Rheological measurement device

Abstract

To facilitate rheological measurement of various samples subjected to high stress.SOLUTION: A rheological measurement device (10) for measuring rheological characteristics of a sample (SA) is provided, the rheological measurement device comprising first and second clamping parts (11, 12) arranged to face each other in a first direction and configured to clamp a sample, and movement elements (13a, 13b) for moving at least one of the first and second clamping parts in a second direction different from the first direction.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a rheology measuring device. [Background technology]

[0002] Rheology measuring devices that measure the rheology of a target object, such as the viscosity and viscoelasticity, are known, such as viscometers (see, for example, Patent Document 1). Viscometers come in various types (for example, double cylinder type, parallel plate type, and capillary type). [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Publication No. 2022-071192 Summary of the Invention [Problem to be solved by the invention]

[0004] However, the above-mentioned conventional techniques have a certain limit to the stress (for example, shear rate) that can be applied to various measurement targets (samples). For example, in a double-cylinder type or parallel-plate type viscometer, a shear force is generated by rotating a motor, but due to the limit of the motor rotation speed, the shear force can be applied within 10 4 It was difficult to achieve a shear rate of more than 1 / s. In addition, in capillary viscometers, the sample (liquid) is passed through the capillary (channel) to increase the shear rate, and 6 However, the capillary is thin and prone to clogging, making it difficult to measure highly viscous samples.

[0005] An object of one aspect of the present invention is to provide a rheology measurement device that facilitates rheology measurements of various samples under conditions where high stress is applied. [Means for solving the problem]

[0006] In order to solve the above problems, a rheology measuring device according to one embodiment of the present invention is a rheology measuring device for measuring the rheological properties of a sample, and includes first and second clamping units arranged opposite each other in a first direction and clamping the sample, and a moving element for moving at least one of the first and second clamping units in a second direction different from the first direction. [Effects of the Invention]

[0007] According to one aspect of the present invention, it is possible to easily measure the rheology of various samples under high stress. [Brief explanation of the drawings]

[0008] [Figure 1] FIG. 1 is a schematic cross-sectional view showing a rheology measurement device according to a first embodiment of the present invention. [Figure 2] FIG. 1 is a perspective view illustrating a rheology measurement device according to a first embodiment of the present invention. [Figure 3] FIG. 1 is a diagram illustrating a rheology measurement device according to a first embodiment of the present invention. [Figure 4] FIG. 4 is a cross-sectional view showing a rheology measurement device according to a second embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0009] [Embodiment 1] An embodiment of the present invention will be described in detail below. Fig. 1 is a schematic cross-sectional view showing an example of a rheology measurement apparatus 10 according to embodiment 1 of the present invention. For ease of understanding, coordinate axes representing the X, Y, and Z directions are shown.

[0010] The rheology measuring device 10 is a device for measuring the rheological properties of the sample SA. Rheology refers to properties related to the viscosity, viscoelasticity, etc. of the sample SA. As will be described later, the rheology measuring device 10 can be used to apply a shear force in the plane direction (in FIG. 1, a direction parallel to the XY plane) to the film-shaped sample SA, allowing the sample SA to be observed.

[0011] Various techniques can be used to observe the sample SA. Examples include observations using electromagnetic waves, quantum beams, and probes. Examples of electromagnetic waves include electromagnetic waves with various wavelengths, such as X-rays, ultraviolet (UV) light, visible light, infrared light, and microwaves. In this case, the sample SA is irradiated with electromagnetic waves, and at least one of the electromagnetic waves that pass through the sample SA and the electromagnetic waves that are reflected by the sample SA is measured. Examples of quantum beams that can be used for observations include beams of neutrons, electrons, protons, and alpha particles. In this case, the sample SA is irradiated with a quantum beam, and at least one of the quantum beams that pass through the sample SA, the quantum beams that are reflected by the sample SA, and the secondary particles emitted from the sample SA as a result of the irradiation of the quantum beam is measured. The probe is a contact-type needle-shaped member. For example, when performing electrical measurements, such as electrical resistance, a metal probe is used. However, when performing measurements other than electrical measurements, the material of the probe is not limited to metal.

[0012] The sample SA is, for example, a solid in the form of a film or a liquid sandwiched between films M, and has a thickness of, for example, 10 μm or less. By reducing the thickness of the sample SA to, for example, 100 μm or less, or even 10 μm or less, the shear rate (stress) applied to the sample SA by the piezoelectric elements 13a and 13b can be increased. As a result, it becomes possible to measure the rheology of a variety of samples (e.g., low-viscosity liquids, high-viscosity liquids, and solids) under high stress.

[0013] The rheology measuring device 10 includes a stage unit 11, a presser unit 12, a piezoelectric element 13a, and a piezoelectric element 13b. The piezoelectric element 13a and the piezoelectric element 13b are examples of moving elements in one aspect of the present invention. Other examples of moving elements will be described later.

[0014] The stage unit 11 has a stage plate 111, a base unit 112, a fixing member 113, and a fixing member 114. The pressing unit 12 has a pressing plate 121, an end portion 122, and an end portion 123.

[0015] The stage unit 11 and the holding unit 12 are arranged opposite each other in a first direction (Z-axis direction) and function as first and second holding units that hold the sample SA. More specifically, the sample SA is placed on a stage plate 111 of the stage unit 11 and is held down by a holding plate 121 of the holding unit 12. The holding plate 121 can be screwed to the stage plate 111, for example, with a screw, and can press and lock the sample SA. The pressing force of the stage plate 111 can be adjusted by adjusting the screw (screw torque) to reduce the thickness of the sample SA. As described below, reducing the thickness of the sample SA can increase the shear rate on the sample SA.

[0016] In this way, the sample SA is placed on the stage unit 11 (stage plate 111) and pressed down by the presser unit 12 (presser plate 121). A solid in film form (for example, a thin film sample) can be placed directly on the stage plate 111 and pressed down by the presser plate 121. If the sample SA is a liquid, as shown in FIG. 1, the sample SA can be sandwiched between films M and sealed with a sealant SE, which makes it easy to place the sample on the stage plate 111 and press down with the presser plate 121. The sealant SE can be used to adjust the thickness of the sample SA.

[0017] Piezo element 13a and piezo element 13b are examples of moving elements that move at least one of the first and second clamping units (stage unit 11, pressing unit 12) in a second direction (X-axis direction) different from a first direction (Z-axis direction). Piezo element 13a and piezo element 13b are piezoelectric elements that use crystals that compress and expand when a voltage is applied to move (e.g., vibrate) an object (here, at least one of stage unit 11 and pressing unit 12). In addition to piezo elements, magnetostrictive elements can also be used as moving elements. Magnetostrictive elements move (e.g., vibrate) an object by using the attraction of a magnetic body due to electromagnetic force.

[0018] The direction of the force generated by the moving element to generate a shear force in the sample SA is a predetermined uniaxial direction (the X-axis direction in FIG. 1 ) among the planar directions of the sample SA. In this manner, when the moving element applies a uniaxial force to a portion of the sample SA, the portion of the sample SA moves along the uniaxial direction. As a result, a shear force is generated in the sample SA. In one aspect of the present invention, the movement includes (1) a movement (i.e., periodic vibration) that periodically expands and contracts the sample SA in both the positive and negative directions of the uniaxial direction (i.e., the positive X-axis direction and the negative X-axis direction), (2) a movement (i.e., a single reciprocating movement) that causes a single expansion or contraction in both directions (i.e., the positive X-axis direction or the negative X-axis direction), and (3) a movement (i.e., a single one-way movement) that causes a single extension or contraction in either the positive or negative direction of the two directions (i.e., the positive X-axis direction or the negative X-axis direction). Examples of periodic vibrations include vibrations based on sine wave or square wave signals. Examples of single-shot reciprocating movements include movements based on a single cycle signal of a sine wave or a square wave, a single signal having a delta function waveform, or a pulse wave signal. Examples of single-shot one-way movements include movements based on a single-step waveform. Controlling the piezoelectric element or magnetostrictive element with an appropriate signal enables movements in a variety of forms.

[0019] Here, the holding portion 12 (second clamping portion) is movable relative to the stage portion 11 (first clamping portion), and the piezoelectric element 13a vibrates the holding portion 12 (second clamping portion), i.e., the holding plate 121, relative to the stage portion 11 (first clamping portion), i.e., the stage plate 111.

[0020] The pressing unit 12 (second clamping unit) has an end 122. The rheology measuring apparatus 10 includes a fixing member 113. The fixing member 113 faces the end 122 and is fixed to the stage unit 11 (first clamping unit). The piezoelectric element 13a vibrates the end 122 in a second direction (X direction) relative to the fixing member 113.

[0021] The pressing unit 12 (second clamping unit) has a second end 123 located in the second direction (X direction) relative to the end 122. The rheology measuring device 10 is provided with a second fixing member 114 that faces the second end 123 and is fixed to the stage unit 11 (first clamping unit), and a second piezo element 13b that vibrates the second end 123 in the second direction (X-axis direction) relative to the second fixing member 114.

[0022] In the first embodiment, it is preferable that the vibrations PVa and PVb of the piezoelectric elements 13a and 13b are in opposite phases. That is, it is preferable that when the piezoelectric element 13a compresses, the piezoelectric element 13b expands, and when the piezoelectric element 13a expands, the piezoelectric element 13b compresses. In this way, both the piezoelectric elements 13a and 13b move the pressing unit 12 in the same direction (the positive direction of the X-axis or the negative direction of the X-axis), and it is possible to apply a large shear force between the piezoelectric elements 13a and 13b and the stage unit 11.

[0023] At least one of the stage unit 11 and the holder unit 12 (stage plate 111, holder plate 121, i.e., the first and second clamping units) has an opening. That is, in this example, the stage unit 11 and the holder unit 12 each have openings OP1 and OP2, but only one of the openings OP1 and OP2 may be provided. Even with only one of the openings OP1 and OP2, it is possible to irradiate the sample SA with electromagnetic waves or quantum beams and measure the reflected electromagnetic waves and particles. It is also possible to observe the sample SA using a probe. Incidentally, when both openings OP1 and OP2 are provided, it is possible to irradiate the sample SA with electromagnetic waves or quantum beams and measure the transmitted electromagnetic waves and particles. In this embodiment, the stage unit 11 and the holder unit 12 each have openings OP1 and OP2, respectively. Visible light, which is a form of electromagnetic wave, is irradiated onto the sample SA, and the visible light transmitted through the sample SA is measured. That is, this embodiment employs a configuration for optically observing changes in the physical properties of a liquid (sample SA) that are caused by high-speed, high-impact shearing.

[0024] ST1 and ST2 in Fig. 2 are perspective views of the rheology measurement apparatus 10. ST1 in Fig. 2 shows a state in which the stage plate 111 and the pressure plate 121 are closed, and ST2 shows a state in which the stage plate 111 and the pressure plate 121 are opened so that the sample SA can be set therein.

[0025] Fig. 3 shows a plan view and a cross-sectional view of the rheology measuring apparatus 10. D1 in Fig. 3 is a top view showing the rheology measuring apparatus 10 as viewed from the Z-axis direction. D2 in Fig. 3 is a cross-sectional view showing the rheology measuring apparatus 10 cut along line AA (X-axis direction) in D1, and D3 in Fig. 3 is a cross-sectional view showing the rheology measuring apparatus 10 cut along line BB (Y-axis direction) in D1. The explanation of these figures will be omitted as they overlap with the explanation of Fig. 1.

[0026] As described above, the rheology measuring device 10 holds the sample SA between the stage 11 and the holder 12, and vibrates one of the stage 11 and the holder 12 (here, the holder 12) relative to the other. By using a relatively thin sample SA, a large shear force can be applied to the sample SA at high speed. The piezoelectric element 13 can apply a relatively large force at high speed, and therefore can apply a high stress (here, a shear rate) at high speed to a variety of samples SA (measurement targets, for example, low-viscosity liquids, high-viscosity liquids, and solids).

[0027] The piezoelectric element 13 can apply vibrations with a frequency of about 20 kHz and an amplitude of about 50 μm. 5 ~10 7 A shear rate of [1 / s] can be applied. The thinner the thickness of the sample SA, the higher the shear rate can be.

[0028] The thickness of the sample SA is 10 μm, and a displacement of 10 μm is applied for 10 μs. 5 Furthermore, by setting the thickness of the sample SA to 100 nm, a shear rate of 10 7Shear rates of 1 / s can be achieved, which are 2 to 4 orders of magnitude higher than the shear rates achieved with conventional rheometers.

[0029] In this way, the rheology measurement device 10 can measure the rheology of a variety of samples SA, for example, solids (rubber, film, polymer) and liquids. Since a shear force is forcibly applied to the thin film sample SA, unlike the capillary method, the viscosity of the sample SA is not an issue. For liquids, up to 10 5 ~10 7 By applying a high shear rate of [1 / s] and a high shear stress of MPa to GPa, it is possible to optically observe the changes in the physical properties of a liquid (sample SA) due to high-speed, high-impact shear. It can also be used for impact testing of solid materials such as gels and rubber.

[0030] [Embodiment 2] Other embodiments of the present invention will be described below. For ease of explanation, the same reference numerals will be used to designate components having the same functions as those described in the above embodiment, and the description thereof will not be repeated.

[0031] FIG. 4 is a cross-sectional view showing a rheology measurement apparatus 10 according to a second embodiment of the present invention. The rheology measuring apparatus 10 according to the second embodiment includes a stage portion 11 (11a, 11b), a holding portion 12 (12a, 12b), piezoelectric elements 13a, 13b, and a base portion .

[0032] The stage parts 11a and 11b are movable relative to each other, and the holders 12a and 12b are movable relative to each other. The stage part 11a and the holder 12a are fixed to each other while sandwiching a part of the sample SA, and the stage part 11b and the holder 12b are fixed to each other while sandwiching another part of the sample SA.

[0033] Stage section 11 (first clamping section) has relatively movable stage sections 11a and 11b (first and second clamping elements), and holding section 12 (second clamping section) has relatively movable holding sections 12a and 12b (third and fourth clamping elements). Stage section 11a and holding section 12a (first and third clamping elements) are fixed to each other while clamping a portion of sample SA, and stage section 11b and holding section 12b (second and fourth clamping elements) are fixed to each other while clamping another portion of sample SA. Piezo element 13a vibrates the second and fourth clamping elements relative to the first and third clamping elements.

[0034] The pedestal 14 has a pedestal body 141, a fixing portion 142, and a fixing portion 143. The pedestal body 141 has an opening OP3. The opening OP3, in combination with the gap OP1 between the stage portions 11a and 11b and the gap OP2 between the holders 12a and 12b, facilitates observation of the sample SA with light. The ends of the stage portion 11a and the holder 12a face the fixing portion 142 and are subjected to vibration by the piezoelectric element 13a. The ends of the stage portion 11b and the holder 12b face the fixing portion 143 and are subjected to vibration by the piezoelectric element 13b.

[0035] In the second embodiment, unlike the first embodiment, it is preferable that the vibrations PVa and PVb of the piezoelectric elements 13a and 13b are in phase. That is, it is preferable that when the piezoelectric element 13a compresses, the piezoelectric element 13b compresses, and when the piezoelectric element 13a expands, the piezoelectric element 13b expands. In this way, the piezoelectric elements 13a and 13b can apply large pressures (compressive forces, expanding forces) between the first and third clamping elements and the second and fourth clamping elements.

[0036] (summary) The rheology measuring device (10) according to the first aspect is a rheology measuring device for measuring the rheological properties of a sample (SA), and comprises first and second clamping parts arranged opposite each other in a first direction and clamping the sample, and a moving element for moving at least one of the first and second clamping parts in a second direction different from the first direction.

[0037] A sample is clamped between first and second clamping parts arranged opposite each other in a first direction, and by moving at least one of the first and second clamping parts in a second direction different from the first direction, stress can be applied to the sample and rheology can be measured.

[0038] The rheology measuring device of the second aspect is the rheology measuring device of the first aspect, wherein the second clamping portion is movable relative to the first clamping portion, and the moving element moves the second clamping portion relative to the first clamping portion.

[0039] By moving the second clamping unit relative to the first clamping unit, a shear force can be applied to the sample, and the rheology can be measured.

[0040] A rheology measuring device (10) according to a third aspect is the rheology measuring device according to the second aspect, wherein the second clamping unit has an end, the rheology measuring device includes a fixed member that faces the end and is fixed to the first clamping unit, and the moving element moves the end in the second direction relative to the fixed member. By using the moving element to move the end of the second clamping unit relative to the fixed member that faces the end and is fixed to the first clamping unit, stress can be applied to the sample.

[0041] The rheology measuring device (10) according to the fourth aspect is the rheology measuring device according to the third aspect, wherein the second clamping portion has a second end portion located in the second direction relative to the end portion, and is provided with a second fixed member facing the second end portion and fixed to the first clamping portion, and a second moving element that moves the second end portion in the second direction relative to the second fixed member.

[0042] By using the second moving element to move a second fixed member that faces the second end of the second clamping portion and is fixed to the first clamping portion, a greater stress can be applied to the sample.

[0043] A rheology measuring device (10) according to a fifth aspect is the rheology measuring device according to the first aspect, wherein the first clamping unit has first and second clamping elements that are relatively movable, the second clamping unit has third and fourth clamping elements that are relatively movable, the first and third clamping elements are fixed to each other while clamping a portion of the sample, the second and fourth clamping elements are fixed to each other while clamping another portion of the sample, and the piezoelectric element moves the second and fourth clamping elements relative to the first and third clamping elements.

[0044] By moving the second and fourth clamping elements, which clamp a portion of the sample, relative to the first and third clamping elements, which clamp another portion of the sample, large compressive and tensile forces can be applied to the sample, allowing the rheological properties of the sample to be measured.

[0045] A rheology measuring device (10) according to a sixth aspect is the rheology measuring device according to any one of the first to fifth aspects, wherein at least one of the first and second clamping parts has a pair of openings that allow light in the first direction to pass through, enabling optical measurement of the sample.

[0046] The sample can be observed by irradiating it with electromagnetic waves or quantum beams through the opening, or by contacting a probe with the sample.

[0047] A rheology measuring device (10) according to a seventh aspect is the rheology measuring device according to any one of the first to sixth aspects, wherein the sample has a thickness of 100 μm or less.

[0048] When the sample has a thickness of 100 μm or less, a large stress, for example, a large shear rate, can be applied to the sample.

[0049] A rheology measurement device (10) according to an eighth aspect is the rheology measurement device according to any one of the seventh aspects, wherein the sample has a thickness of 10 μm or less.

[0050] When the sample has a thickness of 10 μm or less, a larger stress, for example, a larger shear rate, can be applied to the sample.

[0051] A rheology measuring device (10) according to a ninth aspect is the rheology measuring device according to any one of the first to eighth aspects, wherein the sample is a liquid sandwiched between membranes.

[0052] Large stresses, for example large shear rates, can be applied to the liquid.

[0053] A rheology measuring device (10) according to a tenth aspect is the rheology measuring device according to any one of the first to eighth aspects, wherein the sample has a film shape.

[0054] A large stress, for example, a large shear rate, can be applied to a sample in the form of a film.

[0055] The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope of the claims. Embodiments obtained by appropriately combining the technical means disclosed in different embodiments are also included in the technical scope of the present invention. [Explanation of symbols]

[0056] 10 Rheology measurement equipment 11, 11a, 11b Stage section 12, 12a, 12b holding part 13, 13a, 13b Piezo element 14, 112, base 111 Stage Plate 121 Presser plate 113, 114 Fixing member 122, 123 End OP1, OP2 opening

Claims

1. A rheology measurement device for measuring the rheological properties of a sample, comprising: first and second clamping units disposed opposite to each other in a first direction and clamping the sample; a moving element that moves at least one of the first and second clamping units in a second direction different from the first direction; A rheology measuring device comprising:

2. the second clamping unit is movable relative to the first clamping unit, The moving element moves the second clamping unit relative to the first clamping unit. The rheology measuring device according to claim 1 .

3. the second clamping portion has an end portion, the rheology measurement device includes a fixing member that faces the end portion and is fixed to the first clamping unit, The moving element moves the end portion in the second direction relative to the fixed member. The rheology measuring device according to claim 2 .

4. the second clamping portion has a second end portion positioned in the second direction relative to the end portion, a second fixing member facing the second end portion and fixed to the first clamping portion; a second moving element that moves the second end in the second direction relative to the second fixed member, The rheology measuring device according to claim 3 .

5. the first clamping unit has first and second clamping elements that are relatively movable; the second clamping unit has third and fourth clamping elements that are relatively movable; the first and third clamping elements are fixed to each other while clamping a portion of the sample; the second and fourth clamping elements are fixed to each other while clamping another part of the sample; The piezoelectric element moves the second and fourth clamping elements relative to the first and third clamping elements. The rheology measuring device according to claim 1 .

6. At least one of the first and second clamping portions has an opening. The rheology measuring device according to any one of claims 1 to 5.

7. The sample has a thickness of 100 μm or less. The rheology measuring device according to any one of claims 1 to 5.

8. The sample has a thickness of 10 μm or less. The rheology measuring device according to claim 7.

9. The sample is a liquid sandwiched between membranes. The rheology measuring device according to claim 7.

10. The sample has a film shape. The rheology measuring device according to claim 7.

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