JP3121587U - Ultra high viscosity measuring device - Google Patents

Abstract

An ultra-high viscosity measuring apparatus capable of measuring ultra-high viscosity stably and accurately with a small-scale, simple and low-cost configuration and simple and efficient measurement work.
External force application means for applying a constant external force G in one direction parallel to the other surface 12 to one surface 11 of a block-shaped sample 10 having two surfaces 11 and 12 parallel to each other. The movable member 21 that follows the displacement of the one surface 11 of the sample 10 to be measured, the capacitive electrode 31 that is installed in the vicinity of the movable member 21, and the capacitance 10 that appears on the capacitive electrode 31 And a capacitance type displacement meter 30 that measures the amount of displacement of the one surface 11, and the viscosity of the sample 10 to be measured is measured based on the measurement by the capacitance type displacement meter 30.
[Selection] Figure 1

Description

The present invention relates to an ultra-high viscosity measuring apparatus, and is particularly effective when used for measuring a viscosity of an ultra-high viscosity substance having a viscosity of 10 ⁸ Pa · s or more, for example.

Conventionally, as an apparatus for measuring an ultrahigh viscosity of, for example, 10 ⁸ Pa · s or more, an ultrahigh viscosity measuring apparatus as shown in FIG. 4 has been provided. The apparatus shown in the figure is disclosed in Patent Document 1, and uses a rectangular block-shaped sample 10 having a lower surface 12 and an upper surface 11 parallel to each other, and the lower surface 12 of the sample 10 is used as a fixed surface. The plate-like fixing member 22 is fixed and fixed, while the upper surface 11 thereof is fixed and fixed to the plate-like movable member 21 as a displacement surface.

  The movable member 21 is adapted to apply a constant external force G in parallel and in a fixed direction to the lower surface 12 of the sample 10 by an external force applying means including a wire 24, a pulley 25, a weight 26, and the like. .

  When a predetermined external force G is applied to the displacement surface of the sample 10 via the movable member 21 in a state where the sample 10 is in a predetermined measurement temperature environment, the upper surface (displacement surface) 11 of the sample 10 The sample 10 is displaced in parallel according to the viscosity of the sample 10.

  This displacement can be measured as the moving distance of the movable member 21, but the displacement is very small. Therefore, in the conventional technology, the minute displacement is precisely measured by the light wave interferometer 57.

  In order to perform displacement measurement by the light wave interferometer 57, the return reflectors 221 and 222 are attached to the fixed member 22 and the movable member 21, respectively. In addition, a Wollaston polarizing prism 58 and a biprism 59 are provided for temporarily rejoining the input / output optical axis L1 of the light wave interferometer 57 by bifurcating L11 and L12.

  The viscosity measurement is performed in a state where the sample 10 is placed in the vacuum image furnace 60 and the outside air is shut off. This is to prevent the light interference distance from changing due to the influence of air fluctuation (density change) due to temperature fluctuation when the sample 10 is heated (or cooled) to a predetermined measurement temperature condition.

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  In the above-described apparatus, the ultrahigh viscosity is measured by measuring the minute displacement of the sample 10 due to the external force G by the light wave interferometer 57. However, the following problems occur in this measurement.

(1) A complicated and delicate optical path adjustment must be performed, and a high degree of skill is required for measurement.
(2) Although the optical paths L1, L12, and L12 are inevitably longer due to the necessity of branching and re-merging of the optical paths, the optical paths L1, L11, and L12 are long, and thus are easily affected by vibrations and are extremely high in viscosity. It was difficult to measure the temperature stably and accurately.
(3) Further, the interference distance is easily changed due to the influence of air fluctuation. In order to reduce the influence of the air fluctuation (density change), a vacuum environment using a vacuum image furnace 60 or the like is necessary. However, the use of a vacuum environment causes high costs due to the large scale of the apparatus, complicating measurement work, and reducing efficiency.

The present invention has been made in view of the above problems, and its purpose is to stably and accurately achieve ultra-high viscosity with a small, simple and low-cost configuration and simple and efficient measurement work. An object of the present invention is to provide an ultra-high viscosity measuring apparatus capable of measuring.
Other objects and configurations of the present invention will become apparent from the description of the present specification and the accompanying drawings.

The present invention provides the following solutions.
(1) an external force applying means for applying a constant external force parallel to the other surface and in a fixed direction on one surface of a block-shaped sample having two surfaces parallel to each other; Capacitive type that measures the amount of movement of the movable conductor portion based on a change in capacitance appearing on the movable conductor portion, a capacitive electrode that is installed close to the movable conductor portion, and a capacitance change that appears on the capacitive electrode An ultra-high viscosity measuring apparatus comprising: a displacement meter, wherein the viscosity of the sample to be measured is measured from the amount of movement measured by the capacitance displacement meter.

  (2) In the above means (1), the external force applying means is an apparatus that pulls a movable member fixed to one surface of the sample to be measured with a constant force in a fixed direction. measuring device.

  (3) In the above means (1) or (2), the movable conductor portion is formed on the whole or a part of a movable member fixed to one surface of the sample to be measured. High viscosity measuring device.

  (4) In any one of the above means (1) to (3), the capacitance type is attached to the first capacitive electrode installed in the vicinity of the movable conductor and the fixed member to which the sample to be measured is fixed. A fixed conductor portion provided at a position that is the same distance as the movable conductor portion with respect to the displacement meter, a second capacitor electrode disposed in proximity to the fixed conductor portion, and first and second capacitor electrodes Capacitance displacement gauges that measure the amount of movement of the movable conductor portion relative to the fixed conductor portion based on the difference in capacitance change appearing in each of the above, and the movement measured by these capacitance displacement meters An ultra-high viscosity measuring apparatus characterized in that the viscosity of the sample to be measured is measured from the amount.

  (5) In any one of the above means (1) to (4), the capacitive electrode is composed of two independent capacitive electrodes, and the capacitive displacement meter is an electrostatic capacitance generated between the two capacitive electrodes. An ultra-high viscosity measuring apparatus configured to detect a change in capacity.

It is possible to provide an ultra-high viscosity measuring apparatus capable of measuring ultra-high viscosity stably and accurately with a small-scale, simple and low-cost configuration and simple and efficient measurement work.
Operations / effects other than those described above will be apparent from the description of the present specification and the accompanying drawings.

  FIG. 1 is a schematic side view showing an embodiment of an ultra-high viscosity measuring apparatus according to the present invention. The apparatus shown in FIG. 1 performs ultra-high viscosity measurement using a block-like sample 10 having a lower surface 12 and an upper surface 11 formed on flat surfaces parallel to each other, and includes a heating / cooling device 15. , A temperature control device 16, a fixed member 22, a movable member 21, a wire 24, a pulley 25, a weight 26, and the like, a capacitance displacement meter 30, and the like.

As shown in the figure, the sample 10 to be measured is formed in a three-dimensional body, and its lower surface 12 is fixed and fixed to the fixed member 22 as a fixed surface, while its upper surface 11 is fixed to the plate-shaped movable member 21 as a displacement surface.・ Fixed.
The heating / cooling device 15 is configured using an electric heater or a Peltier element, and heats or cools the sample 10 to be measured to a predetermined measurement temperature condition. The heating / cooling device 15 is used together with a temperature control device 16 using a microcomputer.

  The movable member 21 is pulled by a constant force G in a constant direction parallel to the lower surface 12 of the sample 10 by an external force applying means including a wire 24, a pulley 25, a weight 26, and the like. . Accordingly, a constant external force G is applied to the upper surface 11 of the sample 10 in parallel to the lower surface 12 and in a certain direction.

  The electrostatic capacitance type displacement meter 30 has a sensor support shaft 35 whose position can be adjusted, and first and second sensor heads 33 and 34 are provided at the tip of the support shaft 35. A first capacitive electrode 31 is attached to the distal end surface of the first sensor head 33, and a second capacitive electrode 32 is attached to the distal end surface of the second sensor head 34.

  The capacitive electrodes 31 and 32 are connected to the capacitive displacement meter 30 via electrostatically shielded conductive wires (shield wires), respectively.

  The first and second capacitive electrodes 31 and 32 form a pair and are configured and installed so as to perform displacement measurement by capacitance under the same conditions. The first capacitor electrode 31 is positioned in advance so as to face the end surface of the movable member 21 with a predetermined gap distance d. Similarly, the second capacitor electrode 32 is positioned in advance so as to face the end surface of the fixing member 22 with the gap distance d therebetween.

  Each of the movable member 21 and the fixed member 22 has at least a portion facing the capacitor electrodes 31 and 32 or the entirety thereof as a conductor portion. Capacitance electrodes 31 and 32 are placed close to the conductor portion, so that a capacitance is formed between the capacitance electrode 31 and the conductor portion.

  Further, the movable member 21 and the fixed member 22 are provided at positions where the surfaces facing the capacitive electrodes 31 and 32 are the same distance Ls from the capacitive displacement meter 30, respectively.

  The capacitance type displacement meter 30 includes an amount of change in the gap distance d between the first capacitor electrode 31 and the movable member (movable conductor portion) 21 and a gap between the second capacitor electrode 32 and the fixed member (fixed conductor portion) 22. The amount of change in the distance d is detected as the amount of change in capacitance.

  In this case, the gap distance d between the second capacitor electrode 32 and the fixing member 22 should not be changed, but actually varies slightly due to the thermal expansion of the measurement bench due to temperature. This variation greatly affects the displacement measurement result of the movable member 21.

  However, this variation similarly occurs in the gap distance d between the first capacitor electrode 31 and the movable member 21. Therefore, by subtracting and correcting the amount of change in the gap distance d between the second capacitor electrode 32 and the fixed member 22 from the amount of change in the gap distance d between the first capacitor electrode 31 and the movable member 21, the above fluctuations can be corrected. The influence on the displacement measurement result of 21 can be offset.

  For this reason, the capacitance displacement meter 30 extracts only the positional displacement amount of the movable member 21 based on the difference between the two capacitances respectively appearing on the first capacitance electrode 31 and the second capacitance electrode 32. Configured to measure.

  Based on the displacement measured in this way, the viscosity of the sample to be measured can be accurately measured without being affected by disturbance factors such as temperature changes. If necessary, the displacement amount of the movable member 21 is converted into a unit of viscosity and output to a display or the like.

  The capacitance between the capacitive electrode 31 and the movable member 21 is almost inversely proportional to the square of the gap distance between them. The electrostatic capacitance between the capacitive electrode 32 and the fixing member 22 is the same. Therefore, if the gap distance d between the two is preset sufficiently short, a minute displacement of the upper surface (displacement surface) 11 of the sample 10 can be detected and measured with high sensitivity and high accuracy.

  In the ultra-high viscosity sample 10, the amount of displacement that occurs when a constant external force G is applied to the upper surface (displacement surface) 11 in a certain direction is very small. Measured with high accuracy. Based on this measurement, the ultrahigh viscosity can be accurately measured.

  Further, in the ultrahigh viscosity measuring apparatus of the embodiment shown here, heating or cooling of the sample 10 by the heating / cooling device 15 is performed in an open environment with respect to the outside air, not in a vacuum environment where the outside air is blocked. .

  For this reason, when the sample 10 to be measured is heated or cooled in order to set a predetermined measurement temperature condition, an influence due to air fluctuation (density change) can be considered. However, the capacitance generated between two electrodes placed close to each other greatly depends on the gap distance between both electrodes, but is insensitive to air fluctuation (density change) existing between both electrodes. .

  The relative permittivity of air or gas is close to 1 in a vacuum, and even if the air density between the electrodes changes greatly, the change in relative permittivity due to this is small and is almost close to 1. If at least the gap distance between the electrodes is close enough in advance, the change in capacitance due to the gap distance is almost negligible. That is, it may be considered that there is substantially no influence due to air fluctuation (density change).

Therefore, the apparatus of the present invention has the following advantages over the conventional apparatus described above.
(1) Complex adjustment of the optical path is unnecessary, and highly skilled measurement is not required.
(2) There is no long-distance optical path that is susceptible to vibration and the like.
(3) Since the influence of air fluctuation due to temperature fluctuation is small, a vacuum environment becomes unnecessary.

  Thereby, ultra-high viscosity can be measured stably and precisely with a small-scale, simple and low-cost configuration and simple and efficient measurement work.

  FIG. 2 shows a preferred embodiment of the capacitive electrode 31 that forms the sensor part of the capacitance displacement meter 30. In the embodiment shown in the figure, the capacitor electrode 31 is composed of two independent capacitor electrodes 311 and 312. The capacitive electrodes 311 and 312 are connected to the capacitive displacement meter 30 via electrostatically shielded conductive wires (shield wires) 313 and 314, respectively.

  Capacitances C11 and C12 that change approximately inversely proportional to the square of the gap distance d between the electrodes 311 and 312 and the movable conductor portion (22) appear in the two capacitance electrodes 311 and 312 respectively. A series combined capacitance Cx of the capacitances C11 and C12 appears between the two capacitance electrodes 311 and 312.

  By detecting the amount of change in the series composite capacitance Cx, the influence of the floating capacitance is surely eliminated, and the amount of displacement between the electrodes 311 and 312 and the movable conductor portion (22) can be measured more stably and with high accuracy. Can do.

  Although not shown, the second capacitor electrode 32 is configured in the same manner as the capacitor electrode 31.

  FIG. 3 shows a configuration example of the capacitance displacement meter 30. As shown in the figure, a capacitance displacement meter 30 suitable for use in the present invention includes first and second capacitance-voltage conversion circuits 41, 42 by a switched capacitor type capacitive negative feedback circuit. Using sample-and-hold circuits 43 and 44, an analog subtracting circuit 45, an AD converter 46, a data processing unit 47, a display 48 and the like that hold the outputs of the capacitance-voltage conversion circuits 41 and 42 while periodically updating them. Can be configured.

  The first capacitance-voltage conversion circuit 41 converts the capacitance Cx appearing on the first capacitance electrode 31 into a voltage. Similarly, the second capacitance-voltage conversion circuit 42 converts the capacitance Cr appearing on the second capacitance electrode 32 into a voltage.

  Both converted output voltages are once held by the sample-and-hold circuits 43 and 44 and then subtracted by the subtracting circuit 45 (subtraction processing). Thereby, the variation in the distance between the capacitance type displacement meter 30 and the sample 10 to be measured is offset.

  The difference output of the subtracting circuit 45 is converted into digital data by the AD converter 46 and converted into viscosity by the data processing circuit 47. This processing result is transmitted and output to the outside, and displayed numerically on the display 48.

  As the capacitance displacement meter 30, for example, an off-the-shelf product such as a capacitance displacement meter (model number: AS-9000-2) manufactured by MTI, USA may be used as it is.

  As mentioned above, although this invention was demonstrated based on the typical Example, this invention has a various aspect besides the above-mentioned. For example, the capacitor electrode 31 may be other than the above-described two-pole type, for example, a single-pole type or a three-pole type or more. Further, the capacitance type displacement meter 30 may be an analog output type.

  It is possible to provide an ultra-high viscosity measuring apparatus capable of measuring ultra-high viscosity stably and accurately with a small-scale, simple and low-cost configuration and simple and efficient measurement work.

It is an abbreviated side view showing an embodiment of an ultra-high viscosity measuring device according to the present invention. It is an abbreviated sectional view and an equivalent circuit diagram showing a preferred embodiment of a capacitive electrode forming a sensor part of a capacitance displacement meter. It is a circuit diagram which shows the high excitation of an electrostatic capacitance type displacement meter. It is an abbreviated side view showing the configuration of a conventional ultra-high viscosity measuring device.

Explanation of symbols

10 Sample to be measured,
11 Upper surface (displacement surface),
12 Lower surface (fixed surface),
21 movable member (movable conductive part),
22 fixing member (fixed conductive part),
24 wires,
25 pulley,
26 weights,
30 capacitance meter,
31, 32 capacitive electrodes,
311, 312 capacitive electrode,
33, 34 sensor head,
35 Sensor spindle,
G external force,
d gap distance,
C11, C12 capacity,
Cr reference capacity,
Cx composite capacity,
41, 42 capacitance-voltage conversion circuit,
43,44 Sample and hold circuit,
45 Analog subtraction circuit,
46 AD converter,
47 data processing unit,
48 Display.

Claims (5)

  External force applying means for applying a constant external force parallel to the other surface and in a fixed direction on one surface of a block-shaped sample having two surfaces parallel to each other, and displacement of one surface of the sample to be measured A movable conductor portion that is driven, a capacitive electrode that is installed in proximity to the movable conductor portion, and a capacitance displacement meter that measures the amount of movement of the movable conductor portion based on a capacitance change that appears on the capacitive electrode; And measuring the viscosity of the sample to be measured from the amount of movement measured by the capacitance displacement meter.   2. The ultrahigh viscosity measuring apparatus according to claim 1, wherein the external force applying means is an apparatus that pulls a movable member fixed to one surface of the sample to be measured with a constant force in a predetermined direction.   3. The ultrahigh viscosity measuring apparatus according to claim 1, wherein the movable conductor portion is formed on the whole or a part of a movable member fixed to one surface of the sample to be measured.   The movable electrode according to any one of claims 1 to 3, wherein the movable electrode portion is movable relative to the capacitive displacement meter on a first capacitive electrode installed in proximity to the movable conductor portion and a fixed member to which the measured sample is fixed. A fixed conductor portion provided at a position that is the same distance as the conductor portion, a second capacitance electrode that is installed in proximity to the fixed conductor portion, and capacitances that appear on the first and second capacitance electrodes, respectively. A capacitance-type displacement meter that measures the amount of movement of the movable conductor portion relative to the fixed conductor portion based on a change difference, and the viscosity of the sample to be measured from the amount of movement measured by the capacitance-type displacement meter. An ultra-high viscosity measuring apparatus characterized in that     5. The capacitive electrode according to claim 1, wherein the capacitive electrode is composed of two independent capacitive electrodes, and the capacitive displacement meter detects a change in electrostatic capacitance generated between the two capacitive electrodes. An ultra-high viscosity measuring device characterized in that it is configured as described above.

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