JP6425116B2 - Viscosity and elasticity measuring device and viscosity and elasticity measuring method - Google Patents

Description

  The present invention relates to a viscosity / elasticity measuring apparatus and a viscosity / elasticity measuring method for measuring viscosity / elasticity which is a mechanical property of a substance.

Conventionally, in order to detect mechanical physical properties of a target substance, measurement of viscosity (also referred to as viscosity in the following description) or elasticity is performed (see, for example, Patent Document 1).
Viscosity and elasticity measurement, pharmaceutical, food, paint, ink, cosmetics, chemical products, paper, adhesive, fiber, plastic, beer, detergent, concrete admixture, silicon etc. in the manufacturing process, quality control, performance evaluation, raw materials It is an essential measurement technology for management and research and development.
The viscosimetry methods conventionally known include the following methods.

(1) viscosity tube method, (2) method of contacting vibrator, (3) method of using surface acoustic wave, (4) method of using rotor, (5) method of dropping rigid ball, (6) motion Light scattering method, (7) Zimm type viscosity measurement method, (8) EMS (Electro-Magnetically Spinning) viscosity measurement method, and (9) disk levitation type EMS viscosity measurement method.

Patent No. 5093599

However, among the methods described above, with regard to the method (1), many operations such as cleaning the inside of the glass capillary are required for measurement, and the maintenance of the glass viscometer is complicated. there were.
In addition, with regard to the methods (2) to (5), there is a drawback that the viscosity of the low viscosity material can not be measured because accurate measurement can not be performed unless the viscosity is at least 10 mPa · s (pascal second) or more. .
Furthermore, the method (6) has the disadvantage that the measuring apparatus becomes large-scaled, and the method can not be applied to other than transparent samples.

In addition, with regard to the methods (7) and (9), since the probe (rotor) floated on the surface of the sample (sample surface) by the buoyancy force is rotated, the energy loss for causing the sample surface to run out is neglected. There is a drawback that it can not be done. Also, with respect to the methods (7) and (9), when a molecular adsorption film is formed on the sample surface, there is a disadvantage that measurement errors occur due to the surface visco-elasticity of the film, and furthermore, the rotation causes the object to sink There is a constraint that the density of the sample material needs to be known in order to be dependent on the depth from the sample surface being measured.
Further, in all the methods (1) to (7), the sample container is expensive and needs to be used, so it is necessary to clean the sample container after measurement. In addition, if the previously measured sample is not completely removed by this washing, the influence of the immediately preceding sample substance remains, and there is a restriction that the measurement of the viscoelasticity of the sample substance to be measured can not be performed with high accuracy.

Further, the method of (8) has a disadvantage that the accuracy of viscosity measurement is limited by the mechanical friction between the lower part of the rotor and the sample container because the lower part of the rotor is in contact with the sample container. For example, when measuring the viscosity of a sample material having a low viscosity such as pure water, it is difficult to measure the viscosity with a precision higher than 1% due to the influence of mechanical friction. In the method of (8), when an inexpensive aluminum sphere is used as a rotor, since the aluminum sphere with the smallest diameter is 1 mm, theoretical pure viscosity is obtained as described in Patent Document 1 The measurement accuracy is limited to 10%.
In addition, the above-described visco-elastic measurement method generally used so far has a disadvantage that a certain amount or more of the sample material is required to obtain a certain accuracy.

In addition, there is a disadvantage that the measurement accuracy is degraded for sample substances whose viscosity is less than 10 mPa · s, and the device is too large to measure by a rotational viscometer or light scattering, and simple measurement can not be performed. There was a restriction.
For the reasons described above, in the method based on the conventional principle, there is a restriction that it is difficult to measure with a small amount of sample material with respect to universal physical quantities for sample materials such as liquids such as viscosity and elasticity and other soft materials. is there. In addition, in the method based on the conventional principle, it is difficult to measure with low accuracy sample substance with high accuracy, and as described above, it is necessary to completely clean the sample substance attached to the measurement sample container. There is also a restriction.

  The present invention has been made in view of such circumstances, and the amount of the substance of the sample to be detected is smaller than that of the conventional example, and the sample container for containing the substance to be detected is disposable and disposable. An object of the present invention is to provide a visco-elastic measurement device and a visco-elastic measurement method capable of measuring the viscosity of a sample material over a wide range from low viscosity to high viscosity.

In order to solve the problems described above, the viscosity / elasticity measuring apparatus of the present invention is partially or entirely made of a conductive material, and the disc is fixed so that the surface of the disc is perpendicular to the rotation axis. The rotor is formed in a convex shape, and the tip of the rotary shaft has a smooth convex shape, and a substance to be detected whose viscosity is to be detected is inserted, and the surface of the disc is detected. A sample container in which the rotor is disposed in contact with a target substance, a magnet disposed around the sample container for applying a magnetic field to the rotor, and a magnet for applying a dynamic magnetic field to drive the magnet. A time-varying magnetic field is applied to the rotor to induce an induced current in the disc of the rotor, and Lorentz interaction between the induced current and the magnetic field applied to the rotor causes the rotor to rotate. A rotation control unit for applying and rotating a torque, and a rotational speed of the rotor And a viscous elasticity detection unit for detecting the viscosity and elasticity of the detection target material in contact with the rotor according to the rotational speed of the rotor; It is characterized in that the radius is determined by using a sample of which viscosity or elasticity is known in advance by equation (14) described later.

  The apparatus for measuring viscosity and elasticity according to the present invention is characterized in that the convex portion of the axial tip of the rotation shaft of the rotor is in contact with the bottom of the inner surface of the sample container.

  A viscosity / elasticity measuring apparatus according to the present invention is a storage unit for storing standard data obtained by measuring in advance the relationship between the rotational torque applied to the rotor and the rotational speed of the rotor in a plurality of substances whose viscosity is known. Further, the viscosity / elasticity of the substance to be detected is determined by comparing the standard data with the relationship between the rotational torque and the number of rotations of the substance to be detected detected by the viscosity detection unit.

  The viscosity / elasticity measuring apparatus according to the present invention is characterized in that the rotor is marked, and the rotation detecting unit detects the rotation of the mark to detect the number of rotations of the rotor. .

  The viscosity / elasticity measuring apparatus according to the present invention detects the number of rotations of the rotor by irradiating a laser to the disk of the rotor and optically measuring a change in reflected light or an interference pattern thereof. It is characterized by

  The viscosity / elasticity measuring apparatus according to the present invention is characterized in that the bottom of the inner surface of the sample container in contact with the rotor is formed into a smooth flat surface or a smooth curved concave shape.

  The viscosity / elasticity measuring apparatus according to the present invention is provided with a lid for closing the upper opening of the sample container with respect to the sample container, and the rotating shaft of the rotor is a sample filled with the substance to be detected. It is characterized in that it is rotatably provided between the bottom of the inner surface of the sample container and the inner surface of the lid.

  In the viscosity / elasticity measuring apparatus of the present invention, the space inside the sample container is formed to be thicker in proportion to the distance from the rotation axis with respect to the diameter direction of the disc of the rotor. It is characterized by

In the viscosity / elasticity measurement method of the present invention, a sample container is filled with a detection target substance to be detected for viscosity and elasticity, and the detection target substance is partially or entirely made of a conductive material, and a disc In the rotor, the surface of the disc is fixed vertically to the rotation axis, and the tip of the rotation axis has a smooth convex shape, and the substance to be detected is the circle. The process of arranging so as to be in contact with the surface of a plate, and driving a dynamic magnetic field application magnet arranged around the sample container to apply a time-varying magnetic field to the rotor, and the disc of the rotor Induced torque is induced in the rotor and Lorentz interaction between the induced current and the magnetic field applied to the rotor is applied to rotate the rotor for rotation, and the number of rotations of the rotor is detected. Detection in contact with the rotor according to the process and the number of rotations And a viscosity detection step of detecting the viscosity and elasticity of the elephant substance radius of the disc of the rotor will be described later by equation (14), to be determined using samples of known beforehand viscous or elastic It features.

As described above, according to the present invention, viscosity and elasticity are measured from the relationship between the rotational torque applied to the rotor rotating in contact with the object to be detected and the number of rotations. The viscosity over a wide area can be measured by a simple device as compared to the prior art.
In particular, according to the present invention, the rotation of the rotor is inhibited by adjusting the weight of the rotor and the radius of the contact portion with the bottom of the sample container and the rotation radius of the rotor according to a predetermined equation. Since the effect of mechanical friction with other than the sample can be arbitrarily reduced and the measurement accuracy can be improved, highly accurate measurement can be performed.
Further, according to the present invention, a test tube or the like can be used as a sample container for containing an object to be detected, and a rotor capable of mass production can be adopted. It will be possible to disposable it to make work more efficient.

It is a schematic block diagram which shows the structural example of the viscosity * elasticity measuring apparatus by one Embodiment of this invention. FIG. 3 is a conceptual view of the sample container 2 for explaining the arrangement of the rotor 1 in the sample container 2 as viewed from the side. It is a top view which shows the fixed state of the magnet provided in order to generate the rotating magnetic field in the magnet fixed stand 7. FIG. FIG. 2 is a view showing a magnetic field generated by a magnet with respect to the rotary blade 12 with respect to the outer direction of the rotating rotary blade 12 from the rotation shaft 11 of the rotor 1; FIG. 17 is a diagram showing the relationship between the number of revolutions ΩM of the motor 150 and the number of revolutions ΩD of the rotor 110 for the corresponding standard sample in a plurality of standard samples having different viscosities. It is a figure which shows the electromagnet by which the yoke 10 and the teeth 10a, 10b, 10c and 10d which protruded from this yoke 10 were arrange | positioned on a reference | standard two-dimensional plane. It is a schematic diagram showing the new form of the sample container which fills the sample 100. FIG. It is a schematic diagram showing the other structure of the sample container which fills the sample 100. FIG. It is a schematic diagram showing the other structure of a rotor. It is a figure which shows the relationship between rotational speed (omega) M (namely, rotational torque) of the motor 4, and rotation angle (theta) which the floating rotor 1 stops. It is a figure which shows the relationship between elasticity and the ratio of a rotational speed and a rotation angle.

Hereinafter, a viscosity and elasticity measuring apparatus according to an embodiment of the present invention will be described with reference to the drawings. FIG. 1 is a schematic configuration view showing a configuration example of a viscosity / elasticity measurement apparatus according to an embodiment of the present invention.
In this drawing, the viscosity / elasticity measuring apparatus according to the present embodiment includes a rotor 1, a sample container 2, a first magnet 3_1, a second magnet 3_2, a third magnet 3_3, a fourth magnet 3_4, a motor 4, and a rotation detection sensor 5 , The sample stand 6, the magnet fixing stand 7, and the viscosity measurement unit 8.

  The rotor 1 is partially or entirely (whole) constituted of a conductor (for example, a metal material). The rotor 1 also has a rotary shaft 11 and a disk-shaped member, for example, a rotary wing 12 formed of a metal material. Further, in order to detect rotation (described later), the rotor 1 is provided with a mark of a size that can be detected by an imaging device or the like on any of its surface (the rotary wing 12 in the present embodiment).

  Further, only a part of the rotor 1 (especially, the part of the rotary wing 12) uses a conductor such as aluminum, and the other part can be made of a material such as plastic or vinyl. For example, a commercially available aluminum foil or the like may be attached to the upper surface of a plastic disk, for example, to form the portion of the rotary wing 12. Thus, the inexpensive rotor 1 can be easily formed from a commercially available plastic disc and a commercially available alum foil.

  The sample container 2 is composed of a sample container body 21 and a sample container lid 22. Further, the sample container 2 accommodates an object to be detected (hereinafter referred to as a sample) to be measured for measuring the viscosity (that is, the coefficient of viscosity) と し て as a mechanical physical property. Each of the sample container body 21 and the sample container lid 22 is made of, for example, a material such as glass or plastic. The sample container main body 21 is, for example, a cylindrical sample container such as a small petri dish. The inner diameter of the sample container body 21 may be slightly larger than the diameter of the rotor 12 in the rotor 1.

  The sample container lid 22 has a hole in its center part through which the rotation shaft 11 of the rotor 1 passes. In the sample container 2, the rotor 1 is disposed such that the rotor 12 is in contact with the sample 100 as a detection target, that is, part or all of the rotor 12 is submerged in the detection target. The sample container 2 can use a commercially available petri dish or the like made of glass or plastic for both the sample container body 21 and the sample container lid 22. For this reason, a disposable commercially available sample container can be used as the sample container in the sample container 2 and can be prepared inexpensively.

As described above, in the present embodiment, the rotor 1 and the sample container 2 can be inexpensive. For this reason, when a biomaterial or the like becomes the sample 100, the rotor 1 and the sample container 2 can be easily discarded even if a substance requiring special attention for its disposal is to be measured.
As a result, as with post-processing problems such as incineration and sterilization, it can be done as easily as disposal of other medical devices.

FIG. 2 is a conceptual view of the sample container 2 for explaining the arrangement of the rotor 1 in the sample container 2 as viewed from the side. FIG. 2A shows the side of a sample container for explaining the arrangement of the rotor 1 in the sample container 2. FIG.2 (b) has shown the enlarged view of the part of area | region A of Fig.2 (a).
The rotor holding portion 50 has a rotation shaft holding hole 51 through which the rotation shaft 11 passes so that the rotation shaft 11 of the rotor 1 faces the ground in the vertical direction.
The rotation shaft holding hole 51 is formed smoothly so that the inner surface in contact with the rotation shaft 11 is reduced in friction. Further, the rotary wings 12 of the rotor 1 are provided with marks 30 on the surface 12s.

Here, the effect of the gravity applied in the direction in which the rotation shaft 11 falls is extremely small as long as the rotation shaft 11 is substantially in the vertical direction, and the friction force at the contact portion between the rotation shaft 11 and the inner surface of the rotation shaft holding hole 51 is It can be ignored by the following argument.
That is, in the actual structure of the rotary shaft holding hole 51, the rotary shaft 11 rolls on the inner surface of the rotary shaft holding hole 51 by slightly increasing the inner diameter of the rotary shaft holding hole 51 than the diameter of the rotary shaft 11. Exercise. For this reason, the frictional force at the contact portion between the rotary shaft 11 and the inner surface of the rotary shaft holding hole 51 is mainly rolling friction, and the influence on the rotation of the rotary shaft 11 is even smaller.

Further, in the sample container lid 22, a through hole 22 h through which the rotation shaft 11 penetrates is provided at a position overlapping the rotation shaft holding hole 51 in plan view from the top.
In the bottom surface 21s of the inside of the sample container main body 21, a groove 21t is provided in which the lower portion 11e of the rotary shaft 11 of the rotor 1 is inserted. The groove 21 t is provided at a position overlapping with the through hole 22 h and the rotation shaft holding hole 51 in plan view from the upper surface.
The groove 21 t is smoothly formed so that the inner surface in contact with the lower portion 11 e of the rotary shaft 11 has a reduced friction. The lower portion 11 e of the rotary shaft 11 is inserted into the groove 21 t. Here, the lower portion 11e of the rotary shaft 11 is formed smoothly so that the lower surface in contact with the groove 21t is reduced in friction. Therefore, the frictional force at the contact portion between the inner surface of the groove 21t and the lower surface of the lower portion 11e of the rotary shaft 11 is mainly rolling friction, and the influence on the rotation of the rotary shaft 11 is even smaller.

In the sample container 2, the sample 100 is filled in a space sandwiched between the sample container main body 21 and the sample container lid 22. As a result, as the rotor 1 disposed in the sample container 2 rotates, shear flow occurs in the sample 100 sandwiched between the rotary wing 12 and the sample 100, and viscosity resistance to rotation of the rotor 1 is generated. Torque is generated. The viscous drag torque will be described later.
Further, in FIG. 2, the sample 100 is filled in the space sandwiched between the sample container body 21 and the sample container lid 22. However, when the sample 100 can not be prepared so as to be filled in the space between the sample container body 21 and the sample container lid 22, the lower surface of the rotary blade 12 may not be immersed in the sample 100 as a whole. The sample 100 may be inserted so that the whole contacts the liquid surface of the sample 100. In this case, the viscous drag torque, which decreases because the upper surface of the rotor 12 is not in contact with the sample 100, may be predicted from the filling state of the sample 100.

In addition, the rotor 1 rotates in a state where the lower portion 11 e of the rotation shaft 11 is inserted into the groove 21 t. Therefore, the distance between the lower surface of the rotary wing 12 and the bottom surface 21s inside the sample container main body 21 can be accurately maintained constant, and the shift speed of the rotary wing 12 in the sample 100 can be stably maintained. The accuracy of the 100 viscosity measurement is improved.
In FIG. 2, the sample container 2 filled with the sample 100 is provided on the top surface of the sample stand 6. At the lower part of the sample stand 6, a magnet fixing stand 7 to which a motor shaft 4a of the motor 4 is connected is provided in parallel with the sample stand 6. By rotating the motor shaft 4a of the motor 4, the magnet fixing base 7 is rotated. A first magnet 3_1 (third magnet 3_3) and a second sample 3_2 (fourth magnet 3_4) are provided on the top surface of the magnet fixing base 7.

  Returning to FIG. 1, the magnet fixing base 7 is a flat plate member for fixing a magnet that generates a rotating magnetic field. For example, each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet 3_4 is fixedly provided on the upper surface of the magnet fixing base 7. The magnet fixing base 7 is disposed in parallel with the rotary wing 12. Each of the first magnet 3 _ 1 and the second magnet 3 _ 3 is provided such that the S pole is in contact with the upper surface side of the magnet fixing base 7 and the N pole is opposed to the rotary wing 12. Each of the second magnet 3 _ 2 and the fourth magnet 3 _ 4 is provided so that the N pole is in contact with the upper surface side of the magnet fixing base 7 and the S pole is opposed to the rotary wing 12.

  Therefore, in each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet, magnetic poles of polarities different from the adjacent magnets are disposed to face the lower surface of the sample container 2. Further, each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet is a rectangular solid, and the upper surfaces are arranged in parallel with each other so that the heights of the upper surfaces are the same.

  FIG. 3 is a plan view showing a fixed state of a magnet provided for generating a rotating magnetic field in the magnet fixing base 7. FIG. 3A shows the arrangement of each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet. Each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet 3_4 is alternately arranged symmetrically with respect to the rotation axis of the magnet fixing base 7. On the other hand, FIG. 3B shows the arrangement of each of the fifth magnet 3_5 and the sixth magnet 3_6.

  In the present embodiment, although the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet are used, any number of magnets may be used as long as they can generate a rotating magnetic field. That is, although not shown, a plurality of (N, N = 2 n, n is an integer of n ≧ 1) small magnets are arranged along the rotation direction of the rotary wing 12 of the rotor 1 in the sample container 2. The magnetic poles on the top surface may be arranged to alternate between the N pole and the S pole. In addition, the magnet fixing table 7 may be disposed at the upper part of the sample container 2 so as to face the liquid surface of the sample 100 filled in the sample container 2 so that the upper surface of the permanent magnet is horizontal.

FIG. 4 is a view showing a magnetic field generated by a magnet with respect to the rotary wing 12 with respect to the outer direction of the rotating rotary wing 12 from the rotation shaft 11 of the rotor 1.
Here, the deflection angle theta, taking a point on the circular path 2 2, as the rotation axis z-axis and the point, from the x-axis in the two-dimensional coordinate system consisting of x-axis and y-axis, clockwise The rotation angle of the rotor 1 of FIG. Therefore, the deflection angle theta, increases from 0 2 [pi [rad], and it means that goes around circular path 2 2 This 2 [pi.

  That is, when the rotor 1 turns in the counterclockwise direction, it passes in the order of the first magnet 3_1 → the second magnet 3_2 → the fourth magnet 3_4 → the third magnet 3_3. At this time, the argument θ is from 0 to π / 2 to the arrangement region of the first magnet 3_1, from π / 2 to π, to the arrangement region of the second magnet 3_2, from π to 3π / 2, to the fourth magnet 3_4. And the arrangement region of the third magnet 3_3 from 3π / 2 to π.

In FIG. 4, the z-axis is the vertical direction of a plane (two-dimensional plane consisting of x-axis and y-axis) consisting of the surfaces of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet 3_4. It is a coordinate axis parallel to. Open arrows represent magnetic field vectors consisting of the magnitude and the direction of the magnetic field at any height z = z0.
Here, when the magnet fixing base 7 is rotated in the clockwise direction by the motor 4, each of the first magnet 3_1, the second magnet 3_2, the fourth magnet 3_4, and the third magnet 3_3 also rotates in the clockwise direction. In FIG. 4, each of the first magnet 3_1, the second magnet 3_2, the fourth magnet 3_4, and the third magnet 3_3 moves from θ from 0 to 2π, that is, to the right in the figure. .

  At this time, the magnetic field applied to the rotor 1 has components in the z direction and the θ direction. If the thickness of the rotor is sufficiently small compared to the diameter, the component in the θ direction of the magnetic field does not make a large contribution to the torque generated in the rotor. At the position of θ = 0, the z-direction component of the magnetic field is increasing in the + z direction, and around this position, Lorentz current flows clockwise from above, ie, from the + z direction. A torque acts on the current by the current, the magnetic field and the Lorentz interaction. Furthermore, as a total of torque contributions about the rotation axis applied to the entire rotor, the rotor produces torque that tends to rotate following the rotating magnetic field. The calculation of the magnitude of this torque will be described in detail later.

Returning to FIG. 1, the sample stand 6 is a flat plate member for fixing the sample container 2 in which the sample 100 is filled, and is disposed such that the upper surface thereof is parallel to the upper surface of the magnet fixing base 7.
Thereby, the rotor 1 is rotated in the sample 100 inside the sample container 2 when each of the rotary wing 12, the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet rotates. The upper surfaces of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet are parallel to the plane formed.
From the arrangement of each of the sample stand 6, the magnet fixing stand 7, the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet, the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and Each of the fourth magnets can generate a magnetic field in the direction perpendicular to the rotor 1 in the sample container 2 (or a magnetic field component that is perpendicular to the rotor 1).

The motor 4 is a drive mechanism for rotating the magnet fixing base 7 in the direction of the motor axis 4a perpendicular to the surface of the magnet fixing base 7, and fixed so that the motor axis 4a is perpendicular to the upper surface of the magnet fixing base 7. It is done.
Further, in plan view, the rotary shaft 11 of the rotor 1 is disposed at a position where the rotary wings 12 of the rotor 1 do not contact the inner wall of the sample container 2 and rotate in contact with the sample 100. A sample container 2 and a motor 4 are arranged.
That is, in plan view. The sample container 2 and the motor 4 are disposed at a position where the center of the bottom surface of the sample container 2 and the axial direction of the motor shaft 4 a of the motor 4 overlap.

In addition, a rotating magnetic field is applied to the rotary vanes 12 of the rotor 1 in the sample 100 filled in the sample container 2, and the magnet fixing base 7 is rotated by the motor 4 when rotating the rotating shaft 11 as a rotation center. . Thereby, each of 1st magnet 3_1, 2nd magnet 3_2, 3rd magnet 3_3, and 4th magnet rotates, and the rotating magnetic field is given with respect to rotary blade 12. At this time, the rotation shaft 11 of the rotor 1 may be shifted from the center of the bottom surface of the sample container 2 depending on the application state of the rotating magnetic field to the rotary wing 12.
Here, in plan view, the area of the bottom of the inside of the sample container 2 is made larger than the area of the rotor 12 of the rotor 1. Thereby, even if the rotation shaft 11 of the rotor 1 is offset from the center of the bottom surface of the sample container 2, the inner sidewall of the sample container 2 is not contacted. However, in order to make the sample container 2 large, the amount of the sample 100 to be filled in the sample container 2 necessary for the measurement of the viscosity 多 く is increased.

Therefore, as shown in FIG. 2, in the present embodiment, a smooth groove (concave portion) 21 t is provided in a part of the bottom surface 21 s of the sample container 2. By providing the groove 21t, the lower portion (convex portion) 11e of the rotation shaft 11 of the rotor 1 is disposed by gravity so as to center on the groove 21t and to be in contact with the groove 21t when the rotor 1 rotates. .
Moreover, it can fix by making the upper part of the rotating shaft 11 of the rotor 1 penetrate to the rotating shaft holding hole 51 of the rotor holding part 50, and it can suppress that the position of the rotor 1 and the rotating shaft 11 shift. . At this time, as described above, the resistance torque generated by friction at the contact portion between the rotation shaft holding hole 51 of the rotor holding portion 50 and the rotation shaft 11 of the rotor 1 is the axial direction of the rotation shaft 11 of the rotor 1 Is directed perpendicularly to the bottom of the sample container 2, the friction between the rotary shaft 11 and the inner surface of the rotary shaft holding hole 51 of the rotor holder 50 is rolling friction. Therefore, the friction between the rotary shaft 11 and the inner surface of the rotary shaft holding hole 51 of the rotor holding portion 50 is sufficiently smaller than the sliding friction, so the contribution to the rotational resistance of the rotor 1 is sufficiently small. Become.

In FIG. 1, the rotation shaft 11 of the rotor 1 has a bar-like shape, and the rotor holding portion 50 has a rotation shaft holding hole 51 surrounding the rotation shaft 11.
However, the present invention is not necessarily limited to this structure. For example, the rotating shaft 11 is configured as a cylinder, and the upper portion is opened to be configured as a pipe having a hollow hole. And it is good also as a structure which inserts the rod-shaped rotor holding | maintenance part 50 into the open hollow hole of the upper part of a rotating shaft, and rotates the rotor 1. FIG. In this case, in order to reduce mechanical friction generated by the contact of the inner surface of the hollow hole of the rotary shaft 11 with the rotor holding portion 50, lubricating oil may be filled in the hollow hole. Further, the lower portion 11e of the rotating shaft 11 is of a structure in which the cylinder is closed as already described in the present embodiment, and has a smooth shape in order to reduce mechanical friction with the groove 21t.

FIG. 5 is a view showing the relationship between the number of revolutions ΩM of the motor 4 and the number of revolutions ΩD of the rotor 1 for the corresponding standard sample in a plurality of standard samples having different viscosities η. In FIG. 5, the vertical axis indicates the rotation difference ΩMD between the rotation speed ΩM and the rotation speed ΩD (rotation speed ΩM−rotation speed ΩD), and the horizontal axis indicates the rotation speed ΩD of the rotor 1. The viscosity η of each standard sample used here is, for example, 0.5 (mP · s), 1.0 (mP · s), and 2.0 (mP · s), respectively. Then, from FIG. 5, the relationship between the rotational difference ΩMD and the rotational speed ΩD for each standard sample having different viscosity η, that is, the straight line indicating the correspondence of the inclination ΩD / ΩMD is determined by the least square method or the like. The slope ΩMD / ΩD is proportional to the viscosity η of each standard sample. At this time, the thickness of the rotor is 0.3 mm, the distance between the bottom of the sample container and the rotor, ie, the thickness of the sample is 1 mm, the distance between the edge of the rotor and the sample container is 5 mm. The amount of sample used is about 1.2 cc. In addition, although it is known in FIG. 5 that the relationship between the rotational speed ΩD and the rotational difference ΩMD is not correctly linear due to the influence of inertia, in order to show the ability to discriminate viscosity in the low viscosity region of the present invention. Straight lines are written as an eye guide.

  Returning to FIG. 1, the rotation detection sensor 5 is disposed at a position in the upper direction of the sample container 2 as a position where a mark provided on the surface of the rotor 12 of the rotor 1 in the sample 100 of the sample container 2 can be detected. The position of the mark on the surface of the rotary wing 12 (mark 30 in FIG. 2A) is optically detected. That is, the rotation detection sensor 5 emits a laser beam from the light irradiation unit, and the reflected light from the mark on the upper surface of the rotary wing 12 is incident on the light receiving unit, and outputs a detected electric signal corresponding to the intensity of the incident light.

  Also, instead of the rotation detection sensor 5, an imaging device in which an imaging device such as a lens and a CCD (Charge Coupled Device) is added to a microscope is provided, and the moving state of the mark on the rotary wing 12 of the rotor 1 is enlarged and imaged The captured image is output so that the number of rotations of the mark (ie, the number of turns of the mark of the rotary wing 12 and the number of turns of 1 when the mark (mark 30 in FIG. 2A) rotates once) is detected from image processing. It is good.

In addition, a laser is irradiated to the upper surface of the rotary wing 12 of the rotor 1 or the lower portion 11e of the rotary shaft 11, the reflection and interference pattern change due to the rotation are optically measured, and the rotational speed of the rotor 1 is calculated. It is good also as composition which detects.
In addition, a part of the rotary wing 12 of the rotor 1 is replaced with a dielectric, and the electrode pair in which the rotary wing 12 is sandwiched between the measurement electrodes is disposed at a position not obstructing the rotation of the magnet fixing base 7 such as FIG. Configure the capacitor. Then, the rotation detection sensor 5 detects a detection electric signal when a dielectric (for example, provided at the position of the mark 30 in FIG. 2A) as a mark for detecting rotation passes between the arranged electrodes. Output That is, when the dielectric as a mark passes between the electrodes, the rotation detection unit 81 detects a change in capacitance of the capacitor formed by the electrodes, and detects the number of times of this change in capacitance in a predetermined period (for example, one second). Alternatively, the rotational speed of the rotor 110 may be detected.

Here, when the magnet fixing base 7 is rotated by the motor 4, each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet 3_4 is rotated, and a rotating magnetic field as a time-varying magnetic field Is formed in the space on the top surface of the magnet holder 7.
The rotating magnetic field of the rotor 1 applies a torque to the rotors 12 by the rotating magnetic field to rotate the rotor 1 in the sample 100 in the sample container 2 to perform uniform rotational movement. And the method to measure viscosity (eta) of the sample 100 from the rotational speed in the sample 100 of the rotor 1 is demonstrated below.

The viscosity measurement unit 8 includes a rotation detection unit 81, a viscosity detection unit 82, a rotating magnetic field control unit 83, a standard data storage unit 84, and a device control unit 85.
The rotation detection unit 81 detects the rotation of the rotor 1 based on the detection electric signal supplied from the rotation detection sensor 5, and detects the number of detections per unit time (for example, one second) as the number of rotations per unit time (rpm The rotation speed ΩD is obtained and output as revolutions per minute). In addition, when detecting the number of rotations of the rotor 1, the rotation detection unit 81 does not use the detection electric signal of the rotation detection sensor 5 but uses a captured image of the imaging device, the imaging performed by the imaging device From the image, the mark of the rotary wing 12 of the rotor 1 may be detected by image processing to determine the number of revolutions ΩD per unit time. In addition, when the configuration of the capacitor is used, the rotation detection unit 81 detects a change in capacitance of the capacitor formed of the electrode pair from the detected electric signal, and detects the number of times of this change in capacitance in a predetermined period (for example, 1 second) Alternatively, the rotational speed ΩD of the rotor 1 may be detected.

Viscosity detection unit 82, as in the case of the standard samples described above, determine the slope ΩD / ΩMD (= ΩM-ΩD ) in the sample 10 0, we obtain the reciprocal .omega.MD / .omega.d of this inclination. At this time, the viscosity detection unit 82 controls the rotating magnetic field control unit 83 (described later) to rotate the motor 4 at a plurality of different rotational speeds ΩM, and controls the control signal as a rotation detection unit each time the number of rotations is changed. Output to 81 The rotation detection unit 81 inputs the rotation speed ΩD of the rotor 1 in the sample 100 placed in the sample container 2 at the rotation speed ΩM from the rotation detection sensor 5 each time the control signal is supplied from the viscosity detection unit 82. Then, the rotation detection unit 81 outputs the detected rotation speed ΩD to the viscosity detection unit 82 in response to the control signal.

  Then, the viscosity detection unit 82 reads the viscosity η (mP · s) corresponding to the reciprocal ΩMD / ΩD of the sample 100 from the viscosity detection table stored in the standard data storage unit 84 (to be described later). Output as the viscosity η (mP · s) of Here, when the empirical formula is stored in the standard data storage unit 84, the viscosity detection unit 82 reads the above empirical formula from the standard data storage unit 84, and substitutes the inverse of the slope ΩMD / ΩD for this empirical formula. Alternatively, the viscosity η (mP · s) of the sample 100 may be calculated and determined.

  The rotating magnetic field control unit 83 controls the rotation of the motor 4 so that the motor 4 rotates at the set rotation speed. Thereby, the magnet fixing base 7 is rotated via the motor shaft 4a, and the magnetic field generated by each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet 3_4 is rotated and rotated. A rotating magnetic field is generated to rotate the element 1 at the same speed in the sample 100.

The standard data storage unit 84 stores a viscosity detection table indicating the correspondence between the viscosity η (mP · s) obtained from the table in FIG. 5 and the reciprocal of the slope ΩMD / ΩD.
This viscosity detection table is created as follows. As described in FIG. 5, in the viscosity measurement device of the present embodiment, a standard sample whose viscosity is known in advance is put (filled) in the sample container 2, and the rotor 1 is put in the standard sample. When the motor 4 is rotated by the rotation speed ΩM of the rotation speed of the rotor 4, the rotation speed ΩD of the rotor 1 corresponding to the rotation speed ΩM of each motor 4 is measured by the rotation detection unit 81 described above. The measurement of the rotation speed ΩD with respect to this standard sample is performed with respect to a plurality of standard samples having different viscosity η (samples of which viscosity 粘性 is known in advance).
Further, instead of the viscosity detection table, an empirical equation indicating correspondence between the viscosity η (mP · s) and the inverse of the slope ΩMD / ΩD may be stored.
The device control unit 85 controls the operation of each unit in the viscosity measurement unit 8.

Next, a method of applying a rotational torque to the rotary wings 12 of the rotor 1 will be described. In FIG. 1, the magnetic field perpendicular to a reference plane (the plane including the rotary vane 12) by the N pole of the first magnet 3_1 and the fourth magnet 3_4 and the S pole of the second magnet 3_2 and the fourth magnet 3_3. Occurs. This reference plane is taken as a reference two-dimensional plane consisting of an x-axis and a y-axis, and the axial direction of the rotational axis 11 of the rotary wing 12 of the rotor 1 rotating in this two-dimensional plane is taken as the z-axis.
Hereinafter, the z-axis component of the magnetic field in the reference two-dimensional plane or a point (x, y, z) in the vicinity thereof will be denoted as Bz (x, y).

As described above, since the magnetic field is perpendicular to the reference two-dimensional plane, it is assumed that it does not depend on the z-axis, but depending on the z-axis, the following explanation will not be disturbed. In addition, if there is a component of the magnetic field perpendicular to the reference two-dimensional plane, even if there is another component of the magnetic field not perpendicular to the reference two-dimensional plane, the rotational torque with respect to the rotary wing 12 of the rotor 1 It does not interfere with giving.
In the following description, the rotor 12 is formed of metal, and the rotational torque applied to the rotor 12 is calculated. Also, for convenience, at first, orthogonal coordinates are adopted, with the vertically upper side of the rotary wing 12 as the + z direction, the rotary wing 12 rising on the xy plane, and the center of the rotary wing 12 (rotation axis 11 and rotary wing 12 Point of intersection) as the origin. Furthermore, the rotating magnetic field generated by the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet 3_4 by the rotation of the magnet fixing base 7 is expressed by the following equation (1).

In the above equation (1), r represents the distance from the rotation axis, B _z represents the magnetic field in the z-axis direction, B (r) represents the magnetic field in the rotation radial direction, ω represents the rotational angular velocity, and t represents The time is shown, n is the number of sets of magnets, and θ is the rotation angle of the magnet holder 7. In the case of the present embodiment shown in FIG. 1, n is 2 because the magnetic pole facing the sample table 6 has two sets of magnets of N pole and S pole.
Further, the electric field E generated by the time-varying magnetic field B is given by the following equation (2). The magnetic field B and the electric field E are vectors.

In the equation (2), it is assumed that the magnetic field B has a magnetic field _Bz of only the z-direction component, but the following argument holds even if there is a component other than the z-axis direction.
The current vector i flowing in the conductive disk-shaped rotor 12 in the rotor 1 is i = σE, where σ is the conductivity. i and E are vectors. Since the divergence is "0" for the current vector i, div i = 0. Therefore, for the electric field E, there exists a vortex potential φ satisfying the following equation (3).

In the above (3), E _x denotes an electric field in the x-axis direction in the two-dimensional coordinate system, E _y represents the electric field in the y-axis direction in the two-dimensional coordinate system.
The equation (3) is substituted into the equation (2) to obtain the following equation (4).

  The following equation (5) is obtained by the equations (2) and (4).

  When the equation (5) is expressed by a specific expression of a magnetic field, it is expressed as the following equation (6).

  In the above equation (6), B (r) represents a magnetic field in the rotational radius direction, ω represents a rotational angular velocity, t represents time, n represents the number of magnet pairs, and θ represents The rotation angle is shown, and φ shows the eddy potential.

  The following equation (7) is obtained from the equation (6).

In the above equation (7), J _n (kr) represents a Bessel function of the first kind, k represents an integral variable at the time of performing the integration of equation (7), r represents a radius of gyration, , T indicates time, and θ indicates the rotation angle of the magnet holder 7.
Further, in the equation (7), the coefficient A (k) is a Hankel transform coefficient of B (r), and is expressed by the following equation (8).

  The following description transitions from a three-dimensional coordinate system to a cylindrical coordinate system. The electric field Er in the radial direction and the electric field Eθ in the radial direction are respectively obtained from the electric field Ex and the electric field Ey obtained by the equation (3), and can be expressed as the following equation (9). In the equation (9), θ indicates the rotation angle of the magnet holder 7 and r indicates the rotation radius.

In the above equation (9), considering the Lorentz interaction between the electric field and the magnetic field, the total integral of the radial component of the Lorentz force is trivially zero due to the symmetry.
Also, the component in the radial direction is given by F _θ = σE _r B _z . The component of this radial direction is represented by the following (10) Formula by (7) Formula and (9) Formula. In equation (10), ω represents the rotational angular velocity, θ represents the rotation angle of the magnet holder 7, n represents the number of sets of magnets, and the coefficient A (k) represents the Hankel transform coefficient of B (r) In the figure, J _n (kr) indicates a Bessel function of the first kind, k indicates an integral variable when performing the integration of Equation (7), and r indicates a radius of gyration.

In the above equation (10), the radial distribution of the magnetic field can be approximated by the Bessel function for the sake of simplicity. That is, when B (r) = B ₀ J _n (kr), the torque T that the rotating magnetic field applies to the rotary vanes 12 can be obtained by the following equation (11). Here, B ₀ indicates the strength of the magnetic field. In equation (11), n represents the number of sets of magnets, ω represents the rotational angular velocity, B ₀ represents the integral variable when performing the integration of equation (7), and J _n (kr) represents the first Seed Bessel function.

As described above, it has been found that the torque T acts on the rotary wings 12 of the rotor 1 by the rotating magnetic field. In an actual viscosity / elasticity measuring apparatus, the rotor 1 rotates in the sample 100 by the torque T acting on the rotary wing 12, so the rotation speed ΩM of the rotating magnetic field in the above is the rotation speed ΩM of the magnetic field and the rotation The rotational speed difference of the rotor 1 is replaced with the rotational speed difference ΩM-ΩD, which is the difference between the rotational speeds.
As a result, when the eddy current generated in the conductor of the rotary wing 12 of the rotor 1 receives rotational torque (torque T), the rotary torque T is applied to the rotary wing 12 of the rotor 1 . As a result of the rotational torque being applied to the rotary wings 12 of the rotor 1, the rotor 1 rotates in the direction in which the rotational torque T is applied in the sample 100.

In addition, as the rotor 12 rotates, a viscous drag torque due to shear flow corresponding to the viscosity η of the sample 100 is applied to the rotor 12. Because of this viscous drag torque, the rotation speed ΩD of the rotor 1 does not reach the rotation speed ΩM of the magnetic field because it is proportional to the viscous drag torque.
Accordingly, the magnitude of the rotational torque T applied to the rotary wings 12 of the rotor 1 is proportional to the difference between the rotational speed ΩM of the rotational magnetic field (similar to the rotational speed of the motor 4) and the rotational speed ΩD of the rotor 1 It will be done. That is, when the rotation speed ΩD of the rotor 1 becomes constant, the constant rotation speed ΩD has an inverse proportion to the viscosity η of the sample 100.

As described above, the rotational torque T applied to the rotor 12 of the rotor 1, the rotational speed ΩD of the rotor 1 rotating in the sample 100, the radius r of the rotor 1, the rotor 12 and the sample container It can be seen that the thickness の 間 of the sample 100 can be determined from the thickness between the bottom of the inner surface of the main body 21 and the thickness between the rotary wing 12 and the sample container lid 22.
Here, in the measurement of the viscosity η of the sample 100, the rotational torque T applied to the rotary vanes 12 of the rotor 1 is as shown in FIG. 5 already described using a standard sample of which the viscosity 判 っ is known in advance. It is determined as a function of the rotational speed difference ΩMD between the rotational speed ΩM of the rotating magnetic field and the rotational speed ΩD of the rotor 1.

In the case where the sample 100 is filled only from the rotor 12 to the lower space, that is, when the sample 100 is filled only between the bottom of the inner surface of the sample container body 21 and the lower surface of the rotor 12, It contacts only the lower surface of 12.
For this reason, when creating the viscosity detection table shown in FIG. 5, it is necessary to measure the standard sample under the same conditions.
In addition, if the density of the sample 100 whose viscosity η is to be measured is known in advance, an appropriate sample that has a uniform depth when the sample 100 is inserted into the sample container 2 of the common size corresponding to the density of the sample 100 Weigh an amount of 100 by a scale. This processing makes it possible to make the depth of the sample 100 put into the sample container 2 at the time of measurement uniform for every sample 100 with different density.

Here, the accuracy of the viscosity measurement in the viscosity / elasticity measurement apparatus of the present embodiment will be described. In the viscosity / elasticity measurement apparatus of the present embodiment, a known torque T is remotely applied to the rotary vanes 12 of the rotor 1 by the time-varying magnetic field (rotational magnetic field of rotation number ΩM), and the rotation number ΩD The viscosity η of the sample 100 which is the target substance is measured by detection.
The torque T to be applied to the rotary wings 12 of the rotor 1 may be obtained from the magnitude of the applied magnetic field by the above equation (11). Alternatively, it may be determined in advance by measurement using a standard sample having a known viscosity η. In principle, the determination accuracy of the magnitude of the torque T determined from this can be arbitrarily improved, and in practice it can be determined with an accuracy of 0.1% or more.

On the other hand, the factors determining the rotation speed ΩD of the rotor 1 include the lower portion 11e of the rotation shaft 11 of the rotor 1 and the bottom surface 21s inside the sample container body 21 as well as the viscosity η of the sample 100 to be detected. And rotational torque T _f due to mechanical friction at the contact portion of It is also theoretically calculated and experimentally verified that this rotational torque T _f is an extent indicated by the following equation (12).

  In the above equation (12), M represents the weight of the rotor 1, ρ represents the specific gravity of the sample 100, V represents the volume of the part sunk in the sample 100 of the rotor 1, and g represents gravitational acceleration. μ denotes the dynamic friction coefficient between the lower portion 11e of the rotary shaft 11 and the bottom surface 21s of the sample container body 21, Rc is the contact radius of the contact portion between the lower portion 11e of the rotary shaft 11 of the rotor 1 and the bottom surface 21s of the sample container body 21 Is shown.

Further, the rotor blades 12 of the disc-shaped radius R on the rotor 1, with respect to the thickness (depth) samples 100 d, the rotational angle velocity at the upper surface (the surface in contact with the rotating blades 12) omega, the lower surface ( The torque T VIS required to apply the distortion that makes the rotational angular velocity 0 at the surface contacting the bottom surface 21 s of the sample container body 21 is calculated by the following equation (13).

  In the above equation (13), Rc represents the contact radius of the contact portion of the lower portion of the rotor with the container bottom, M represents the weight of the rotor 1, and V represents the volume of the portion sunk in the sample 100 of the rotor 1 Indicates the specific gravity of the sample 100, g indicates the gravitational acceleration, R indicates the radius of gyration of the rotor 1, η indicates the viscosity of the sample 100 to be detected, and μ indicates the rotation of the rotor 1 The dynamic friction coefficient between the lower portion 11e of the shaft 11 and the bottom surface 21s of the sample container body 21 is shown, and d is the thickness of the sample 100 sandwiched between the rotary wing 12 of the rotor 1 and the bottom surface 21s of the sample container body 21 .

Also, let α be the required viscosity and elasticity measurement accuracy. For example, when the required measurement accuracy α is 1%, α = 0.01. If the rotational torque T _f obtained from the equation (12) is smaller than α times the torque T _VIS obtained from the equation (13), that is, if the following equation (14) holds, the required measurement accuracy α is obtained be able to. The torque T _VIS due to the viscosity of the sample 100 is superior to the torque T _f of mechanical friction due to the contact between the rotor 1 and the bottom surface 21s of the sample container main body 21 by 1 / α or more, thereby making the accuracy α Viscosity measurement of

The measurement accuracy α is about 10% in the conventional method, but more preferably about 1%. Furthermore, it is desirable that about 0.1%, which is a difficult accuracy with the conventional method, be obtained.
As described above, according to the present embodiment, the amount of the sample 100 which is a substance to be detected can be reduced as compared with the conventional measurement.
Further, according to the present embodiment, each of the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet 3_4 that generates the rotating magnetic field is in the lower direction of the sample stand 6 in which the sample container 2 is disposed. It is possible to reduce the size of the visco-elastic measurement device compared to the prior art.

  Further, in FIG. 1, a combination of a first magnet 3_1, a second magnet 3_2, a third magnet 3_3, and a fourth magnet 3_4 is used as a magnet that generates a rotating magnetic field. In this case, in a plan view, a rotating magnetic field is generated by a combination of two pairs in which two N poles and two S poles are alternately arranged. On the other hand, according to the equation (11), the number of sets of magnets for applying torque to the rotary wings 12 of the rotor 1 may be one or more arbitrarily, for example, two square magnets in plan view, The S pole and the N pole may be arranged alternately.

In addition, the magnet fixing base 7 described above is rotated, and a rotating magnetic field is generated using an electromagnet instead of generating a rotating magnetic field by the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet 3_4. It is good also as composition.
FIG. 6 is a view showing an electromagnet in which the yoke 10 and the teeth 10a, 10b, 10c and 10d protruding from the yoke 10 are disposed on a reference two-dimensional plane. The winding CL1 is wound around the teeth 10a and 10c in different winding directions, and the winding CL2 is wound around the teeth 10b and 10d in the winding directions different from each other to constitute an electromagnet.
Instead of generating the rotating magnetic field from the magnetic field emitted by the first magnet 3_1, the second magnet 3_2, the third magnet 3_3 and the fourth magnet 3_4 which are permanent magnets, the magnet fixing base 7 is rotated by the motor 4 in FIG. The rotating magnetic field may be generated using the configuration of the electromagnet shown in FIG. 6 described above.

That is, current is supplied to the windings CL1 and CL2, a magnetic field perpendicular to the reference two-dimensional plane is generated, the direction of the flowing current is periodically changed, and the magnetic field perpendicular to the reference two-dimensional plane is generated. It may be rotated to form a rotating magnetic field. That is, the respective electromagnets are driven such that each of the electromagnets arranged on the circumference has a different polarity from that of the other adjacent electromagnets. When driving the electromagnets, the rotating magnetic field may be generated by changing the polarity of each electromagnet temporally.
In this case, the rotating magnetic field control unit 83 applies a current to the windings CL1 and CL2 of the electromagnets of FIG. 6, and periodically changes the direction of the flowing current to generate a rotating magnetic field.
As in the case of using a magnet, torque is applied to the rotor 12 of the rotor 1 by this rotary magnetic field, and the rotary motion of the rotor 12 is performed around the rotary shaft 11 within the sample 100. The viscosity η of the sample 100 is determined.

In addition, the rotating magnetic field control unit 83 may arbitrarily change the rotation period and the rotation direction of the rotating magnetic field to be applied to the rotary wings 12 of the rotor 1.
For example, by periodically sweeping the rotating direction of the rotating magnetic field and the rotating speed, it is possible to give the rotor 1 a rotating torque that changes periodically.

FIG. 7 is a schematic view showing another configuration of the sample container in which the sample 100 is filled. According to the embodiment shown in FIG. 7, the cross section of each of the sample container main body 201 and the sample container lid 202 constituting the sample container 200 has a triangular shape. That is, the cross section of each of the sample container body 201 and the sample container lid 202 is formed to be thinner in thickness from the central portion toward the outer peripheral portion.
Thereby, the thickness of the sample 100 sandwiched between the rotary wing 12 and each of the bottom surface 201s of the sample container body 201 and the sample container lid 202 increases in proportion to the distance from the rotation shaft 11 of the rotor 1 . Thereby, uniform shear rate deformation can be realized everywhere in the sample 100 filled in the sample container 200. Therefore, the configuration of the sample container 200 is effective for measuring the viscosity and elasticity of a non-Newtonian fluid whose viscosity value changes with shear rate. The mark 19 is a mark for detecting the rotation of the rotating shaft 11.

FIG. 8 is a schematic view showing another configuration of the rotor and the sample container in which the sample 100 is filled. In FIG. 8, the rotor 401 includes a rotary wing 412 and a convex portion 411 as a rotational axis of the rotary wing.
Further, the sample container 420 includes a sample container main body 421 and a sample container lid 422. The sample 100 is filled in an internal space formed by each of the sample container main body 421 and the sample container lid 422. The entire bottom surface 421s of the inside of the sample container main body 421 is flat. That is, in the bottom surface 421s of the sample container main body 421 in FIG. 9, a groove such as the groove 21t for inserting the rotation shaft 11 of the rotor 1 shown in FIG. 2 is not provided.

In the rotor 401, the rotary wing 412 is a disk-like member, and a convex portion 411 is provided at the center of the lower surface 412s facing the bottom surface 421s of the sample container main body 421.
The bottom 411e of the convex portion 411 of the rotor 401 in contact with the bottom surface 421s of the sample container main body 421 is the lowermost point of the convex portion 411, and is formed in a smooth shape to reduce mechanical friction on the contact surface. ing. The radius of curvature of the region where the bottom 411e of the convex portion 411 contacts the bottom surface 421s of the sample container main body 421 is RT.
Further, in the state of being sunk in the sample 100, the distance between the gravity center position RG in consideration of the buoyancy of the rotor 401 and the bottom portion 411e of the convex portion 411 of the rotor 401 is h. The convex portion 411 of the rotor 401 is configured such that the condition of RT <h is satisfied.

When the above condition is satisfied, the rotor 401 makes contact with the bottom surface 421 s of the sample container main body 421 with the bottom portion 411 e of the convex portion 411 in contact with the bottom surface 421 s (plane) of the sample container main body 421. The attitude to keep level is stable. That is, only by disposing the rotor 401 in the state of being sunk in the sample 100, the rotary wing 412 and the bottom surface 421s of the sample container main body 421 can be maintained in parallel and in the horizontal plane.
For this reason, it is not necessary to finely adjust the attitude of the rotor 401, and it becomes possible to make the shear speed in the whole of the sample 100 stable and uniform, and to measure the viscosity and elasticity with high accuracy. Further, there is no need to provide the rotary shaft holding hole 51 of the rotor holding portion 50 for inserting the rotary shaft 11 in the configuration of FIG. 2 to stabilize the rotation of the rotor 1 and to reduce extra mechanical contact. It is possible to expect to improve the measurement accuracy. Moreover, since it is not necessary to provide the rotor holding | maintenance part 50, the structure of a viscosity * elasticity measuring apparatus can be simplified.

FIG. 9 is a schematic view showing another configuration of the rotor. In FIG. 9, the sample container 20 has the same configuration as that of FIG. The rotor 1A has a structure in which a member 11m is provided on the upper portion 11t of the rotation shaft 11 of the rotor 1 of FIG. The member 11m is formed of a magnetizable material.
Further, a rotor holding portion 600 is provided at an upper portion in the axial direction of the rotary shaft 11 with a gap of a predetermined distance so as to face the member 11m. The rotor holding portion 600 is formed of a magnet. Therefore, the rotor holding portion 600 applies a force to pull up the member 11m, that is, the rotor 1A. Here, the rotor holding portion 600 and the groove portion 21t formed on the bottom surface 21s of the sample container main body 21 are provided at overlapping positions in plan view. As a result, the rotating shaft 11 is kept in the vertical direction since a force that is always pulled upward acts. Further, the lower portion 11e of the rotary shaft 11 and the inner surface of the groove 21t formed on the bottom surface 21s of the sample container main body 21 are formed smoothly so as to reduce mechanical friction in contact.

The rotor 1A keeps the rotary wing 12 horizontal to the bottom surface 21s of the sample container body 21 in a state where the lower portion 11e of the rotary shaft 11 is in contact with the inner surface of the groove 21t of the bottom surface 21s of the sample container body 21. Becomes stable. That is, only by disposing the rotor 1A in the state of being sunk in the sample 100, the rotary wing 12 and the bottom surface 21s of the sample container main body 21 are maintained in parallel and in the horizontal plane.
For this reason, there is no need to provide the rotary shaft holding hole 51 of the rotor holding portion 50 for inserting the rotary shaft 11 in the configuration of FIG. 2 and stabilizing the rotation of the rotor 1 in order to hold the posture of the rotor 1A. As a result, it is possible to reduce excessive mechanical contact with the rotor 1A, and it is possible to realize the measurement of viscosity and elasticity with high accuracy. Moreover, since it is not necessary to provide the rotor holding | maintenance part 50, the structure of a viscosity * elasticity measuring apparatus can be simplified.

Next, measurement of elasticity using the viscosity / elasticity measurement apparatus according to the present embodiment will be described. The viscosity and elasticity measuring apparatus having the configuration of FIGS. 1 and 2 will be described.
According to the present embodiment, the viscosity is not determined as in the liquid, but a substance having an elastic modulus such as gel or rubber, or a substance such as a polymer solution in which the elastic modulus is generated due to the relaxation of viscosity, It is possible to simultaneously measure the viscosity and the modulus of elasticity due to the displacement from the rest position when a constant torque is applied.

Here, the elastic modulus is a so-called spring constant, and corresponds to a restoring force proportional to the rotational deformation of the sample 100.
Therefore, when there is elasticity in addition to viscosity, the restoring force by the elastic modulus increases in proportion to the degree of strain. For this reason, after starting to rotate, the rotor 1 stops rotation at a rotation angle θ at which the elastic force proportional to the spring constant of the sample and the rotation torque by the rotating magnetic field are balanced. As described above, the counterclockwise rotation torque is applied to the rotor 1 in the sample 100 as the magnet fixing base 7 rotates counterclockwise.

Then, the rotation of the floating rotor 1 is stopped at the position of the rotation angle θ at which the rotational torque applied to the rotor 1 and the repulsive force due to the elasticity are balanced.
Here, in the rotation detecting unit 81, the motor 4 is not rotating, and the motor 4 is rotated at a predetermined rotation speed ΩM and the position of the mark 30 of the rotary wing of the rotor 1 when the magnet fixing base 7 is stopped. After that, the rotation angle θ is obtained from each captured image with the position of the mark 30 when the rotation is stopped. The elasticity can be determined from this angle θ.

FIG. 10 is a view showing the relationship between the rotational speed ΩM of the motor 4 (ie, the rotational torque) and the rotational angle θ at which the rotor 1 stops. In FIG. 10, the horizontal axis indicates the rotation speed ΩM of the motor 4 and the vertical axis indicates the rotation angle θ at which the rotor 1 stops.
That is, in the case of the viscosity / elasticity measuring apparatus shown in FIGS. 1 and 2, the first magnet 3_1, the second magnet 3_2, and the second magnet 3_2 disposed on the magnet fixture 7 when the magnet fixture 7 is rotated by the motor 4. Magnets of the third magnet 3 _ 3 and the fourth magnet 3 _ 4 generate a rotating magnetic field corresponding to the rotation speed of the motor 4.

  Then, the rotating magnetic field control unit 83 changes the rotational speed of the motor 4 in accordance with preset steps, obtains the rotational angle θ for each rotational speed, and obtains the relationship between the rotational speed ΩM and the rotational angle θ Create the graph shown in 10. Here, the processing described above is performed on a plurality of standard samples whose elasticity is known in advance, in order to create standard data used for measuring the elasticity of the sample 100 whose elasticity is unknown, like the viscosity. As in the preparation of the viscosity standard data, a standard sample is placed in the sample container 2 and the above-described measurement of the rotation angle θ is performed.

FIG. 11 is a diagram showing the relationship between the elasticity and the ratio of the rotational speed and the rotational angle. The horizontal axis is elastic (modulus of elasticity: Pa) 1 1 and the vertical axis represents the proportional coefficient between the rotational speed ΩM rotation angle theta. Here, the viscosity is inversely proportional to the rotation angle θ.
This FIG. 11 is standard data of elasticity used for elasticity measurement created by correlating the inclination of each standard sample in FIG. 10 (the ratio between the rotational speed Ω M and the rotation angle θ) and the viscosity of the corresponding standard sample. is there.
In the measurement of the sample 100 of the actual unknown elasticity, the sample 100 to be measured is put in the sample container 2, and the rotating magnetic field control unit 83 rotates the motor 4 at a preset rotation speed as in the case of the standard sample. .

Then, the rotation detection unit 81 obtains a rotation angle θ for each rotation speed, and outputs the rotation angle θ to the viscosity detection unit 82.
The viscosity detection unit 82 obtains a proportionality coefficient between the rotation speed ΩM supplied from the rotation detection unit 81 and the rotation angle θ, and reads data of elasticity corresponding to the proportionality coefficient from the standard data of the standard data storage unit 84, The read data is output as the elasticity of the sample 100.

It is also possible to measure elasticity and viscosity simultaneously by temporally changing the rotational torque applied to the rotary wings 12 of the rotor 1. In this case, a magnet that generates a rotating magnetic field is configured by an electromagnet shown in FIG.
For example, after applying an excitation current to the electromagnet and applying a predetermined rotational torque to the rotary vanes 12 of the rotor 1, the application of the excitation current is stopped and the rotation state of the rotor 1 after being stopped Observe.

At this time, the rotor 1 causes rotational vibration according to the elasticity of the sample 100 in contact with itself. Here, the period and the vibration time of the rotational vibration are proportional to the elasticity, and the damping rate of the amplitude of the rotational vibration is proportional to the viscosity.
Therefore, for each of a plurality of standard samples of which viscosity and elasticity are known in advance, applying a rotational magnetic field to the rotary wing 12 of the rotor 1 with the attenuation rate of the amplitude of the rotational vibration and the period and vibration time. The standard data is prepared and stored in advance in the standard data storage unit 84.

Next, when measuring a substance to be measured having an actual unknown viscosity and elasticity, the viscosity detection unit 82 is a rotor for the attenuation factor of the amplitude of the sample 100 which is the substance to be measured, and the period and vibration time. The viscosity corresponding to the attenuation factor of the measured amplitude and the elasticity corresponding to the period and the vibration time are read out from the standard data of the standard data storage unit 84, respectively.
Then, the viscosity detection unit 82 outputs the viscosity and elasticity read from the standard data as the viscosity and elasticity of the sample 100 to be measured.
As described above, according to the present embodiment, it is possible to simultaneously measure the viscosity and elasticity of the sample 100 simultaneously.

Also, by periodically sweeping the rotational direction of the rotating magnetic field applied to the rotor 12 of the rotor 1 and the rotation torque (rotational speed Ω M of the motor 4), the rotor 1 of the rotor 1 is periodically scanned. Torque can be applied.
Then, while changing the cycle of sweeping the rotational direction and the rotational torque, the amplitude and phase of the rotational vibration of the rotor 1 are observed from the captured image obtained by imaging the mark 30 of the rotary wing 12. It is possible to measure elasticity independently.
That is, the observation of this rotational vibration is to detect the damped vibration after erasing the magnetic field as a frequency spectrum as described above, and is in principle similar to the measurement of viscosity and elasticity after erasing the magnetic field. .

Next, a specific application example of the viscosity / elasticity measuring apparatus (mechanical physical property measuring apparatus) shown in FIG. 1 will be described.
The inner diameter of the sample container body 21 was 40 mm, and a glass petri dish with a height of 10 mm of the inner side wall was used. Then, 5 mL of the sample 100 which is a substance to be measured was placed in the sample container main body 21, and then the sample container main body 21 was sealed by the sample container lid 22. Here, for example, the temperature of the sample 100 is 20 ° C.
As a standard sample whose viscosity is known in advance, three types of 0.5 (mPa · s), 1.0 (mPa · s), and 2.0 (mPa · s) were used as shown in FIG. .

  Then, a rotational torque was applied to the rotary vanes 12 of the rotor 1 on the surface of this standard sample to rotate the rotor 1. In this case, the lower surface of the rotor 12 is in contact with the sample 100. Here, the rotary wing 12 attached an aluminum ball with a diameter of 2 mm to the lower end of the rotary shaft 11 as a lower portion 11 e on a disc of an aluminum plate with a diameter of 28 mm and a thickness of 0.1 mm. The rotating shaft 11 was a glass tube having a diameter of 1.6 mm and a length of 30 mm.

Next, the rotating magnetic field control unit 83 drives the motor 4 to rotate the magnet fixing base 7.
As a result, a magnetic field perpendicular to the rotary wings 12 of the rotor 1 generated by the first magnet 3_1, the second magnet 3_2, the third magnet 3_3, and the fourth magnet 3_4 is represented by the first magnet 3_1, the second magnet 3_2, the third By rotating the magnet 3 _ 3 and the fourth magnet 3 _ 4, a rotating magnetic field is applied to the rotary wings 12 of the rotor 1. By this rotating magnetic field, the rotating blades 12 of the rotor 1 are applied with rotating torque, and rotate in the same direction as the rotating direction of the applied rotating magnetic field.
Then, the rotation detection unit 81 stores, for example, a moving image of the mark 30 of the rotary wing 12 of the rotor 1 which is imaged by a rotation detection sensor (imaging element) as a captured image in its own storage unit. The rotation cycle of the mark 30 is determined by processing, and the number of rotations of the rotor 1 is determined from the rotation cycle of the mark.

The rotation speed ΩD of the corresponding rotor 1 is determined each time the rotation speed ΩM of the motor 4 is changed, and as shown in FIG. 5, the rotation speed ΩD of the rotor 1 and the rotation speed ΩM for each standard sample different in viscosity. And the correspondence with the difference of and ΩM is determined.
In FIG. 5, the relationship between the rotational speed ΩD of the rotor 1 of each standard sample and the difference between the rotational speeds ΩM and ΩM is a straight line. Therefore, FIG. 5 shows that the viscosity can be obtained only from the relationship between the number of rotations of the rotor 1 and the rotational torque applied to the rotor 1.
As a result, it is understood that the viscosity can be accurately measured by using the standard data.

Note that a program for realizing the function of the viscosity / elasticity measurement apparatus of FIG. 1 in the present invention is recorded in a computer readable recording medium, and the computer system reads the program recorded in the recording medium and executes it. Thus, processing may be performed to determine the viscosity of the sample. Here, the “computer system” includes an OS and hardware such as peripheral devices.
The "computer system" also includes a WWW system provided with a homepage providing environment (or display environment). The term "computer-readable recording medium" refers to a storage medium such as a flexible disk, a magneto-optical disk, a ROM, a portable medium such as a ROM or a CD-ROM, or a hard disk built in a computer system. Furthermore, the "computer-readable recording medium" is a volatile memory (RAM) in a computer system serving as a server or a client when a program is transmitted via a network such as the Internet or a communication line such as a telephone line. In addition, those that hold the program for a certain period of time are also included.

  The program may be transmitted from a computer system in which the program is stored in a storage device or the like to another computer system via a transmission medium or by transmission waves in the transmission medium. Here, the “transmission medium” for transmitting the program is a medium having a function of transmitting information, such as a network (communication network) such as the Internet or a communication line (communication line) such as a telephone line. Further, the program may be for realizing a part of the functions described above. Furthermore, it may be a so-called difference file (difference program) that can realize the above-described functions in combination with a program already recorded in the computer system.

1, 1A: Rotor 2, 200, 420: Sample container 4: Motor 4a: Motor shaft 5: Rotation sensor 6: Sample base 7: Magnet fixing base 8: Viscosity measurement unit 11: Rotating shaft 11m: Member 11t: lower portion 12 ... Rotor wing 21, 201, 421 ... Sample container main body 21s, 421s ... Bottom surface 21t ... Grooved portion 22, 202, 422 ... Sample container lid 22h ... Through hole 30 ... Mark 3_1 ... 1st electromagnet 3_2 ... 2nd electromagnet 3 3 ... 3rd ... 3rd Electromagnets 3_4 Fourth electromagnet 50, 600 Rotor holding portion 51 Rotational shaft holding hole 81 Rotation detection portion 82 Viscosity detection portion 83 Rotational magnetic field control portion 84 Standard data storage portion 85 Device control portion 411 Convex Department

Claims (9)

A part or the whole is made of a material having conductivity, and the disc has a piece shape in which the surface of the disc is fixed perpendicularly to the rotation axis, and the tip of the rotation axis is smooth A convexly formed rotor,
A sample container in which the substance to be detected whose viscosity is to be detected is placed, and the rotor is disposed in a state where the surface of the disc is in contact with the substance to be detected;
A magnet disposed around the sample container for applying a magnetic field to the rotor;
The dynamic magnetic field application magnet is driven to apply a time-varying magnetic field to the rotor to induce an induced current in the disc of the rotor, and the induced current and the magnetic field applied to the rotor A rotation control unit that applies rotation torque to the rotor to rotate the rotor by Lorentz interaction;
A rotation detection unit that detects the rotation speed of the rotor;
A visco-elasticity detection unit that detects viscosity and elasticity of the detection target material in contact with the rotor according to the rotational speed of the rotor;
The apparatus for measuring viscosity and elasticity according to claim 1, wherein the radius of the disk of the rotor is determined using a sample of which viscosity or elasticity is known in advance according to the following equation.

Rc: Contact radius of the contact portion with the bottom of the sample container at the bottom of the rotor M: Weight of the rotor V: Volume of the part immersed in the sample of the rotor :: Specific gravity of the sample g: Gravity acceleration R: Rotor of the rotor Radius η: viscosity of the substance to be detected μ: dynamic friction coefficient between the lower part of the rotor and the bottom of the sample container d: thickness of the sample sandwiched between the rotor and the sample container α: measurement accuracy of required viscosity and elasticity
ω: Rotational angular velocity at the top of the sample The apparatus for measuring viscosity and elasticity according to claim 1, wherein a convex portion of an axial tip of the rotation shaft of the rotor is in contact with a bottom of an inner surface of the sample container. It further comprises a storage unit for storing standard data obtained by measuring in advance the relationship between the rotational torque applied to the rotor and the rotational speed of the rotor in a plurality of substances whose viscosity is known,
The viscosity / elasticity of the substance to be detected is determined by comparing the standard data with the relationship between the rotational torque and the number of revolutions of the substance to be detected detected by the viscosity detection unit. The viscosity and elasticity measuring device according to item 2. The rotor is marked,
The viscosity / elasticity measuring apparatus according to any one of claims 1 to 3, wherein the rotation detection unit detects the rotation speed of the rotor by detecting the rotation of the mark. The number of rotations of the rotor is detected by irradiating a laser to the disk of the rotor and optically measuring a change in reflected light or interference pattern thereof. The viscosity and elasticity measuring device according to any one of claims 3 to 10. 6. The viscosity according to any one of claims 1 to 5, wherein a bottom of an inner surface of the sample container in contact with the rotor is formed in a smooth flat surface or a smooth curved concave shape. Elasticity measuring device. The sample container is provided with a lid for closing an upper opening of the sample container,
The rotary shaft of the rotor is rotatably provided between the bottom portion of the inner surface of the sample container filled with the detection target substance and the inner surface of the lid. The viscosity / elasticity measuring apparatus as described in any one of Claim 6. The internal space of the sample container is formed to be thicker in proportion to the distance from the rotation axis with respect to the diameter direction of the disc of the rotor. The viscosity and elasticity measuring device as described in any one of claim | item 7. A sample container is filled with a detection target substance to be detected for viscosity and elasticity, and the detection target substance is partially or entirely made of a conductive material, and the disc is a surface of the disc with the rotation axis The rotor is formed in the shape of a vertically fixed shaft, and the tip of the rotary shaft is formed in a smooth convex shape so that the substance to be detected is in contact with the surface of the disc. Process,
A dynamic magnetic field application magnet disposed around the sample container is driven to apply a time-varying magnetic field to the rotor to induce an induced current in the disc of the rotor, and the induced current and the induced current Applying a rotational torque to the rotor to rotate the rotor by Lorentz interaction with a magnetic field applied to the rotor;
Detecting the number of revolutions of the rotor;
By the rotational speed by the equation radius of less of the disc of the rotor and a viscosity detection step of detecting the viscosity and elasticity of the detection target in contact with the rotor, the sample with a known pre-viscous or elastic The viscosity / elasticity measuring method characterized in that it is determined using

Rc: Contact radius of the contact portion with the bottom of the sample container at the bottom of the rotor M: Weight of the rotor V: Volume of the part immersed in the sample of the rotor :: Specific gravity of the sample g: Gravity acceleration R: Rotor of the rotor Radius η: viscosity of the substance to be detected μ: dynamic friction coefficient between the lower part of the rotor and the bottom of the sample container d: thickness of the sample sandwiched between the rotor and the sample container α: measurement accuracy of required viscosity and elasticity
ω: Rotational angular velocity at the top of the sample

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