KR20170126681A - Geometry for measuring rheological properties in drying process - Google Patents

Abstract

The present invention relates to a geometry to measure rheological properties capable of simulating a drying process. More specifically, the geometry to measure rheological properties capable of simulating a drying process is used with a rotary rheometer to measure rheological properties during a drying process of a sample; has a wide area coming in contact with a sample when compared to a conventional technique; improves durability to transfer an accurate force to be useful in measuring rheological properties of a low-viscosity sample; comprising: a lower end tool (100) which has a disk shape, is installed in a lower end of the rheometer, includes a rim protrusion unit (120) protruding upwards and a protrusion unit (121) protruding upwards from a center of a circle, and allows a sample to be measured to be placed in an accommodation unit (110) formed between the rim protrusion unit (120) and the protrusion unit (121); and an upper end tool (200) installed in an upper end facing the lower end wherein an end of a lower side thereof comes in contact with the sample, or is immersed in the sample when measuring rheological properties. The lower end tool (100) and the upper end tool (200) are rotated by the rheometer, and are coaxially aligned with a rotary shaft of the rheometer.

Description

TECHNICAL FIELD [0001] The present invention relates to a geometry for measuring rheological properties in drying process,

The present invention relates to a geometry for measuring a rheological property capable of simulating a drying process, and more particularly to a geometry for measuring a rheological property such as viscosity and elastic modulus of a sample in a drying process, The present invention relates to a geometry for measuring rheological properties capable of simulating a drying process.

Rheological properties refer to properties such as viscosity, elasticity, stress and shear rate of a material. Rheometers are instruments for measuring the rheological properties of a sample. Samples measured by rheometers range from very low viscosity liquids to emulsions, suspensions, thermosets, cosmetics, pharmaceuticals, biogels, films, and bar-shaped solids. Depending on the type of rheometer, the measurement method of the sample is different. In the case of a rotary type rheometer, the geometry including the upper and lower plates arranged in the form facing each other is used. A concrete method is to measure a force transferred to a material and a force transmitted to an opposite flat plate by placing a measurement target material on a lower flat plate of the geometry and rotating one of the flat plates. The rheometer calculates the viscosity and elasticity of the material by taking into consideration the transmitted force and the time taken to be transmitted. For the conventional rheometer and geometry, Korean Patent Publication No. 2008-0070266 ("Mixed Flow Rheometer Quot ;, Jul. 30, 2008, hereinafter referred to as Prior Art 1), and Fig. 1 shows a representative drawing of Prior Art 1. Fig. As shown in FIG. 1, a specimen is placed between the lower friction plate 10 and the upper friction plate 10 'installed at the stop. The geometry is installed at the positions of the lower friction plate 10 and the upper friction plate 10' do.

On the other hand, in an industrial field where a solution used for coating or coating is used, it is necessary to monitor real-time changes in viscosity and change in elastic properties, such as change in elasticity, during drying of the coating or solution, And the geometry developed to simulate such a drying process is described in U.S. Patent No. 7472584 ("Device to measure the solidification properties of a liquid film and method therefor", Jan. 16, 2009, ).

Prior Art 2 is a T-shaped bar shape, which simulates a drying process. However, since the contact area with the solution is limited, there is a problem in that it is difficult to measure the absolute value of the fluid property during the drying process of the low viscosity solution.

1. Korean Patent Publication No. 2008-0070266 ("Mixed Flow Rheometer ", Jul. 30, 2008) 2. US Patent No. 7472584 ("Device to measure the solidification properties of a liquid film and method therefor ", Jan. 16, 2009).

Accordingly, it is an object of the present invention to provide a geometry for measuring a rheological property capable of simulating a drying process capable of more precise measurement.

Further, according to the present invention, the durability of the geometry itself is improved, so that a more accurate force can be transmitted to the opposite side of the sample and the rotary plate, thereby enabling accurate measurement.

In order to solve the above problems, a geometry for measuring a rheological property capable of simulating a drying process according to the present invention is a geometry for measuring a rheological property capable of simulating a drying process used in a rotational rheometer, A rim protrusion 120 protruding upward and a protrusion 121 protruding upward from a center of the circle. The rim protrusion 120 and the protrusion 121 protrude upward from the center of the circle, And a top tool 200 installed at an upper end facing the lower end and having a lower end in contact with or immersed in the sample when measuring the rheological properties of the sample, Wherein the lower tool 100 or the upper tool 200 is rotated by the rheometer and coaxially aligned with the rotation axis of the rheometer.

The upper tool 200 includes a first connection member 210 connected to the lower side of the upper end portion, a second connection member 220 extending downward from the first connection member 210, And a probe 230 surrounding a part of the lower part of the member 220 and having a lower end abutting the sample and having a plurality of ventilation holes 231 formed therethrough.

The upper tool 200 includes a first connection member 210 connected to the lower side of the upper portion, a second connection member 220 extending downward from the connection member 210, And a plurality of third linking members 250 radially connecting the second linking member 220 and the rim 240 to each other, .

The third connecting member 250 may have a first angle formed by the third connecting member 250 and the rim 240 when the third connecting member 250 is viewed from above, the third linking member 250 can be moved in a direction in which the upper tool 200 rotates or in a direction in which the lower tool 100 is rotated when the first angle? ) Is inclined in a direction opposite to the rotation direction. The geometry for measuring a rheological property capable of simulating a drying process.

The geometry for measuring the rheological properties, which can be used to simulate the drying process according to the preferred embodiments of the present invention, can be used together with a rheometer to simulate the drying process of the sample to precisely measure the rheological properties of the sample during the drying process .

According to the present invention, since the sample is received between the protruding portion protruding upward from the center of the lower tool and the rim protruding portion, and the upper tool contacts the sample, the torque transmitted from the protruding portion and the rim protruding portion is measured Therefore, it is possible to perform precise measurement even if the sample has characteristics of low viscosity.

According to the present invention, since the third connecting member is inclined in the direction in which the upper tool rotates or in the opposite direction in which the lower tool rotates, the durability is improved, and the force transmitted from the upper side of the rheometer is transmitted to the sample So that the accuracy of measurement can be improved.

1 is a schematic diagram of a conventional rheometer;
Figure 2 is a perspective view of a lower tool of geometry for measuring rheological properties capable of simulating the drying process of the present invention.
Figure 3 is a perspective view of a first embodiment of a top tool of geometry for measuring rheological properties capable of simulating the drying process of the present invention.
4 is a use cross-sectional view of a first embodiment of a lower tool and a top tool of a geometry for rheological properties measurement capable of simulating the drying process of the present invention.
5 is a perspective view of a second embodiment of a top tool of geometry for measuring rheological properties capable of simulating the drying process of the present invention.
6 is a perspective view of a third embodiment of a top tool of geometry for measuring rheological properties capable of simulating the drying process of the present invention.
Figure 7 is a top plan view of Figure 6;
8 is a graph showing changes in rheological properties according to Experimental Example.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout.

The geometry for measuring the rheological properties, which can be simulated by the drying process according to the present invention, is used in a rotatable rheometer and includes a lower tool 100 and an upper tool 200.

2, the lower tool 100 of the geometry for measuring the rheological property according to the present invention is installed at the lower end of the rheometer with the temperature control device, as shown in FIG. And a sample to be measured is contained. The lower tool 100 may have various shapes, but it is in the shape of a circular plate as shown in FIG. 2, and the lower tool 100 has a circular shape that shares the center of the circle of the lower tool 100 And includes a rim protrusion 120 and a protrusion 121 protruded upward from the center of the circle of the lower tool 100. The rim protrusions 120 and the protrusions 121 form a receiving portion 110 therebetween.

The material of the lower tool 100 may be formed of a metal or a polymer compound such as aluminum, titanium, stainless steel (SS 410, SS 430, SS 304, SS 316, SS 631, SAF 2205, SAF 2507) , PMMA, and PVC.

The reason why the lower tool 100 includes the receptacle 110, the rim protrusions 120 and the protrusions 121 is that the geometry for measuring the rheological properties, which can be simulated by the drying process according to the present invention, Since the sample in a gel state is dried, a liquid or gel sample contained in the lower tool 100 is prevented from flowing down.

The lower end of the rheometer to which the lower tool 100 is coupled is provided with a motor to rotate the lower tool 100 about an imaginary line extending upward from the center of the lower tool 100 However, this depends on the specification of the rheometer, and the motor may be installed at the upper end facing the lower end.

Although the geometry for measuring the rheological properties of the present invention described herein has various embodiments, the configuration of the lower tool 100 does not change, and the upper tool 200 has various embodiments The embodiments of the upper tool 200 will be described below.

[First embodiment of upper tool, when upper tool is cylindrical]

FIG. 3 illustrates a first embodiment of the top tool 200. FIG. As shown in FIG. 3, the upper tool 200 is installed at the upper end of the rheometer facing the lower end, and the lower end of the upper tool 200 is contacted with or immersed in the sample when measuring the rheological properties.

3, the upper tool 200 is installed at an upper end facing the lower end, and the lower end of the upper tool 200 contacts or is immersed in the sample when measuring the rheological properties, and the first connecting member 210, A connection member 220, and a probe 230. The upper end portion where the upper tool 200 is installed may be a motor portion provided with a motor according to the design of the rheometer as described above. When the motor is not installed, the force transmitted from the lower tool 100 is measured, This is the transducer to which other geometry can be installed.

The first linking member 210 is connected to the upper end of the rheometer and connected to the lower end of the rheometer, and has a cylindrical shape as shown in FIG.

As shown in FIG. 3, the second linking member 220 extends in a lower direction of the first linking member 210, and has a cylindrical shape like the first linking member 210.

3 and 4, the probe 230 surrounds a lower part of the second connection member 220, has a lower end abutting the sample, and has a plurality of ventilation holes 231 formed therein to be. As shown in FIG. 4, the probe 230 has a cylindrical shape with a lower side opened.

4, the end of the lower end of the probe 230 is in contact with a sample accommodated in the accommodating portion 110, and the protruding portion 121 is formed in a hollow space at the lower center of the probe 230. [ .

As shown in FIG. 3, a plurality of ventilation holes 231 are formed on the upper side of the probe 230. If the vent 231 is not formed, the lower end surface of the probe 230 may contact with the portion of the sample 230. In this case, This is because it may interfere with drying.

In the enlarged view of FIG. 4, a schematic direction of a force (torque) transmitted from the lower tool 100 is shown. When the lower tool 100 is rotated, the rim protrusions 120 and the protrusions 121 of the lower tool 100 transmit the force to the probes 230. The arrows in FIG. It shows a schematic situation. As the probe 230 receives the force from the rim protrusions 120 and the protrusion 121, it is possible to perform more precise measurement. In the past, since the protrusion 121 has no configuration corresponding to the protrusion 121, The measurement was not precise because the probe only received force from the rim protrusion formed on the outer periphery of the sample.

The material of the upper tool 200 may be formed of a metal or a polymer compound in the same manner as the material of the lower tool 100. The material of the upper tool 200 may be aluminum, titanium, stainless steel (SS 410, SS 430, SS304, SS 316, SS 631 , SAF 2205, SAF 2507), PTFE, PP, PMMA, and PVC. At this time, the entirety of the second connection member 220 or a part thereof perpendicular to the height direction may be formed of a material to be adiabatic. This is because the heat generated by the temperature regulating device is prevented from being transmitted to the upper end of the rheometer, and the material forming part or the whole of the second connecting member may be any material Typically, however, the air layer may be used as a heat insulating material in a hollow form, and may be formed of a ceramic mat or a synthetic resin material.

[Second embodiment of upper tool, when upper tool is radially connected]

Fig. 5 shows a second embodiment of the top tool 200. Fig. 4, the upper tool 200 includes a first connecting member 210, a second connecting member 220, a rim 240, and a third connecting member 250. As shown in FIG.

Since the first connecting member 210 and the second connecting member 220 have the same configuration as the first embodiment with the same name and drawing number, a description thereof will be omitted.

As shown in FIG. 5, the rim 240 is spaced apart from the second connecting member 220 by a predetermined distance. 4, the cross-section of the second linking member 220 is smaller than the cross-section of the rim 240 because the rim 240 has a diameter corresponding to the cross-section of the lower tool 100 Because. The diameter of the rim 240 may be the same as the cross section of the lower tool 100 and may be smaller. The lower end surface of the rim 240 is in direct contact with the sample accommodated in the lower tool 100 and functions as a lower end surface of the upper tool 200.

As shown in FIG. 5, a plurality of third connecting members 250 radially connect the second connecting member 220 and the rims 240. The shape of the third linking member 250 is a shape broken by a translator. When the rim 240 is radially formed as shown in FIG. 4, the narrow cross section of the rim 240 is in contact with the sample, but a large space between the plurality of third connection members 250 serves as the vent hole , Which is an advantageous embodiment for creating a drying environment.

[Third embodiment of the upper tool, the upper tool is radially connected, and the third connecting member is inclined]

FIG. 6 shows a third embodiment of the top tool 200. FIG. The third embodiment of the upper tool 200 shown in FIG. 6 is different from the second embodiment in that the third connecting member 250 is inclined with respect to the second connecting member 220 and the rim 240 It is a form that connects. This will be described in more detail with reference to FIG. FIG. 7 is a top view of the upper tool 200 shown in FIG. 7, the third linking member 250 has a normal line connecting the third linking member 250 and the rim 240 as viewed from above, and the third linking member 250 ) Is an acute angle rather than a right angle. 7, the third connecting member 250 is inclined in the same direction, so that the second angle? Facing the first angle? Is the first angle? the first angle? and the second angle? alternate along the outer rim of the rim 240 because the third linking member 250 is inclined in the same direction, Respectively. In the case of the second embodiment, the first angle is a right angle.

7, the direction in which the third linking member 250 is inclined is a direction in which the upper tool 200 rotates because the frictional force generated while rotating is transmitted from the sample to the third linking member 250 Accordingly, the force is more accurately transmitted to the upper end of the rheometer while improving the structural stability. If the third linking member 250 is inclined in the direction opposite to the rotation of the upper tool 200, the structural stability is lowered, and there is a possibility that structural deformation will occur. When a structural deformation occurs, the force will not be transmitted evenly, so the transmission of force is not correct.

When the lower tool 100 is rotated without rotating the upper tool 200, the lower tool 100 is rotated in a direction opposite to the tilting direction of the third link member 250.

In the case of the upper tool 200, the rotation direction may be rotated alternately. At this time, a third connecting member, which is inclined as shown in FIG. 7, is additionally provided, You can make it look zigzag when you see it. 7, the lower end of the added third connecting member is engaged with and joined to the lower end of the third connecting member which is already joined, and the upper end of the added third connecting member is connected to the first connecting member 210 and the upper end of the adjacent third connecting member 250 are coupled together.

 In this case, the same effect as that of the third embodiment can be obtained even if the upper tool 200 rotates in the opposite direction

[Experimental Example]

The experimental conditions use the second embodiment of the upper tool embodiment. First, a thermostat (APS) is installed at the lower end of the rotary type rheometer (ARES-G2), and the lower tool is attached. The rotary type rheometer used in the experiment has the motor at the lower end, so that the lower tool will rotate. Then, a second embodiment of the upper tool is installed in the transducing part which is the upper end of the rotary type rheometer. An appropriate amount of a polymer solution containing PGMEA (propyl glycol monomethyl ether acetate) as a solvent is added to the lower tool, and the upper tool is lowered so as to contact the solution. Thereafter, the temperature is gradually raised by 5 ° C. per minute using a thermostat, the motor speed at the lower end is fixed at 6.28 rad per second, and the viscoelastic property with time is measured at a strain value of 1%. FIG. 8 is a graph obtained as a result of the experiment. As shown in FIG. 8, it is possible to accurately measure the complex viscosity, which is one of the viscoelastic properties of the sample during the drying process.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention as defined by the appended claims. Accordingly, such modifications and changes are within the scope of protection of the present invention as long as it is obvious to those skilled in the art.

?: first angle
100: Lower Tool
110:
120: rim protrusion
121:
200: Top tool
210: first connecting member
220: second connecting member
230: probe
231: Vents
240: rim
250: third connecting member

Claims (4)

In a geometry for measuring rheological properties capable of simulating a drying process used in a rotating rheometer,
A rim protrusion 120 protruding upward and a protrusion 121 protruding upward from a center of the circle, wherein the rim protrusion 120 and the protrusion 120 protrude upward from the center of the circle, A lower tool (100) containing a sample to be measured in a receiving part (110) formed between the upper and lower plates (121, 121); And
An upper tool (200) installed at an upper end facing the lower end and contacting a lower end of the upper end of the sample (200) when the rheological property is measured;
/ RTI >
Wherein the lower tool (100) or the upper tool (200) is rotated by the rheometer and coaxially aligned with the rotational axis of the rheometer.
The method of claim 1, wherein the top tool (200)
A first connection member 210 connected to a lower side of the upper end portion,
A second connection member 220 extending downward from the first connection member 210,
The apparatus may further include a probe 230 that surrounds a lower portion of the second connection member 220 and has a lower end abutting the sample and has a plurality of ventilation holes 231 formed therethrough. Geometry for measuring rheological properties.
The method of claim 1, wherein the top tool (200)
A first connection member 210 connected to the lower side of the upper portion,
A second connection member 220 extending downward from the connection member 210,
A rim 240 formed at a predetermined distance below the second linking member 220,
A plurality of third linking members 250 radially connecting the second linking member 220 and the rim 240,
Characterized in that it comprises the following steps:
4. The apparatus of claim 3, wherein the third connecting member (250)
The first angle? Formed by the third connecting member 250 and the normal of the third connecting member 250 and the rim 240 is a right angle or an acute angle,
When the first angle (?) Is an acute angle, the third linking member (250)
Wherein the lower tool (100) is inclined in a direction in which the upper tool (200) rotates or in a direction opposite to the rotation of the lower tool (100) when viewed from above.

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