorten the cutting time, the moving speed (-X direction moving speed) of the cutting edge 2 during the return may be made greater than the moving speed (+X direction cutting speed) of the cutting edge 2 during the second X-direction cutting process. In addition, when the cutting edge 2 returns to the start position of the next second Z-direction cutting process, the return moving speed may be reduced immediately before the start position, that is, immediately before the stop position of the cutting edge 2. In this way, it is possible to prevent the positional deviation of the cutting edge 2 that occurs when the cutting edge 2 is suddenly stopped from the state of moving in the -X direction at high speed.

[0075] Perform a combined process of the second Z-direction cutting process and the second X-direction cutting process one or more than two times. The number of times of performing the second Z-direction cutting process and the second X-direction cutting process is set according to the type of the specimen 3. For example, in the case of a battery electrode, it may be performed two to three times.

[0076] In the case of performing a second Z-direction cutting process once, the second Z-direction cutting process can be started from the cutting surface of the first Z-direction cutting process or the first X-direction cutting process; in the case of performing the second Z-direction cutting process two or more times, the later-performed second Z-direction cutting process can be started from the cutting surface of the immediately preceding second Z-direction cutting process or the second X-direction cutting process. In other words, the first second Z-direction cutting process is started from the cutting surface of the first Z-direction cutting process or the first X-direction cutting process, and the second and subsequent second Z-direction cutting processes are started from the cutting surface of the immediately preceding second Z-direction cutting process or the second X-direction cutting process. In this way, compared with the case where cutting is started from the sample surface in each second Z-direction cutting process, the cutting distance is shortened, so that the time required for analysis can be significantly reduced. It should be noted that the cutting surfaces of the first Z-direction cutting process and the second Z-direction cutting process refer to the cutting surfaces (inclined surfaces) formed when the cutting edge 2 is moved in the +Z direction and the +X direction to cut the sample 3 in the first Z-direction cutting process and the second Z-direction cutting process.

[0077] In each of the first X-direction cutting process and the second X-direction cutting process, the cutting ranges in the X direction and the Y direction may also include the same area. In this way, the state of a specific three-dimensional area inside the sample 3 can be analyzed with high precision using the load measurement value in the X direction.

[0078] [Analysis process]

[0079] After the cutting operations (the first Z-direction cutting process, the first X-direction cutting process, the second Z-direction cutting process, and the second X-direction cutting process) performed by the cutting edge 2 of the sample analysis device 1 (cutting device) are completed, an analysis process is performed. In this analysis process, the internal state of the sample 3 is analyzed based on the loads in the X direction measured in the first X-direction cutting process and the second X-direction cutting process. By comparing the loads in the X direction (horizontal loads) applied to the cutting edge 2 at different depths (Z-direction positions) in the sample 3, the uniformity inside the sample 3 can be evaluated, and the Z-direction layer state of the sample 3, such as the degree of adhesion, etc., can be evaluated based on the absolute value of the horizontal load. Therefore, analysis of, for example, electrodes of lithium-ion batteries, all-solid-state batteries, etc., specifically, the active material layer on the electrodes, can be performed. It should be noted that the active material of the all-solid-state battery deteriorates due to moisture in the air, so load measurement is performed in an inert atmosphere such as a glove box.

[0080] The analysis process may also include a first analysis process and a second analysis process. In the first analysis process, the average value of the loads in the X direction measured in the same specific interval in the X direction in the first X-direction cutting process and the second X-direction cutting process is obtained. In the second analysis process, the internal state of the specimen 3 is analyzed by comparing the average values of the loads in the X direction obtained in the first analysis process with each other. The specific interval can be preset before the cutting starts, or the range with small fluctuations in the load in the X direction (horizontal load) can be set as the specific interval after the load measurement ends. When setting the specific interval after the load measurement ends, the specific interval can also be defined based on the result of plotting the horizontal load against the measurement time or the moving distance.

[0081] <Analysis Example>

[0082] Next, Figures 4 to 6 An example of the specimen analysis method using the specimen analysis apparatus 1 of the present embodiment will be described.

[0083] As Figure 4 shown, in this example, after performing the first Z-direction cutting process and the first X-direction cutting process, a combined process of performing the second Z-direction cutting process and the second X-direction cutting process three times is performed. In Figure 4 , "the first time" represents the first Z-direction cutting process, "the second time" represents the first second Z-direction cutting process, "the third time" represents the second second Z-direction cutting process, and "the fourth time" represents the third second Z-direction cutting process. In the first Z-direction cutting process and the second Z-direction cutting process, the cutting edge 2 is moved an equal distance (feed amount) in the +Z direction each time. In the third second Z-direction cutting process, the cutting edge 2 reaches the final reaching depth of the specimen 3. The first second Z-direction cutting process is performed starting from the cutting surface of the first X-direction cutting process, the second second Z-direction cutting process is performed starting from the cutting surface of the first second X-direction cutting process, and the third second Z-direction cutting process is performed starting from the cutting surface of the second second X-direction cutting process.

[0084] As Figure 4 and Figure 5 shown, in this example, in the first X-direction cutting process and the second X-direction cutting process, the cutting ranges in the X direction and the Y direction include the same area (specific area) R.

[0085] Figure 6 Shows the load in the X direction (horizontal load Fh) measured in the specimen analysis method shown in Figure 4 . In Figure 6In this case, "the first time" represents the change of the horizontal load Fh measured in the first cutting process in the X direction with respect to the measurement time, "the second time" represents the change of the horizontal load Fh measured in the second cutting process in the X direction for the first time with respect to the measurement time, "the third time" represents the change of the horizontal load Fh measured in the second cutting process in the X direction for the second time with respect to the measurement time, and "the fourth time" represents the change of the horizontal load Fh measured in the second cutting process in the X direction for the third time with respect to the measurement time.

[0086] In this example, based on Figure 6 the results shown, a specific interval R is set, and the average value of the horizontal load Fh measured in the specific interval R in the first cutting process in the X direction and the second cutting process in the X direction is obtained. By comparing these average values with each other, the internal state of Specimen 3 is analyzed.

[0087] <Features of the Embodiment>

[0088] As described above, according to the specimen analysis method of the present embodiment, in the first cutting process in the X direction and the second cutting process in the X direction, while cutting by moving the cutting edge 2 relative to the specimen 3 in the X direction, the load in the X direction applied to the cutting edge 2 is measured. Therefore, the load in the X direction at different depths (Z-direction positions) in the specimen 3 can be obtained with high precision. Therefore, the internal state of the specimen 3 can be analyzed three-dimensionally and with high precision using the measured values of the load in the X direction.

[0089] In the specimen analysis method of the present embodiment, in each of the first cutting process in the X direction and the above-mentioned second cutting process in the X direction, the cutting ranges in the X direction and the Y direction may also include the same area. In this way, the state of a specific three-dimensional area inside the specimen 3 can be analyzed with high precision using the measured values of the load in the X direction.

[0090] In the specimen analysis method of the present embodiment, in the case of performing the second cutting process in the Z direction once, the second cutting process in the Z direction may also start from the cutting surface of the first cutting process in the Z direction or the first cutting process in the X direction; in the case of performing the second cutting process in the Z direction two or more times, the second cutting process in the Z direction performed later may also start from the cutting surface of the immediately preceding second cutting process in the Z direction or the second cutting process in the X direction. In this way, compared with the case of starting cutting from the surface of the specimen 3 in each second cutting process in the Z direction, the cutting distance is shorter, so the time required for analysis can be significantly shortened.

[0091] In the sample analysis method of the present embodiment, the analysis process may also include a first analysis process and a second analysis process. In the first analysis process, an average value of the loads in the X direction measured in the same specific interval in the X direction in the first X-direction cutting process and the second X-direction cutting process is obtained. In the second analysis process, the internal state of the sample 3 is analyzed by comparing the average values of the loads in the X direction obtained in the first analysis process with each other. In this way, the internal state of the sample 3 can be analyzed with higher precision using the average values of the loads in the X direction at different depths (Z-direction positions) in the sample 3.

[0092] In the sample analysis method of the present embodiment, the sample 3 may also be an electrode for a battery. In this way, the internal state of the electrode for a battery can be analyzed three-dimensionally and with high precision.

[0093] According to the sample analysis device 1 of the present embodiment, while cutting by moving the cutting edge 2 relative to the sample 3 in the X direction in the first X-direction cutting process and the second X-direction cutting process, the load in the X direction applied to the cutting edge 2 is measured. Therefore, the loads in the X direction at different depths (Z-direction positions) in the sample 3 can be obtained with high precision. Therefore, the internal state of the sample 3 can be analyzed three-dimensionally and with high precision using the measured values of the loads in the X direction.

[0094] (Other embodiments)

[0095] The embodiments have been described above. However, it should be understood that various changes can be made to the manner and specific circumstances without departing from the gist and scope of the claims. In addition, as long as the functions of the objects of the present disclosure are not affected, the above embodiments can be appropriately combined or replaced. Furthermore, the terms such as "first", "second",... used above are used to distinguish the phrases using these terms, and do not limit the quantity and order of these phrases.

Claims

1. A sample analysis method for analyzing the internal state of a sample using a cutting device, characterized in that: The cutting device comprises a cutting edge, a sample table and a driving unit. The sample stand fixes the sample. The driving unit causes the cutting edge and the sample stage to move relative to each other. The cutting edge and the sample stage can be relatively moved in the X direction, the Y direction and the Z direction respectively, the X direction and the Y direction are parallel to the surface of the sample and are orthogonal to each other, and the Z direction is perpendicular to the surface of the sample, The sample analysis method comprises a first Z-direction cutting step, a first X-direction cutting step, a second Z-direction cutting step and a second X-direction cutting step. In the first Z-direction cutting step, the cutting edge is relatively moved relative to the sample stage in a downward direction in the Z direction, or in a downward direction in the Z direction and in a forward direction in the X direction, thereby starting cutting from the surface of the sample. After the first Z-direction cutting step, in the first X-direction cutting step, the sample is cut by relatively moving the cutting edge in the forward direction in the X-direction relative to the sample stage, while measuring the load in the X-direction applied to the cutting edge, After the first X-direction cutting step, in the second Z-direction cutting step, the sample is cut by relatively moving the cutting edge in the downward direction in the Z-direction or in the downward direction in the Z-direction and in the forward direction in the X-direction relative to the sample stage. After the second Z-direction cutting step, in the second X-direction cutting step, the sample is cut by relatively moving the cutting edge in the forward direction in the X-direction relative to the sample stage, while measuring the load in the X-direction applied to the cutting edge, The second Z-direction cutting step and the second X-direction cutting step are performed at least once respectively, In the first second Z-direction cutting step, the sample is cut until the cutting edge reaches a position lower in the Z-direction than the cutting position in the first X-direction cutting step. In the second Z-direction cutting step performed for the second time or later, the sample is cut to a position lower in the Z-direction than the cutting position in the second X-direction cutting step performed immediately before. The sample analysis method further includes an analysis step of analyzing an internal state of the sample based on the load in the X direction measured in the first X direction cutting step and the second X direction cutting step.

2. The sample analysis method according to claim 1, characterized in that: In each of the first X-direction cutting step and the second X-direction cutting step, the cutting ranges in the X-direction and the Y-direction include the same region.

3. The sample analysis method according to claim 1 or 2, characterized in that: When the second Z-direction cutting step is performed once, the second Z-direction cutting step is performed starting from the cutting surface of the first Z-direction cutting step or the first X-direction cutting step. When the second Z-direction cutting step is performed two or more times, the second Z-direction cutting step performed later is performed from the cutting surface of the second Z-direction cutting step or the second X-direction cutting step performed immediately before.

4. The sample analysis method according to claim 1 or 2, characterized in that: The analysis process includes a first analysis process and a second analysis process. In the first analysis step, an average value of the load in the X direction measured in the same specific section in the X direction in the first X direction cutting step and the second X direction cutting step is obtained. In the second analysis step, the internal state of the sample is analyzed by comparing the average values ​​of the load in the X direction obtained in the first analysis step.

5. The sample analysis method according to claim 1 or 2, characterized in that: The sample is a battery electrode.

6. A sample analysis device for analyzing the internal state of a sample, characterized in that: The sample analysis device includes a cutting edge, a sample stage, a driving unit, a control unit, and an analysis unit. The sample stand fixes the sample. The driving unit causes the cutting edge and the sample stage to move relative to each other. The control unit controls the driving of the driving unit. The analyzing unit analyzes the internal state of the sample, The cutting edge and the sample stage can be relatively moved in the X direction, the Y direction and the Z direction respectively, the X direction and the Y direction are parallel to the surface of the sample and are orthogonal to each other, and the Z direction is perpendicular to the surface of the sample, The control unit includes a first instruction, a second instruction, a third instruction, and a fourth instruction. The first instruction causes a first Z-direction cutting process to be implemented, in which the cutting edge is relatively moved relative to the sample stage in a downward direction in the Z direction, or in a downward direction in the Z direction and in a forward direction in the X direction, thereby starting cutting from the surface of the sample. The second instruction causes a first X-direction cutting step to be performed immediately after the first Z-direction cutting step, wherein in the first X-direction cutting step, the sample is cut by relatively moving the cutting edge in the forward direction in the X-direction relative to the sample stage, while measuring a load in the X-direction applied to the cutting edge, The third instruction causes a second Z-direction cutting process to be performed at least once after the first X-direction cutting process, and in the second Z-direction cutting process, the sample is cut by relatively moving the cutting edge in a downward direction in the Z direction or in a downward direction in the Z direction and in a forward direction in the X direction relative to the sample stage, The fourth instruction causes a second X-direction cutting step to be performed at least once immediately after the second Z-direction cutting step, wherein in the second X-direction cutting step, the sample is cut by relatively moving the cutting edge in the forward direction in the X-direction relative to the sample stage, while measuring the load in the X-direction applied to the cutting edge, The third instruction includes the following instruction, under which, in the first second Z-direction cutting step, the sample is cut to a position closer to the lower side in the Z direction than the cutting position in the first X-direction cutting step, and in the second Z-direction cutting step after the second time, the sample is cut to a position closer to the lower side in the Z direction than the cutting position in the second X-direction cutting step immediately before. The analysis unit analyzes an internal state of the sample based on the load in the X direction measured in the first X direction cutting step and the second X direction cutting step.

Images