JP2011080869A - Mesh and method for observation of test piece - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a mesh for accurate and highly reproducible observation of a test piece in a drawing process and further a test piece through the drawing process to a contraction process, and a method of observation of a test piece using the mesh. <P>SOLUTION: The method of observation of a test piece includes: a process of mounting and fixing the test piece onto a mesh; a process of fixing the mesh to a holder for observation; a subsequent process of drawing the test piece fixed to the mounting area of the mesh by moving the holder for observation in the drawing direction; and a process of observing the test piece in the drawing process; wherein after fixing of the test piece to the holder for observation, the mesh is divided in the drawing process. The mesh suitable for the observation method is also provided. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a test piece observation mesh and a test piece observation method, and in particular, enables a precise and reproducible observation of a test piece in a stretching process and a test piece in a contraction process from a stretching process. is there.

Conventionally, when observing a sample with a microscope such as a transmission electron microscope (TEM), the sample is sliced in advance with a cutting device or the like, and then the test piece that is the sliced sample is placed on a sample support material called a mesh. The test piece is observed after fixing and fixing this mesh to a dedicated observation holder.
As shown in FIG. 5 (a), the commercially available mesh 1 that has been conventionally used has a disk shape with a diameter of about 3 mm, and is provided with a mesh-like opening 1d and the like so as to transmit an electron beam. Yes. As shown in FIG.5 (b), the test piece 3 thinned to the center part upper surface of the commercial mesh 1 which has the opening 1d is fixed. Here, the test piece needs to be thinned to a thickness capable of transmitting an electron beam. As conventional test piece thinning methods, a processing method using a microtome device, a processing method using a focused ion beam processing device (FIB processing), and the like are known.

  Japanese Patent Application Laid-Open No. 2008-96161 proposes a mesh having a specially shaped slit process and an observation method using the mesh. As shown in FIG. 6, a special-shaped mesh 1 in which the slit 4 is cut by a required length from the outer edge of the mesh 1 and a special-shaped mesh in which slits 4 a and 4 b for dividing the mesh 1 from the outer edge of the mesh 1 are inserted. A mesh 1 is disclosed.

If the sample is a highly stretchable rubber, resin, plastic, etc., observing the test piece in the drawing process or the test piece from the drawing process to the shrinking process (returning process) It is useful for various analyzes such as deterioration, wear analysis, analysis of hysteresis loss mechanism, and design of blending.
However, since it is almost impossible to stretch a conventional commercial mesh to which a test piece is fixed, there is a problem that a stretched test piece cannot be observed. In addition, even if the conventional commercial mesh is forcibly stretched, the amount of stretching is small, and the commercial mesh is deformed by stretching and strain remains, so the test piece stretched on the commercial mesh remains in its original state. There is a problem that the test piece in the contraction process (return process) cannot be observed.

The technique disclosed in Japanese Patent Application Laid-Open No. 2008-96161 is an excellent technique for observing the stretching process and the shrinking process of a test piece, which was impossible with a commercially available mesh. There is still room for improvement with respect to simple, reliable and reproducible observations.
For example, when slit processing for dividing the mesh before fixing to the observation holder is performed, as described in the above publication [0022] column, etc., the mesh is divided and is difficult to handle, and its handling property is low. Therefore, there is a high possibility that the test piece is damaged when it is fixed to the observation holder. Furthermore, there is a risk that uneven tensile force or compressive force may be locally applied to the test piece fixed to the left and right through the divided slits, such as rattling that is difficult to notice with the naked eye. There is a problem of distortion before observation of the stretching process. For this reason, there exists a problem that observation of an exact origin (drawing zero) cannot be confirmed certainly. On the contrary, when the slit processing is performed to cut the mesh after fixing to the observation holder, the handling of the mesh is improved, but the processing difficulty and skill that cutting of the mesh often fails are required. As well as the problem of losing valuable specimens. Although it depends on the hardness of the mesh, even when processing by pushing the cutting blade or by pulling the cutting blade, even an expert applies locally uneven force due to unforeseeable tearing irregularities, etc. There is a problem that the thinned test piece is distorted before the observation of the stretching process, making it difficult to observe with good reproducibility. This cutting process may be performed by advanced processing methods that are difficult to apply force, such as FIB processing method or ion milling processing method. However, it takes a long time for processing and occupies expensive equipment for a long time. Problems arise.
Further, the special mesh that has been subjected to the slitting process for expansion disclosed in the above publication has a risk of locally applying uneven force to the test piece in the process of stretching or shrinking. For example, as described in the above publication [0043] column and the like, there is a problem that the mesh is twisted or the like during the stretching process without special measures. In addition, as described in the above publication [0042] column and the like, there is a problem that distortion or the like occurs in the test piece during the shrinkage process without designing an appropriate shrinkage rate that requires high skill.
In addition, as described in the above publication [0009] column and the like, there is a problem that a high level of skill is required for setting the widening slit. This is because trial and error for each test piece and a high level of skill are required to determine whether the test piece on the mesh can be extended by extending the mesh in the drawing direction. A high level of skill is required to adjust the required length each time according to the opening shape of the mesh, the shape of the test piece fixed on the mesh, the fixing position of the test piece, and the like.
Furthermore, if there is only one test piece that can be fixed to the mesh, damage due to observation may occur, and in this case, a reliable observation result can be obtained only in the stretching process or only in the contraction process. There is also.

JP 2008-96161 A

  The present invention has been made in view of the above problems, and is a test piece observation method that enables precise and reproducible observation of a test piece in a stretching process, and further a test piece in a contraction process from the stretching process, and the test piece. It is an object to provide a mesh suitable for the observation method.

  In order to solve the above problems, the inventors of the present invention have a specific test piece stretching step, that is, after fixing the test piece to the observation holder, the test piece observation method characterized by dividing the mesh in the drawing process. And the mesh suitable for this observation method was found, and it came to complete this invention.

  That is, the observation method of the test piece of the present invention includes a step of placing and fixing the test piece on the mesh, a step of fixing the mesh to the observation holder, and subsequently moving the observation holder in the extending direction. The test piece is fixed to the observation holder in a test piece observation method including a step of stretching the test piece fixed to the placement region of the mesh and a step of observing the test piece in the stretching process. Thereafter, the method for observing a test piece is characterized in that the mesh is divided in the stretching process.

  Further, following the step of observing the test piece in the stretching process, further, the step of shrinking the test piece fixed to the placement region of the mesh by moving the observation holder in the shrinking direction; A step of observing the test piece in the contraction process, and the method of observing the test piece further includes fixing the test piece to the observation holder without completely dividing the mesh. Desirably, it is more desirable to observe with a microscope, it is even more desirable to divide the mesh within the microscope, and it is particularly desirable to place and fix a plurality of the test pieces on the mesh.

  Furthermore, it is desirable that the mesh is composed of a cross mesh formed by intersecting bone-like columns, and it is more desirable that an outer edge between the left and right connection regions is cut, and in the extension direction, the It is even more desirable that at least one part of the bone-like column holding the test piece is cut and remains.

The mesh for observation of the test piece of the present invention is a test piece in the stretching process, and a mesh that holds the test piece in the contraction process from the stretching process in an observable manner, and the bone shape of the mesh that holds the test piece in the extending direction. The mesh is characterized in that at least a part of the pillar is cut.
In addition, the mesh is fixed to an observation holder whose upper surface at the center is used as a mounting area for fixing the test piece, and both right and left sides sandwiching the mounting area are moved in the extending direction and the contracting direction. When the connection region is moved in the direction of separation by the movement of the observation holder, the test piece whose left and right sides are fixed to the placement region is stretched and / or from the stretched position. When the connection area is moved in the proximity direction by the movement of the observation holder, it is preferable that the test piece is contracted, and the cross-mesh is formed by crossing the bone-like columns. Is more preferable, and it is even more preferable that the outer edge between the left and right connection regions is cut.

  In the observation mesh of the test piece of the present invention, it is preferable that 1 to 10 of the bone-like columns remain, more preferably 1 to 5 remain, More preferably, two remain.

According to the test piece observation method of the present invention, after fixing the test piece to the observation holder, the mesh is divided in the drawing process. It can be ensured and the handling property of the test piece can be improved.
In addition, according to the mesh of the present invention, at least a part of the bone-like column of the mesh that holds the test piece in the extending direction is cut, so that the test piece is attached to the observation holder. After fixing the mesh, it is suitable for an observation method in which the mesh is divided in the stretching process.

By this handling property improvement, in the test piece observation method of the present invention, the order of placing and fixing the test piece on the mesh and the step of connecting and fixing the mesh to the observation holder can be freely changed. Is possible. Even before the mounting and fixing step, the test piece is not distorted, and even when the connection and fixing step is first, the left and right sides of the mesh are integrated, and there is a situation where it is difficult to break apart. Does not occur. On the other hand, in the prior art of Patent Document 1, when the mesh is divided before the mounting and fixing process, the mesh is likely to be separated from side to side, or the test piece may be distorted. A semi-processed commercial mesh is first subjected to a connection and fixing process, and then a special slit process is applied to the mesh, and then a mounting and fixing process is performed. This makes the observation procedure complicated and laborious.
Furthermore, after the start of observation, the test piece can be stretched to an arbitrary stretching ratio without causing distortion or the like to the mesh by simply moving the observation holder in which the right and left sides of the mesh are fixed in the stretching direction. In the stretching process, the mesh is divided so that the mesh is separated and separated from each other, and the test pieces fixed to the left and right meshes are uniformly stretched in the stretching direction by dividing and separating the mesh. It becomes. Therefore, the test piece can be stretched to an arbitrary stretching ratio without deforming the mesh itself by simply moving the observation holder to which the right and left sides of the mesh are fixed in the stretching direction. The state of the test piece at the rate can be observed directly. As a result, it is possible to observe the shape change (morphological change) of the test piece in the stretching process.
Further, when the observation holder is moved in the contraction direction in which the right and left fixing parts are brought close to each other from the stretching process, the meshes divided into the left and right are brought close to each other, and finally the mesh itself remains distorted. It is possible to return to an integrated mesh before division without any problems. Therefore, the test piece can be returned to the state before stretching, and not only the stretching process but also the state of the test piece in the contraction process (returning process) can be observed.
Accuracy and reproducibility are ensured by maintaining the original state before starting observation (zero stretched state) and improving the handleability of the specimen while maintaining good specimen observation in this way. Even in this case, sufficient observation becomes possible.

It is a schematic plan view which shows the one aspect | mode of the mesh of this invention. It is a schematic plan view which shows the state which mounted and fixed the test piece on the mesh of FIG. It is a schematic plan view which shows the state which connected and fixed the mesh of this invention to the holder for observation. FIG. 4 is a schematic plan view showing a state in which the mesh of FIG. 3 is divided and subsequently in a stretching process or a subsequent contraction process. It is a schematic plan view which shows the state which mounted and fixed the test piece to the commercial mesh which is a prior art example, and a commercial mesh. It is a schematic plan view which shows the state which mounted and fixed the test piece to the mesh of the prior art example disclosed in patent document 1, and a prior art example mesh.

Hereinafter, the present invention will be described in detail. 1 to 4 show an embodiment of the present invention, and FIGS.
The test piece observation method of the present invention includes a step of placing and fixing the test piece 3 on the mesh 1, a step of fixing the mesh 1 to the observation holders 5a and 5b, and moving the observation holders 5a and 5b in the extending direction. In the test piece observation method including the step of stretching the test piece 3 fixed to the placement region 1e of the mesh 1 and the step of observing the test piece 3 in the stretching process, the observation holders 5a and 5b After fixing the test piece 3, the mesh 1 is divided in the stretching process.
Further, the observation mesh 1 for the test piece of the present invention holds the test piece 3 in the extending direction in the test piece 3 in the stretching process and the mesh 1 that holds the test piece 3 in the contraction process from the stretching process. It is characterized in that at least a part of the bone-like column 1a of the mesh 1 is cut.

[mesh]
The mesh 1 which is embodiment of this invention can process and prepare the commercially available mesh 1, for example. As the mesh 1 of the present invention, for example, a mesh in which bone-like columns 1a are arranged in parallel in the sample stretching direction can be used, and a cross mesh is preferable. Here, the cross mesh is a mesh 1 composed of components obtained by intersecting the skeleton pillars 1a in a lattice shape or a cross shape. Here, as one of the modified examples of the cross mesh, a hexagonal cross mesh having a configuration in which the bony columns 1a are arranged in parallel in the sample extending direction and the bony columns 1a intersect at an angle of 120 degrees is also included. It is.
Conventionally, various meshes 1 are provided as commercial products. The material of the mesh 1 is preferably copper or the like, and the mesh size can be 100, 150, 200 mesh or the like, and 200 mesh is preferable. Here, the unit of mesh size: mesh means the number of meshes between 1 inch (25.4 mm), and in the present invention, parallel to the sample stretching direction between 1 inch in the direction orthogonal to the sample stretching direction. The number of bone-like columns 1a arranged in
Patent Document 1 [0015] discloses a modification of the mesh 1 in which a mesh opening 1d is provided at the mounting position 1e of the test piece 3. “In the case of the mesh 1 provided with the mesh-like opening 1d, not only the peripheral portion constituting the outer peripheral frame (outer edge 1b) but also the mesh thread portion (bone-like pillar 1a) surrounding the mesh hole (opening 1d) If the expansion slit 4 and the dividing slit 4 are not cut also at the peripheral edge of the mesh, the expansion slit 4 is opened to extend the mesh 1 in the extending direction, or the mesh 1 is divided into left and right. It has been understood that having a slit 4 is almost essential for observation, and that observation with a mesh 1 having no slit 4 is difficult. Surprisingly, however, the test piece observation mesh 1 of the present invention is not subjected to the special slit processing disclosed, and the test piece 3 is fixed to the observation holders 5a and 5b, and then the mesh 1 is applied in the stretching process. It is found that the mesh 1 can be divided, and preferably, by performing a specific cutting process on the mesh 1, it is found that the mesh 1 is automatically divided into left and right during the stretching process, and the test piece 3 in the stretching process and the shrinking process is accurately measured. It was completed as an invention that can be observed with good reproducibility.
In addition, the mesh 1 serves as a placement region 1e for fixing the test piece 3 to the upper surface of the central portion of the mesh 1, and the observation holder 5a in which the left and right sides sandwiching the placement region 1e are moved in the extending direction and the contracting direction. Test pieces 3 that are fixed to the mounting area 1e when the connection areas 1f and 1g are moved away from each other by the movement of the observation holders 5a and 5b. It is preferable that the test piece 3 is contracted when the connection regions 1f and 1g are moved in the proximity direction by moving the observation holders 5a and 5b from the stretched position. More preferably, the mesh 1 is composed of a cross mesh formed by intersecting the skeleton pillars 1a. This is because this structure is resistant to distortion in the mesh processing, stretching process, and shrinking process, so that handling before fixing and division in the stretching process can be realized in a balanced manner.

[Mesh processing]
It is preferable that the processing of the mesh 1 is performed in advance before the test piece 3 is placed and fixed. This is because the bone-like column 1a is covered with the test piece 3, so that it is difficult to cut from the upper surface. On the other hand, the outer edge 1b can be processed even after the test piece is placed and fixed. This is because it is desirable to avoid the opportunity to give no distortion. A cutting blade (such as a razor blade) can be used for processing. First, the outer edge 1b of the commercially available mesh 1 is cut. Processing may be excision processing or cutting processing.
Moreover, it is preferable that the outer edge 1b between the left and right connection regions 1f and 1g is cut, and at least one of the bone-like columns 1a holding the test piece 3 in the extending direction is cut. Is preferably left. This is because handling before fixing and splitting in the stretching process can be balanced. For example, even if the half of the bone-like column 1a is left, there is no problem in the division in the stretching process, and there is no problem even if the whole number is left. When the test piece 3 is to be placed so as not to straddle the bone-like column 1a, the number of places on which the test piece 3 is placed may be reduced if the remaining number is large.
Further, at least a part of the bone-like column may be cut, and it is preferable that a part of the bone-like column remains 1 to 10 and further 1 to 5 remain. More preferably, it is more preferable that one or two remains. With these configurations, handling before fixation and splitting in the stretching process can be achieved in a well-balanced manner. Furthermore, by controlling the remaining number of bone-like columns, the stretching process and contraction process of the specimen 3 can be made more finely and precise. It becomes possible to observe with good reproducibility.
In the microscopic observation using the light or electron beam transmission mode, it is preferable to further remove the bone-like column 1a cut in the placement region 1e in the central portion and process it into an aspect that forms the opening 1d.

[Cut out specimen]
First, a test using a microtome (trade name: Ultra Microtome, manufactured by Leica) from a sample of a rubber composition, resin, plastic, etc. (for example, urethane resin, phenol resin, polymer alloy, etc.) having a large stretchability. Piece 3 is produced. The size of the test piece 3 should just be the range which can be mounted and fixed to the mesh 1 of this invention. For example, a length of 200 μm × width of 400 to 600 μm × thickness of 100 nm is suitable. If the test piece 3 is excessively thick, not only is it not suitable for observation with a transmitted beam, but a thick part and a thin part may occur locally. On the contrary, if the test piece 3 is too thin, not only processing with good reproducibility becomes difficult, but also a complicated and advanced device is required to ensure that an unexpected force does not reach the test piece 3.

[Placement of test piece on mesh]
As shown in FIG. 2, the test piece 3 is placed and fixed so as to straddle the opening 1d on the placement region 1e on the upper surface of the center portion of the mesh 1 (diameter 3 mm) of the present invention.
As shown in FIG. 2B, it is desirable to fix a plurality of test pieces 3 to the mesh 1. If there is only one test piece that can be fixed to the mesh 1, the test piece 3 that may be damaged by observation caused by a high-power laser or electron beam has multiple test pieces 3. By changing the field of view one after another, such as changing the specimen 3 to be observed before receiving, there is an effect that it is easy to obtain highly reliable observation results in both the stretching process and the shrinking process.

[Fixing the mesh to the observation holder]
As shown in FIG. 3, the mesh 1 is placed on the observation holder 5, and the connection regions 1f and 1g on the left and right sides of the mesh 1 are sandwiched between the holding plates 5c and 5d of the observation holders 5a and 5b and tightened with screws 5e and 5f. And fix.
In the embodiment shown in FIG. 3, since the mesh 1 is processed in advance before the test piece 3 is placed and fixed on the mesh 1, a high degree of processing such as processing performed after fixing to the observation holder 5 is performed. It requires no skill, is easy to handle, and can be fixed with good reproducibility. Furthermore, the observation can be performed with the origin state reliably maintained without distorting the test piece 3.
In addition, since the mesh 1 is not completely divided, it is easy to adjust the angle with respect to the extension direction, and even a slight misalignment of the mesh 1 can be easily fine-tuned without worrying about distortion to the test piece 3. In addition, since it can be surely confirmed that the test piece 3 before the start of observation is in the origin state (the stretched zero state), observation with high accuracy and good reproducibility becomes possible.

[Observation (for example, transmission microscope observation)]
Specifically, in the observation step, the observation holder 5 to which the mesh 1 is fixed is set in a transmission electron microscope (for example, CM30 manufactured by Philips, acceleration voltage 200 KV), and an arbitrary stretching ratio or after stretching is desired to be observed. The test piece 3 having an arbitrary shrinkage ratio is observed.

[Observation of stretching process]
First, as shown in FIG. 3, the state where the stretching ratio of the observation holder 5 is 0% is observed. Since the mesh 1 is not completely divided, or because the mesh 1 is divided in the microscope, it can be reliably confirmed that the test piece 3 is in the origin state (the stretched zero state).
Next, as shown in FIG. 4, the observation holders 5 a and 5 b to which the left and right connection regions 1 f and 1 g of the mesh 1 are fixed are moved in the extending direction (the direction in which the left and right are expanded in FIG. 4). 3 is stretched, and a test piece 3 having an arbitrary stretching ratio in the stretching process, for example, 50%, 100%, 150%, etc. is observed. When the observation holders 5a and 5b are moved away from each other in the stretching direction, the bone-like column 1a and the test piece 3 of the mesh 1 are initially stretched integrally, and in the middle of the stretching process of the test piece 3, the mesh 1 Since the remaining bone-like column 1a reaches the breaking limit elongation, the mesh 1 is divided without giving strain or the like to the test piece 3.
The separation gap gradually expands, and the test piece 3 having both the left and right sides fixed to the meshes 2a and 2b is extended in the left and right direction in the drawing and stretched.

[Observation of contraction process]
Further, after the observation in the stretching process, the meshes 2a and 2b separated by moving the observation holders 5a and 5b in the contraction direction (the directions in which the left and right in FIG. Shrink and observe the test piece 3 at an arbitrary stretch ratio in the shrinking process (returning process), for example, 100%, 50%, 0%, etc.
When the observation holders 5a and 5b are moved in the contraction direction (the direction in which the left and right sides in FIG. 4 are close to each other) from the stretching process, the meshes 2a and 2b that have been divided to the left and right are close to each other. The self 2a and 2b themselves can return to the position where the integrated mesh 1 was present before separation without leaving any distortion. Therefore, as long as the test piece 3 does not have a remarkable hysteresis characteristic, it can be returned to the state before stretching, in which the strain is zero, and not only the stretching process but also the state of the test piece 3 in the contraction process (returning process). It becomes possible to observe.

  The above-described test piece observation mesh 1 and the test piece observation method of the present invention described above can be particularly preferably used for a transmission electron microscope (TEM) and a scanning electron microscope (SEM). Furthermore, it can be used for a scanning probe microscope (SPM), a laser microscope, an optical microscope, and the like.

  Thus, the observation mesh 1 and the test piece observation method of the test piece of the present invention not only observe the test piece 3 in the stretching process, but also accurately and reproduce the observation of the test piece 3 in the contraction process (return process). Rupture analysis, damage, deterioration analysis, wear, etc. for test pieces 3 such as rubber, resin, plastic, etc. (for example, urethane resin, phenol resin, polymer alloy, etc.) that have been made thin It is effective for various analyzes such as analysis, analysis of the reinforcement mechanism of polymers and fillers, analysis of the mechanism of hysteresis loss generation, and blending design based on these analyses.

  EXAMPLES Hereinafter, although this invention is demonstrated concretely based on an Example, this invention is not limited to these Examples.

[Examples 1 to 5, Comparative Examples 1 to 4]
Examples 1 to 5 using the observation mesh 1 of the test piece of the present invention, Comparative Examples 1 to 3 using the conventional mesh 1 disclosed in Patent Document 1, and Comparative Examples using the conventional commercial cross mesh 1 Table 1 shows the results of observation and evaluation of No. 4.
The commercially available cross mesh 1 used for the test has a disk shape with a diameter of about 3 mm, and the bone-like pillar 1a intersects the upper edge 10 × the right and left 10 at a right angle from the outer edge 1b, and has a substantially square basic shape. An opening 1d is formed. This commercially available cloth mesh 1 was subjected to processing such as cutting under the conditions described in Table 1 and tested. The sample used for the test was rubber, and its formulation is shown in Table 2. The number of samples used for the test was placed and tested in the number shown in Table 1.
Quantitative evaluation by observation of reproducibility, etc. and qualitative evaluation by observation of handling, etc. were performed, and the results were comprehensively evaluated.

[Evaluation methods]
Ten meshes 1 were prepared for each condition, and the success rate was calculated from the number of meshes 1 that could be observed until the contraction process. The factors that could not be observed were ascertained for each process. The damage rate was calculated from the number of meshes 1 that were damaged during mounting and fixing, and the deformation was calculated from the number of meshes 1 in which distortion was observed during the stretching process and the contraction process.

According to the result of Table 1, in Examples 1-5 in which at least one bone-like column 1a remains as compared with Comparative Examples 1 and 2 in which the bone-like column 1a is completely divided, the test piece 3 It can be seen that observation with good reproducibility can be performed with excellent handling properties without causing damage or the like.
Further, compared with Comparative Example 3 in which the outer edge 1b is not completely divided and in Example 4 in which the outer edge 1b is not divided at all, in Examples 1 to 5, the test piece 3 is not damaged and is not distorted. It can be seen that observation with good reproducibility can be performed with excellent accuracy.

[Observation of damage, distortion, etc.]
In Comparative Examples 1 and 2, the bone 4 is completely divided by the slit 4 and the remaining bone-like columns 1a are zero. Before the test piece 3 is fixed, all of the 10 bone-like columns 1a are provided with the dividing slits 4b. It is. This is because, after fixing, the bone-like column 1 a is covered with the test piece 3, so that it cannot be cut from the upper surface direction. In Comparative Example 1, since the mesh 1 is completely divided by the slits 4, handling properties are low, and when moving to the observation holder 5 or fixing with screws, 9 out of 10 are distorted by rattling or the like. . It was evaluated that it required special devices such as special dedicated jigs and advanced skills. Further, in Comparative Example 2 in which the cutting slit 4a was inserted into the outer edge 1b after the test piece 3 was placed and fixed, the undesired force was applied at the time of the cutting process. In addition, distortion was observed during the stretching and shrinking processes. Since the longitudinal direction of the test piece 3 could not be adjusted with the extending direction, or the so-called “single tightening” that was offset by the screw tightening of the observation holder 5, it is considered that an unexpected bias occurred in the mesh 1.
In Comparative Example 3, the slit 4 was cut to about half of the outer edge 1b. It seems that skill is required because of variations in the depth of cut. At the time of processing, distortion occurred in 4 out of 10 pieces. The mesh 1 was deformed by stretching and the strain remained. Since the slit 4a was insufficient and the distortion of the outer edge 1b was remarkable, the test piece 3 stretched on the mesh 1 could not be returned to its original state, and the test piece 3 in the contraction process could not be observed. .
In Comparative Example 4, the conventional commercially available cross mesh 1 is used without being processed, and it is almost impossible to stretch the test piece 3 fixed to the mesh 1, and therefore, the stretched test piece 3 is observed. I could not. Moreover, although the conventional commercially available cross mesh 1 was forcibly stretched, the amount of stretching was slight, and the mesh 1 was deformed by stretching and strain remained. In particular, since the distortion of the outer edge 1b was remarkable, the test piece 3 stretched on the mesh 1 could not be returned to the original state, and the test piece 3 in the contraction process could not be observed.

* 1: Number of bone-like columns remaining in the stretching direction (0 to 10).
* 2: With respect to the outer edge, it is indicated by “partial cut”, “partial cut”, “1/2 cut”, and “no processing”.
* 3: An asterisk (*) was added when processing was performed before mounting and fixing.
* 4: An asterisk (*) was added when processing was performed before mounting and fixing.
* 5: Sample types such as rubber and resin.
* 6: Indicates the number of test pieces placed.
* 7: Comprehensive evaluation was shown by suitable “◯”, observable “Δ”, and unsuitable “×”.
* 8: “0/10 to 10/10” indicates the success rate of observation until the contraction process.
* 9: “0/10 to 10/10” indicates the breakage rate when mounted and fixed.
* 10: “0/10 to 10/10” indicates the breakage rate during processing such as parting.
* 11: “0/10 to 10/10” indicates a distortion rate in the stretching process.
* 12: “0/10 to 10/10” indicates the distortion rate during the contraction process.
* 13: The handling property was evaluated as “good”, “good”, and “poor”.
* 14: The evaluation of the shortness of work time was shown by good “◯”, acceptable “Δ”, and impossible “×”.
* 15: The evaluation of observability during the stretching process was shown with good “◯”, acceptable “Δ”, and impossible “×”.
* 16: The evaluation of observability during the contraction process was shown with good “◯”, acceptable “Δ”, and impossible “×”.

The test piece observation mesh and the test piece observation method of the present invention are suitable for observing the state of the test piece in the stretching process and the shrinking process, and the test piece is a sample to be stretched, for example, stretchable. It can be applied to the observation of stretching and shrinking processes of large rubber, resin and plastic specimens.
The test piece observation mesh and the test piece observation method of the present invention can be applied to observation with a scanning electron microscope, a transmission electron microscope, a scanning probe microscope, a laser microscope, an optical microscope, or the like.

DESCRIPTION OF SYMBOLS 1 Test piece observation mesh 1a Bone column 1b Outer edge 1c Outer edge cutting part 1d Opening 1e Placement area 1f, 1g Left and right connection area 2 Divided test piece observation mesh 2a, 2b Left and right test piece Observation mesh 3 Test piece 4 Slit 4a Dividing slit 4b in the outer edge 4b Dividing slit 5 in the skeleton-like column 5 Observation holder 5a, 5b Left and right observation holder 5c, 5d Left and right holding plate 5e, 5f Left and right Screw

Claims (16)

A step of placing and fixing the test piece on the mesh;
Fixing the mesh to the observation holder;
Subsequently, the step of extending the test piece fixed to the placement region of the mesh by moving the observation holder in the extending direction;
In the method for observing a test piece including the step of observing the test piece in the stretching process,
After fixing the test piece to the observation holder, the mesh is divided in the stretching process. Following the step of observing the test piece in the stretching process,
Furthermore, the step of shrinking the test piece fixed to the placement region of the mesh by moving the observation holder in the shrinking direction;
The method for observing a test piece according to claim 1, further comprising: observing the test piece in the contraction process.   3. The test piece observation method according to claim 1, wherein the test piece is fixed to the observation holder without completely dividing the mesh.   It observes with a microscope, The observation method of the test piece in any one of Claims 1-3 characterized by the above-mentioned.   The test piece observation method according to claim 4, wherein the mesh is divided in the microscope.   The test piece observation method according to claim 1, wherein a plurality of the test pieces are placed and fixed on the mesh.   The method for observing a test piece according to any one of claims 1 to 6, wherein the mesh is composed of a cross mesh formed by intersecting bone columns.   7. The test piece observation method according to claim 1, wherein an outer edge between the left and right connection regions is cut.   The method for observing a test piece according to any one of claims 1 to 6, wherein a part of the bone-like column holding the test piece in the extending direction is cut and at least one remains.   In the mesh that holds the test piece in the stretching process and the test piece in the contraction process from the stretching process in an observable manner, at least a part of the bone-like column of the mesh that holds the test piece in the extending direction is cut. Mesh characterized by. The mesh is a connection region in which the upper surface of the center portion is a mounting region for fixing the test piece, and the right and left sides sandwiching the mounting region are fixed to an observation holder that is moved in the extending direction and the contracting direction. And
When the connection region is moved in the direction of separation by the movement of the observation holder, the test piece, which is fixed on both the left and right sides, is stretched and / or the observation holder is moved from the stretched position. The mesh according to claim 10, wherein the test piece is contracted when the connection region is moved in the proximity direction by movement.   The mesh according to claim 10 or 11, wherein the mesh is composed of a cross mesh formed by intersecting bone columns.   The mesh according to any one of claims 10 to 12, wherein an outer edge between the left and right connection regions is cut.   The mesh according to any one of claims 10 to 13, wherein 1 to 10 of the bone-like columns remain.   The mesh according to claim 14, wherein 1 to 5 of the bone columns remain.   The mesh according to claim 15, wherein one or two of the bone-like columns remain.

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