JP6265196B2 - Method and apparatus for evaluating flexibility of sheet-like object - Google Patents

Description

  The present invention relates to a method and an apparatus for evaluating the flexibility of a sheet-like object.

Sheet-like materials such as metal films are used in many fields. Depending on the application, flexibility may be required for the sheet-like material. In order to obtain a sheet-like material excellent in flexibility, it is necessary to establish a method capable of appropriately evaluating the flexibility.
As a method for evaluating the mechanical properties of the sheet-like material, for example, a tensile strength test (Japanese Industrial Standard JIS Z2241) can be mentioned. In the tensile strength test, a test piece having a predetermined shape is prepared, both ends of the test piece are gripped, and a load is applied to one end, whereby the relationship between the load and the elongation of the test piece is measured. However, when the sheet material to be tested is, for example, a metal film having a very thin film thickness (for example, 100 μm or less), mechanical properties such as flexibility cannot be appropriately evaluated. This is because in the tensile strength test, it is necessary to cut the test object into a predetermined shape in order to produce a test piece, and the measurement results are affected by burrs and shape variations that occur at that time.
In addition, examples of methods for evaluating the mechanical properties of materials include bending tests, sagging tests, and Vickers hardness tests. However, when the film thickness of the test object is thin, the flexibility cannot be evaluated appropriately. There is.

  Therefore, an object of the present invention is to provide an evaluation method and an evaluation apparatus for the flexibility of a sheet-like test object that can appropriately evaluate the flexibility even when the film thickness is extremely thin.

The inventors of the present invention have found that the above problem can be solved by pressing the pressing jig perpendicularly to the sheet-like object and measuring the force applied to the pressing jig and the amount of displacement of the pressing jig. .
That is, the present invention includes the following matters.
(1) a step of supporting the entire circumference of the sheet-like test object so that a non-supporting region having a closed shape is formed on the sheet-like test object by the test object support jig;
A step of pushing one end of the pushing jig perpendicularly to the sheet-like object into the non-supporting region and measuring a relationship between a force received by the pushing jig and a displacement amount of the pushing jig. The evaluation method of the flexibility of a sheet-like test object.
[2] The sheet-like test object is a metal film,
The method described in [1] above.
[3] The thickness of the sheet-like test object is 0.1 μm to 100 μm.
The method described in [1] or [2] above.
[4] The supple value of the sheet-like test object is 0.5 N / mm to 30.0 N / mm, and the supple value is the displacement of the push jig by the force (N) received by the push jig. It is a value represented by a value (N / mm) divided by an amount (mm).
The method according to any one of [1] to [3].
[5] The sheet-like test object is a support film for a hydrogen permeable metal film,
The method according to any one of [1] to [4].
[6] The specimen support jig has a pair of clamping members that clamp the sheet-shaped specimen,
One of the pair of clamping members is provided with an opening,
On the other of the pair of clamping members, an opening or a recess is provided at a position corresponding to the opening provided on the one clamping member,
The method according to any one of [1] to [5], wherein the non-supporting region is formed at a position corresponding to an opening provided in the one clamping member.
[7] The non-supporting region is a circle having a diameter of 9 mm to 14 mm.
The method according to any one of [1] to [6].
[8] One end of the pressing jig has a shape corresponding to a part of a sphere having a diameter of 5 mm to 10 mm.
The method according to any one of [1] to [7].
[9] Further, based on the relationship between the force applied to the pushing jig and the displacement amount of the pushing jig, the force (N) received by the pushing jig is divided by the displacement amount (mm) of the pushing jig. The method according to any one of [1] to [8], further comprising a step of obtaining the measured value (N / mm) as a supple value of the sheet-like test object.
[10] A test object support jig configured to support the entire circumference of the sheet test object so that a closed non-support region is formed in the sheet test object,
A pressing jig supporting portion configured to support the pressing jig and to push one end of the pressing jig into the non-supporting region perpendicularly to the sheet-like object;
A measurement mechanism for measuring the relationship between the force received by the pressing jig and the amount of displacement of the pressing jig;
Comprising
An apparatus for evaluating the flexibility of a sheet-like object.
[11] The evaluation apparatus according to [10], wherein the thickness of the sheet-like test object is 0.1 μm to 100 μm.
[12] The supple value of the sheet-like test object is 0.5 N / mm to 30.0 N / mm, and the supple value is the displacement of the push jig by the force (N) received by the push jig. It is a value represented by a value (N / mm) divided by an amount (mm).
The evaluation apparatus according to [10] or [11].
[13] The sheet-like test object is a support film for a hydrogen permeable metal film,
The method according to any one of [10] to [12].
[14] The evaluation device according to any one of [10] to [13], wherein the non-support region is a circle having a diameter of 9 mm to 14 mm.
[15] The evaluation apparatus according to any one of [10] to [14], wherein one end of the pushing jig has a shape corresponding to a part of a sphere having a diameter of 5 mm to 10 mm.

  ADVANTAGE OF THE INVENTION According to this invention, even if it is a case where a film thickness is very thin, the evaluation method and evaluation apparatus of the flexibility of a sheet-like test object which can evaluate flexibility smoothly are provided.

FIG. 1 is a schematic diagram showing an evaluation apparatus. FIG. 2 is an enlarged view showing a part of the evaluation apparatus. FIG. 3 is a cross-sectional view schematically showing a pair of clamping members. FIG. 4 is a schematic view showing a pushing jig. FIG. 5 is a schematic view showing a method for evaluating the flexibility of a sheet-like test object. FIG. 6 is a graph showing the relationship between the amount of displacement obtained in Examples 1 to 3 and the test force.

  FIG. 1 is an external view of an evaluation apparatus 1 according to an embodiment of the present invention. FIG. 2 is a schematic diagram showing the evaluation device 1. As shown in FIGS. 1 and 2, the evaluation apparatus 1 according to this embodiment includes a main body 6, a pedestal 2, a pressing jig support section 3, a measuring apparatus 10, a pressing jig 4, and a test object support jig. 5 and a drive mechanism 12 are provided. The pushing jig 4 and the test object supporting jig 5 are detachable, and are depicted only in FIG. 2 and are not depicted in FIG.

The pedestal 2 is provided to support the test object support jig 5 and is fixed to the main body 6.
The specimen support jig 5 is provided to support the sheet-like specimen 9 that is a test target. The test object support jig 5 is detachably attached to the base 2. FIG. 3 is a cross-sectional view schematically showing the test object support jig 5. The test object support jig 5 has a pair of clamping members (5-1 and 5-2). One clamping member 5-1 has an opening 8. The other clamping member 5-2 is provided with a recess 7 at a position corresponding to the opening 8. Each of the opening 8 and the recess 7 is circular having a predetermined diameter a. In addition, it may replace with the recessed part 7 and the opening may be provided in the clamping member 5-2. Each clamping member (5-1, 5-2) is provided with a thread (11-1 and 11-2), and the clamping member 5-1 is held in a state where the sheet-like object 9 is clamped. Can be screwed into the clamping member 5-2.
On the other hand, the sheet-like object 9 is a circle having a slightly larger diameter than the opening 8. The sheet-like test object 9 is clamped by a pair of clamping members (5-1, 5-2) at the periphery.
The central portion of the sheet-like object 9, that is, the region corresponding to the opening 8 does not contact the object support jig 5. That is, the specimen support jig 5 is configured to support the entire circumference of the sheet-like specimen 9, and a closed shape corresponding to the opening 8 is formed at the center of the sheet-like specimen 9. An unsupported region is formed.

The pressing jig support portion 3 (see FIGS. 1 and 2) is provided to support the pressing jig 4. The pressing jig support part 3 is attached to the main body part 6 so as to be movable in a direction perpendicular to the sheet-like object 9.
The drive mechanism 12 is attached to the main body 6 and has a function of moving the push jig support 3. The drive mechanism 12 is, for example, a motor.

The pushing jig 4 has a rod shape. The pressing jig 4 is supported by the pressing jig support portion 3 so as to extend in a direction perpendicular to the sheet-shaped test object 9 above the sheet-shaped test object 9. Further, the pushing jig 4 is supported so that one end thereof is located immediately above the center of the opening 8 of the test object supporting jig 5.
FIG. 4 is a schematic diagram illustrating an example of the pushing jig 4. Preferably, as shown in FIG. 4, one end (tip) of the pressing jig 4 has a shape corresponding to a part of a sphere having a predetermined diameter b.

  The measuring device 10 has a function of detecting a force applied to the pushing jig 4 and a displacement amount of the pushing jig 4. Specifically, the measurement apparatus 10 includes a load cell 10-1 and an encoder 10-2 (see FIG. 2). The load cell 10-1 is provided between the pressing jig support 3 and the pressing jig 4 and has a function of detecting a force applied to the pressing jig 4. The encoder 10-2 is connected to the drive mechanism 12, and is configured to detect the displacement amount of the pushing jig support portion 3, that is, the displacement amount of the pushing jig 4.

Subsequently, an evaluation method according to an embodiment of the present invention will be described.
First, the sheet-like object 9 is supported by the object-supporting jig 5 and attached to the base 2. Further, the pressing jig 4 is attached to the pressing jig support 3 via the load cell 10-1.
Next, the driving mechanism 12 moves the push jig support 3 downward (to the object support jig 5 side). As a result, as shown in FIG. 5, one end of the pushing jig 4 is pushed vertically into the sheet-like object 9 from the center of the opening 8 provided in the clamping member 5-1. The pushing jig 4 is pushed in until it breaks through the sheet-like object 9. At this time, the force received by the pressing jig 4 and the amount of displacement of the pressing jig 4 are measured by the measuring device 10. The measurement result is stored in a computer (not shown) or the like as data indicating the relationship between the force received by the pressing jig 4 and the amount of displacement of the pressing jig 4.

Based on the obtained data, a parameter indicating the flexibility of the sheet-like object 9 is calculated. As such a parameter, for example, “flexible value” can be cited.
Here, in this specification, the “flexible value” is a value represented by a value (N / mm) obtained by dividing the force (N) received by the pushing jig by the displacement (mm) of the pushing jig. Shall. Specifically, a graph with the horizontal axis representing the amount of displacement and the vertical axis representing the force (test force) received by the pressing jig 4 is created, and a good linearity range (for example, a correlation coefficient R obtained by linear approximation). ^A supple value can be calculated by obtaining the slope in the region where ² exceeds 0.9.

According to the evaluation method described above, it is possible to appropriately evaluate the flexibility of the sheet-like object 9 even when the film thickness is extremely thin. Specifically, the evaluation method of the present embodiment provides data indicating the relationship between the displacement and the test force with extremely high linearity. In the test force-displacement graph, the range where the linearity is high is a region where the test force and the displacement amount are proportional, and is a region where the relationship between the test force and the displacement amount is expressed most simply. In this region, the flexibility of the sheet-like object 9 is appropriately reflected in the evaluation result.
In addition, according to the evaluation method according to the present embodiment, unlike the case where the tensile strength test is used, it is possible to reduce the influence of the variation in the shape of the test piece on the measurement result. From this point of view, it is possible to accurately evaluate the flexibility.

  The kind of the sheet-like test object 9 to be measured is not particularly limited. However, the evaluation method of this embodiment is suitable for evaluating the mechanical properties of metal films (for example, Ni film, Al film, and Cu film).

  In addition, when the sheet-like test object 9 is a metal film, the film thickness is preferably 0.1 to 100 μm, more preferably 5 μm to 50 μm, and still more preferably 5 μm to 20 μm. Most preferably, it is 5 micrometers-15 micrometers. If the thickness of the metal film is too small, it is easy to break the film, and accurate measurement tends to be difficult. On the other hand, when the film thickness is too large, the structure of the sheet-like test object 9 is close to a plate shape, and the evaluation by the tensile tester may be more accurate and flexible.

  Further, the sheet-like object 9 to be measured preferably has a supple value of 0.5 N / mm to 30.0 N / mm, and more preferably 1.0 N / mm to 20.0 N / mm. 2.0 N / mm to 10.0 N / mm is more preferable. If the supple value is too small, sufficient test force cannot be obtained with respect to the displacement, and it becomes difficult to obtain a high linearity relationship (test force-displacement graph). In addition, even when the supple value is too large, a sufficient amount of displacement cannot be obtained with respect to the test force, and it is difficult to obtain a relationship with high linearity.

  The diameter a (see FIG. 3) of the opening 8 provided in the holding member 5-1 is preferably 9 mm to 14 mm, more preferably 10 mm to 13 mm, and still more preferably 11 mm to 12 mm. If the diameter a is too small, a sufficient amount of displacement cannot be obtained for the test force, and if it is too large, a large sample area is required.

Although the shape (refer FIG. 4) of the end of the pushing jig | tool 4 is not specifically limited, As mentioned above, it is preferable that it is a shape corresponding to a part of ball | bowl which has the diameter b. For example, when the shape of one end of the pushing jig 4 is a polygon, the pushing jig 4 comes into contact with the sheet-like test object 9 at corner portions, and the force applied to the sheet-like test object 9 is increased. Concentrating on the corner portion, the sheet-like object 9 is easily torn along the way. As a result, it is difficult to secure a region having a high linearity relationship in the test force-displacement amount graph. Further, when the shape of one end of the pressing jig 4 is a flat plate shape such as a flat plate shape, the sheet-shaped test object 9 is deformed so as to form an acute angle at the end portion of the flat plate shape. High relationships are difficult to obtain. On the other hand, when the shape of one end of the pressing jig 4 has a shape corresponding to a part of the sphere, the pressing jig 4 is in contact with the sheet-like object 9 with a curved surface. In this case, since the sheet-like object 9 is smoothly stretched while forming an obtuse angle when the pushing jig 4 is pushed in, a relationship with higher linearity is easily obtained.
The diameter b is preferably 5 mm to 10 mm, more preferably 6 mm to 9 mm, and still more preferably 7 mm to 8 mm. When the diameter b is too small, the sheet-like object 9 is pressurized at a point, and the sheet-like object 9 is easily broken easily, and it is difficult to secure a region with high linearity. On the other hand, when the diameter b is too large, it is necessary to increase the specimen support jig 5, and the required sample area also increases.
Further, the ratio of the diameter b to the diameter a of the opening 8 (diameter b / diameter a) is preferably 0.3 to 0.9, more preferably 0.4 to 0.8, and More preferably, it is 5-0.7. When the ratio of the diameter b to the diameter a is in such a range, a relationship with high linearity is easily obtained.

  The pushing speed of the pushing jig 4 is preferably 0.1 mm / min to 10.0 mm / min, more preferably 0.5 mm / min to 5.0 mm / min, and 1.0 mm / min to More preferably, it is 2.0 mm / min. If the indentation speed is too slow, a long test is required. On the other hand, when the pushing speed is too high, the sheet-like object 9 is likely to break, and the film is likely to break without sufficiently securing a region with high linearity.

The evaluation method of this embodiment is suitable for evaluating the flexibility of a metal film used as a support film for a hydrogen permeable metal film, for example. The hydrogen permeable metal film is a film having a function of selectively permeating hydrogen, and includes a hydrogen permeable metal layer and a support film that supports the hydrogen permeable metal layer. As the hydrogen permeable metal layer, for example, palladium, palladium-silver alloy, palladium-copper alloy, or the like can be used. The thickness of the hydrogen permeable metal layer is, for example, 0.01 μm to 50 μm, preferably 0.5 to 20 μm. On the other hand, as the support film, for example, a porous Ni film can be used. The thickness of the porous Ni film is, for example, 1.0 μm to 100 μm, preferably 1 μm to 15 μm.
The hydrogen permeable metal membrane is used to separate and purify hydrogen in, for example, a fuel reformer using a gas or liquid hydrocarbon such as a methane-containing gas, an alcohol such as methanol, and water (steam). . The support membrane used for such a hydrogen permeable metal membrane is required to be thin and flexible from the viewpoint of hydrogen permeability. And the evaluation method which concerns on this embodiment can evaluate appropriately the mechanical characteristic of the metal film which has a film thickness and the flexibility of the magnitude | size calculated | required by the support body film | membrane for hydrogen permeable metal films.

Subsequently, examples will be described in order to explain the present invention in more detail.
[Example 1]
Using a 10 μm-thick Ni film obtained by a rolling method as the sheet-like object 9 to be measured, the relationship between the test force and the displacement is measured using the evaluation apparatus 1 described with reference to FIGS. did.
Specifically, the sheet-like object 9 was cut into a circle having a diameter of 20 mm. A sheet-like test object 9 was clamped using a pair of clamping members (5-1 and 5-2) having an opening 8 and a recess 7 having a diameter of 12 mm and fixed to the base 2. Further, a jig having a shape corresponding to a part of a sphere having a diameter of 7 mm was prepared at one end as the pressing jig 4 and attached to the pressing jig support 3. By moving the pressing jig support portion 3 toward the pair of clamping members 5 at a speed of 1 mm / min, one end of the pressing jig 4 was brought into contact with the sheet-like object 9 from the center of the opening 8. Further, the pushing jig 4 was pushed in until the sheet-like object 9 was broken, and the relationship between the displacement amount of the pushing jig 4 and the test force (the force received by the pushing jig 4) was measured by the measuring device 10.

[Example 2]
A 10 μm-thick Cu film obtained by a rolling method was used as the sheet-like object 9 and the relationship between the displacement and the test force was measured in the same manner as in Example 1.
[Example 3]
As the sheet-like object 9, a 10 μm thick Al film obtained by a rolling method was used, and the relationship between the displacement and the test force was measured in the same manner as in Example 1.

FIG. 6 is a graph showing the relationship between the amount of displacement obtained in Examples 1 to 3 and the test force. In FIG. 6, the result of Example 1 is indicated by a line “a”, the result of Example 2 is indicated by a line “b”, and the result of Example 3 is indicated by a line “c”. Here, in each graph of FIG. 6, the portion where the test force rapidly decreases corresponds to the point where the sheet-like test object 9 is broken (hereinafter, the breaking point).
In the graph shown in FIG. 6, a range with good linearity (correlation coefficient R ² > 0.9 by linear approximation) was obtained, and the slope was calculated as a supple value. As a result, the flexible value of Example 1 (Ni film) is 15.78 N / mm, the flexible value of Example 2 (Cu film) is 13.50 N / mm, and the flexible value of Example 3 (Al film). The value was 1.97 N / mm.

  As shown in FIG. 6, in any of Examples 1 to 3, the relationship between the displacement and the test force shows very high linearity in the region from the origin to the breaking point. This indicates that the data obtained by the method according to the present invention accurately reflects the elastic properties of the sheet-like object 9.

[Comparative example]
Using the sheet-like specimen 9 used in Examples 1 to 3, an attempt was made to evaluate mechanical properties by a tensile strength test. However, when any sheet-shaped specimen 9 is used, the thickness of the sheet-shaped specimen 9 is too thin to properly grip the test piece, and an appropriate test result cannot be obtained. It was. In the tensile test, the burrs generated when the sheet-like specimen 9 is cut out often breaks the sheet-like specimen 9 during the test, and the tendency is more prominent as the film thickness becomes thinner.

DESCRIPTION OF SYMBOLS 1 Evaluation apparatus 2 Base 3 Push jig support part 4 Push jig 5 Test object support jig 5-1, 5-2) Holding member 6 Main part 7 Recess 8 Opening 9 Sheet-like test object 10 Measuring apparatus 10- DESCRIPTION OF SYMBOLS 1 Load cell 10-2 Encoder 11 (11-1 to 11-2) Screw thread 12 Drive mechanism

Claims (15)

A step of supporting the entire circumference of the sheet-like specimen so that a non-supporting region of a closed shape is formed on the sheet-like specimen by the specimen-supporting jig;
Perpendicularly to the sheet-like test object, pressing one end of the pressing jig into the non-supporting region, measuring the relationship between the force received by the pressing jig and the displacement amount of the pressing jig;
Based on the relationship between the force applied to the pressing jig and the displacement amount of the pressing jig, a value obtained by dividing the force (N) received by the pressing jig by the displacement amount (mm) of the pressing jig (N / mm) as a supple value of the sheet-like test object,
Comprising
A method for evaluating the flexibility of a sheet-like object.   A step of supporting the entire circumference of the sheet-like specimen so that a non-supporting region of a closed shape is formed on the sheet-like specimen by the specimen-supporting jig;
  A step of pushing one end of the pressing jig perpendicularly to the sheet-like object into the non-supporting region and measuring a relationship between a force received by the pressing jig and a displacement amount of the pressing jig;
With
  The specimen support jig has a pair of clamping members that clamp the sheet-shaped specimen.
  One of the pair of clamping members is provided with an opening,
  On the other of the pair of clamping members, an opening or a recess is provided at a position corresponding to the opening provided on the one clamping member,
  The non-supporting region is formed at a position corresponding to an opening provided in the one clamping member, and is a method for evaluating the flexibility of a sheet-like test object.   Furthermore, based on the relationship between the force applied to the pushing jig and the displacement amount of the pushing jig, a value obtained by dividing the force (N) received by the pushing jig by the displacement amount (mm) of the pushing jig ( N / mm) is calculated | required as a supple value of the said sheet-like test object, The method described in Claim 2 is provided. The sheet-like object is a metal film,
The method according to any of claims 1 to 3. The thickness of the sheet-like test object is 0.1 μm to 100 μm,
The method according to any of claims 1 to 4. The supple value of the sheet test object is 0.5 N / mm to 30.0 N / mm.
The method according to any one of claims 1 to 5 . The sheet-like test object is a support membrane for a hydrogen permeable metal membrane,
The method according to any one of claims 1 to 6 . The non-supporting region is a circle having a diameter of 9 mm to 14 mm;
A method according to any of claims 1 to 7 . How one end of the pressing pin has a shape corresponding to a portion of a sphere having a diameter of 5 mm to 10 mm, according to any of claims 1 to 8. A specimen support jig configured to support the entire circumference of the sheet-like specimen so that a non-supporting area of a closed shape is formed in the sheet-like specimen;
A pressing jig supporting portion configured to support the pressing jig and to push one end of the pressing jig into the non-supporting region perpendicularly to the sheet-like object;
A measurement mechanism for measuring the relationship between the force received by the pressing jig and the amount of displacement of the pressing jig;
A calculation unit that calculates a value (N / mm) obtained by dividing a force (N) received by the pressing jig by a displacement amount (mm) of the pressing jig as a supple value;
An apparatus for evaluating the flexibility of a sheet-like object. The evaluation apparatus according to claim 10, wherein a thickness of the sheet-like test object is 0.1 μm to 100 μm. Supple value of the sheet specimen is Ru 0.5N / mm~30.0N / mm der,
The evaluation apparatus according to claim 10 or 11. The sheet-like test object is a support membrane for a hydrogen permeable metal membrane,
The evaluation apparatus according to claim 10. The evaluation device according to claim 10, wherein the non-supporting region is a circle having a diameter of 9 mm to 14 mm.   The evaluation apparatus according to claim 10, wherein one end of the pressing jig has a shape corresponding to a part of a sphere having a diameter of 5 mm to 10 mm.

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