This application claims the priority, under 35 U.S.C. § 119, of Austrian application AT A50408/2015, filed, May 20, 2015; the prior application is herewith incorporated by reference in its entirety.
The invention relates to a rotary rheometer.
The object of the invention is above all, for rheometers and therefore also for viscosimeters which do not have their own built-in normal force measurement, to provide normal force limitation which keeps the measurement gap constant and prevents damage in the event of excessively high forces. In the case of the invention, viscosimeters are regarded as equivalent to rheometers.
By definition, rheology deals with the deformation and flow behavior of substances. Rotary rheometers are measuring instruments for studying the rheological properties of different material samples. Viscosimeters are special rheometers for determining viscosity. In this case, the measurement sample to be studied is introduced into a generally narrow measurement gap between two measurement parts, the two measurement parts are rotated and/or oscillated relative to one another, and the material sample is subjected to a shear load between the measurement parts. Elastic material functions are additionally obtained from the axial forces which act perpendicularly to the shear plane in cone/plate and plate/plate rheometers or similar arrangements. In this case, a multiplicity of further possible measurement part geometries are known. Rotary rheometers make it possible to combine a multiplicity of different test runs in which either the shear stress, the shear deformation or the shear rate can be predetermined. Rotary rheometers may in principle have different embodiments with a measurement motor, a rotation motor and a separate measurement motor, or the combination of two measurement motors, and are described for example in Austrian patent AT508706 B1, corresponding to U.S. Pat. No. 8,453,496.
The torque determination in the rotary rheometer may be carried out with (measurement) motors configured for driving and for torque determination, or alternatively by two separate motor units for drive/rotation and for torque determination, which are respectively assigned to one of the measurement parts. Depending on the instrument type, the upper measurement part or the lower measurement part, for example a measurement cup, in this case rotates. The resulting torque and/or the phase angle are determined. Furthermore, a double motor system with two measurement motors is also known, for example Austrian patent AT 508 706 B1. In addition to this, different systems for determining the normal forces (axial forces) occurring are known.
The rheometer shown here by way of example has a measurement motor M, which rotates or drives in rotating oscillation a measurement shaft 22 and the upper measurement part 20 connected thereto. In this case, the relationship between the torque on the measurement shaft 22 and the power consumption of the measurement motor M is accurately known or can be determined by calibration. Different measurement systems and maximally low-friction bearing arrangements make it possible to determine the rotation angle and rotation speed. All the values are available in an evaluation unit, which is not represented.
The rheological characteristics of the medium sample are determined in the evaluation unit from the torque or from the supply parameters, in particular from the electricity consumption of the measurement motor M and/or from the frequency and/or from the phase angle of the measurement shaft 22 and the gap data while taking into account measurement geometry data of the measurement parts and the temperature.
The determining factors for the measurement accuracy in the rheometer or viscosimeter are, besides precise determination of the torque and the stability of the ambient conditions, maximally friction-free mounting of the drive and/or measurement shafts, and in particular also the stiffness of the stand. In order to measure the respective instantaneously acting torque with minimal frictional and tensile forces, for example magnetic and air bearings for the rotating components are known.
The actual distance of the two measurement parts from one another, or the height or thickness of the gap S, in this case also has a great influence on the measurement accuracy. The measurement motor and the measurement parts lie at an adjustable axial distance from one another, which is kept constant during the measurement, on a stand 32 or frame 33. In this case, at least one of the measurement parts is actuated by an optionally automatic setting unit, or adjustably carried by setting parts.
Other features which are considered as characteristic for the invention are set forth in the appended claims.
Although the invention is illustrated and described herein as embodied in a rotary rheometer, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
Referring now to the figures of the drawings in detail and first, particularly to
Under constant ambient conditions, predetermined gap heights S can therefore be approached with micrometer accuracy, and at the same time the required forward feed in the mm or cm range for introduction of the sample medium into the measurement gap, or for changing the measurement parts, can be achieved.
Nevertheless, any differently designed precise mechanical linear forward feed may also be used, for example linear motors, pneumatically driven adjustment devices, Uhnig nut drives, and the like, in order to be able to introduce the sample into the measurement gap S by lowering and raising the lower measurement part 30 and/or the upper measurement part 20 and establishing the desired measurement gap between the measurement parts 20, 30.
In a rheometer having a stand, and above all in automated gap systems, the problem arises that when the measurement system is immersed in the sample and when the measurement system is extracted from the sample, different normal forces act on the bearing of the measurement motor. These forces likewise depend on the viscosity of the sample, as well as on the nature of the measurement system and the displacement speed. In the event of a displacement speed selected incorrectly by the user, a mechanical overload may be triggered, the drive may be blocked, or the measuring apparatus may even be damaged. In all these cases, the measurement gap S is modified, the sample must be taken out of the measuring instrument, and the latter must be re-referenced.
In many cases, rheometers have normal force measurement devices which make it possible not only to study the torques acting, which act against the shear load because of the sample viscosity, but also to measure the normal forces acting perpendicularly to the shear load. These forces almost always occur because of the elastic components of real viscoelastic samples. A wide variety of variants for normal force measurement are known in the prior art, for example contactlessly operating normal force sensors located in the air bearing of a rotary rheometer.
Economical viscosimeters or rheometers, for example for monitoring and standard characterization of samples in production processes, are however often configured without normal force measurement for cost reasons. In this accuracy class, the measurement drives are for example configured with a ball bearing or favorable air bearings.
The object of the invention is to develop a system which can record normal forces in the positive and/or negative direction up to a maximum limit force without significant or no negligible movement of the measurement parts, and therefore without a substantial measurement gap change, i.e. it holds the rheometer entirely stiffly but, when this limit force is exceeded, directly opens a contact and therefore makes the occurrence of a normal force exceeding the limit force detectable. In this way, the rheometer can stop the displacement movement until the normal force is reduced below the limit value. Once the normal force has decreased below the limit value again, the contact is closed and the mechanical position is again absolutely identical to that before the opening.
Since one key element for accurate characterization of the sample is the consistency of the measurement gap, all safety devices must essentially be configured without travel, and the measurement gap between the measurement parts must be kept constant.
For example, the normal force discontinuity when reaching the contact point of the upper measurement part with the sample is used to establish when the two measurement parts 20, 30 have come in contact with the sample when being brought together and therefore that the approach of the two measurement parts must be slowed. In particular, viscoelastic samples with a high elastic component, for example polymer melts, asphalt, chocolate, etc. are not compressed in shape until they are between the two measurement parts 20, 30 and possibly protruding sample edges are trimmed after the desired measurement gap width has been adjusted. If the rheometer has a normal force measurement unit, it is ensured by means of the latter that the sensitive components, in particular bearings, etc. of the rheometer are not damaged. The outline profile, represented in
The two measurement parts 20, 30 of the rheometer, here a plate/plate measurement system, are brought toward one another in the direction R. The distance between the two measurement parts 20, 30 is selected at the start of the test so that the sample can be introduced well between the measurement parts, and the distance between the measurement parts is therefore large. The schematic diagrams represent the variation of the gap width of the measurement gap S between the plates and the measured or occurring normal force between the measurement parts 20, 30. The first section shows rapid approach of the two measurement parts until the time t0—in this case, the normal force increases abruptly. After this time, the sample surface is in contact with the two measurement parts. The further approach generally only takes place more slowly, in order to introduce the sample uniformly between the measurement parts. If at a time (here t1) the highest permissible normal force is exceeded, then the adjustment speed can be reduced again by the control and regulation unit, or the adjustment device. The approach takes place with V3 or is stopped, in order to allow adaptation of the sample to the gap width. When the desired (measurement) gap width Sm is reached, the sample may optionally be trimmed and the measurement may be started. The normal force profiles shown may naturally also not extend linearly, depending on the sample, and are represented here only by way of example.
A further problematic case is the limitation of the forces occurring when the two measurement parts are moved away from one another after the test has been carried out.
Many studied samples, for example after the hardening of rubber, solidification of chocolate, etc. adhere to the measurement parts. In particular when using cylindrical measurement systems, with naturally large contact areas between the measurement part surface and the sample, the measurement system may be damaged. When there is a normal force measurement, the system reduces the displacement speed of the carrier of the measurement part because of the negative normal forces occurring.
After the end of the measurement with a defined distance of the measurement parts Sm, at time t3 the separation of the measurement parts from the sample begins by movement with the speed V3. If the normal forces in this case increase because of effects, for example adhesion, and exceed the adjusted limit force (time t4), the speed of the drive is adapted (V4) or the drive is stopped. When the sample has been fully separated from one of the measurement parts or contact with the sample residues adhering to the two measurement parts is broken, movement may continue at maximum speed. At time t5 NF decreases to 0.
Here again, the profiles of the distance between the measurement parts 20, 30 and the variation of the normal force NF are represented schematically. Actual profiles show different functional dependencies depending on the sample properties.
Another problem is the extremely high normal forces occurring for many samples, which may arise during the conduct of a test, for example thermal regulation of the sample, shear thickening or the like, and require immediate interruption of the measurement.
If an economical rheometer or viscosimeter, for example for standard characterization, has not implemented any normal force measurement, apart from the sensitive measurement and bearing parts, an automatic or motor-controlled stand which may be used may also be damaged by the overloads occurring, when the stepper motor cannot be throttled or stepped down by the motor control.
Hitherto, this problem has been resolved by having to select extremely slow speeds for automatic movement with the stand, and an unnecessary time loss has therefore had to be tolerated even for quality measurements.
Even with manual adjustment on the stand, the sensitive motor bearing may in this case suffer damage when the adjustment mechanism of the stand is moved further despite high forces occurring.
If precise force measurement or a limiter switch were installed in this case, the measurement gap must not be influenced. Particularly when moving the measurement parts toward one another, the switching mechanism must generate no delay in the triggering, since otherwise the gap geometry could be modified.
Because of the hysteresis which any switch has for its triggering behavior, conventional switches entail a variation of the gap due to the normal force occurring. The gap, however, must not vary as a function of the forces occurring, especially when the measurement parts are being moved toward one another.
According to the invention, these problems are resolved in a rotary rheometer of the type mentioned in the introduction. According to the invention, at least one switching unit is provided, which responds to changes in the force flow in the force circuit, delimited by the measurement parts, of the rotary rheometer and has switching contacts for the activity of the adjustment device, which stops the adjustment device when a predetermined limit force value is exceeded for the force flow in the positive or negative direction, optionally without relative movement of the measurement parts, or with the measurement parts remaining in the same position.
For precise switching, it is advantageous that the contact parts of the switching contact are arranged movably relative to one another in a direction which extends parallel to the direction of the relative movement of the measurement parts in the course of their adjustment, or has a component extending parallel to this movement direction.
A mechanically advantageous structure is obtained when the two contact parts of the respective switching contact respectively lie on one of two members of the force circuit of the rotary rheometer which can be moved relative to one another or are structurally independent of one another or can be separated from one another, and at least one spring unit is provided, with which these two members and the contacts of the switching contact can be pressed onto one another or toward one another by spring force and are held in this position.
Depending on the intended use of the rheometer, it is possible that the switching contact is arranged on individual components of the force circuit of the rotary rheometer, preferably a carrier or a carrier plate of the measurement or drive motor, along a measurement shaft, along a drive spindle of the adjustment device or along the holder for the measurement or drive motor, or respectively between the individual components or in the connection or transition region from one component to the other.
For the structure of the rotary rheometer, it is expedient that the force circuit of the rotary rheometer contains as components a stand, a frame, a carrier for the drive or measurement motor and the measurement part and the measurement shaft, and the adjustment device for height adjustment of the measurement part or the spindle and/or its drive.
A simple and accurate structure is obtained when the contact parts of the switching contact, which interact for switching off or stopping the adjustment device, and are optionally formed as contact surfaces, lie on physically separable and independently movable members or components of the force circuit, which are pressed with a spring force, in particular parallel to the component of the normal force occurring in the sample and optionally measured, in the direction in which the measurement gap is variable and adjustable, or in which the measurement parts can be moved toward one another or away from one another.
In order to avoid damage, it is advantageous that the adjustment device abruptly terminates the adjustment movement of the measurement parts relative to one another when the switching contact is opened and/or, when the carrier is formed at least with two members. The respective members which lie successively in the force circuit respectively being pressed against one another by at least one spring unit with a predetermined spring force, and in that when a separating force exceeding the spring force acts on the members the two members pressed against one another can be removed from one another and at the same time the contact parts of the switching contact can therefore be separated from one another.
A rheometer which can be used advantageously in practice and is constructed simply with a nut mounted adjustably in height on the drive spindle, is obtained when the nut carries a preferably annular contact member with an upwardly projecting contact part, a contact part preferably formed by a contact ring lying above the contact part and being connected to a clamp sleeve which carries a clamping ring on its lower end, a coil spring with a predetermined spring force being arranged between the clamping ring and the carrier of the drive or measurement motor or of the measurement shaft, and a further coil spring with a predetermined spring force being arranged between the nut and the clamping ring and/or when the carrier carries an upwardly projecting contact part, in that a contact member with a downwardly projecting contact part, which can be applied from above onto the contact part carried by the carrier, is arranged above the carrier, which contact part is carried by a clamping sleeve which carries a clamping ring at its lower end, a coil spring with a predetermined spring force being arranged between the clamping ring and the carrier of the drive or measurement motor or of the measurement shaft, and a further coil spring with a predetermined spring force being arranged between the nut and the clamping ring.
A structure which is advantageous for the geometry of the rheometer is obtained when the coil spring encloses the further coil spring and optionally extends below the switching contact, and/or in that the clamping sleeve lies between the coil spring and the further coil spring, and/or in that the further coil spring encloses the spindle, and/or when the contact parts are loaded with leaf or helical or coil springs, the spring force of which acts in the direction of the opening and closing movement of the contact parts or has a spring force component acting in this direction.
In practice, it is very expedient that in order to detect the by at least one measurement part in the course of its adjustment by a force exerted by the sample, in addition to the switching unit or switching contacts responding to the force flow in the force circuit, a device for measuring the normal force FN exerted by the sample and directed positively or negatively with respect to the direction of the force flow is provided.
For the guidance of the measurement method, it is advantageous that the lifting spring and the lowering spring are respectively prestressed with a prestressed force or a limit force value, which corresponds to the weight of the components or apparatus to be carried of the rotary rheometer and a predetermined force value. The predetermined force value corresponds to a force value exerted by the sample onto the measurement part in the positive and negative directions of the force flow and still regarded as tolerable.
According to the invention, the switching unit may be a spring system, prestressed on one or both sides against a stop, with switching contacts. Therefore, no movement takes place in the detection system until the triggering by exceeding the limit force value. When the limit force value is exceeded, the switching contact, which may be produced electrically via the contact surfaces of the prestressed spring units, is broken by a minimum excursion in the μm range.
By application of the spring units, for example helical springs, leaf springs or the like, the electrical switching contact can be prestressed against the limit force value, or the maximum permissible force NF. The spring(s) arranged for this purpose press the prestressed components or members of the rheometer against one another along the force circuit and establish there an electrical contact on the mutually touching contact surfaces. If the force occurring exceeds the limit implemented by the stiffness of the springs, the contact is broken and this interrupts the movement of the displacement unit, for example the current supply of the stepper motor.
This pre stressed switching contact may be installed at different positions in the force circuit of the rheometer. In this case, the two contact parts of the switching contact may be installed in any desired way separately in the force circuit of the rheometer, or alternatively the contact parts are installed preferably mirror-symmetrically with respect to the spindle or the measurement shaft together with the spring elements in the rheometer.
One spring unit 50 presses the segment II, configured as a T-shaped carriage with the force F1 against the left-hand carrier arm part I, and a second spring element 50 presses the segment III with the force F2 against the carrier arm part, or the segment II. At the same time, contact parts 31, 41 of switching contacts 40 are pressed against one another.
In the case of the two switching contacts 40, the electrical contact parts 31, 41 are kept closed by the spring force and the current circuit or supply circuit of the displacement mechanism of the adjustment device 1 can be switched with these switching contacts.
If the carrier arm or carrier 10 is now moved with the upper measurement part 20 and the measurement motor M with the speed v1 onto the lower measurement part 30, then beyond the adhesion to the sample, since the sample is in contact with the two measurement parts 20, 30, normal forces FN1 occur against the movement direction R′. Until the triggering force or limit force value FN1=−F1 is reached, the stand 32 and the frame 33 and the displacement device 1 remain unaffected by the forces occurring.
When the force limit value is reached, the spring force is equalized and the contact surfaces of the contact parts 31, 41 are lifted off one another, and the activity of the displacement device 1 is interrupted with the least possible displacement movement and without a time delay or hysteresis by opening the switching unit 40.
The same applies for the movement of the carrier 10 in the opposite direction with the speed v2 and the forces FN2 occurring in the opposite direction.
Until the triggering force or limit force FN2=−F2 is reached, the stand 32 and the frame 33 and the displacement device 1 remain unaffected by the forces occurring; the spring-loaded contact parts 31, 41 remain pressed against one another.
It is also possible to divide the carrier arm or carrier 10 only once. Correspondingly, it is then only possible to switch off the adjustment unit when the normal force FN1 or FN2 occurs.
In order to be able to implement the inventive principle, the spring unit 50 schematically represented here may be produced with any desired spring geometry; for example, leaf springs or coil springs may be used.
A principle for normal force limitation is therefore implemented without explicit or actual measurement of the normal force. This purely mechanical alternative embodiment is robust and economical, and operates reliably.
In the context of the invention, a spring unit 50 is intended to include all elements which can press the contact surfaces 31, 41 of the switching contacts 40 against one another with a defined prestress. Besides mechanical spring systems, it is also possible to select pneumatic cylinders and/or electromagnetic springs and/or permanent magnets as alternative implementation variants.
By way of example, different installation variants of the switching unit and of the spring units 50 in the force circuit K of the rheometer are represented here. If the measurement gap S is closed and the two measurement parts 20, 30 are in contact with the sample, the force circuit K represented in outline is closed. The stand 32 and the measurement motor M are configured to be as stiff as possible, so that the measurement gap S is not modified by the forces occurring in the components that convey force. The spring units 50 provided according to the invention may be installed at different positions in this force circuit K. In
If adjustment is merely carried out manually, then instead of stopping the adjustment unit by the switching unit it is possible to emit a warning signal, and the manual adjustment is ended.
Preferably, the normal force limitation for both movement directions R is carried out in a combined member, in which two spring units 50 act against one another and prestress the contact surfaces 31, 41 against the two force directions R′, as is represented in
A preferred alternative embodiment for the installation of a switching unit, or of switching contacts 40, in the spindle 23 of a linear drive for the carrier 10 is represented in
The rotational movement of the spindle 23 is converted by means of the nut 2 into a vertical movement with the speed v, the rotation of the nut 2 optionally being prevented by an overload pin, which is for example guided in a driver jaw or holding ring 8.
If the nut 2 moves upward according to
The movement of the nut 2 upward acts against a normal force—FN. This force action is transmitted via the carrier 10 and the holding ring 8 to the lifting spring 7, which acts between the clamping ring 6 and the nut 2. With opening of the NF-plus contact 9, the adjustment movement of the carrier 10 ends abruptly. In
If the nut 2 moves downward according to
The movement of the nut 2 downward acts against a normal force FN. This force action is transmitted via the carrier 10, the driver jaw 8, the NF-plus contact 9, the contact surface 13, the clamping sleeve 5 and the clamping ring 6, and acts against the predetermined pre stressed force of the lowering spring 11.
The force flow may also change without the measurement parts 20, 30 executing a movement.
Number | Date | Country | Kind |
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A 50408/2015 | May 2015 | AT | national |
Number | Name | Date | Kind |
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8453496 | Lauger | Jun 2013 | B2 |
9702809 | Wolf | Jul 2017 | B2 |
20080022758 | Cottais | Jan 2008 | A1 |
20100269571 | Raffer | Oct 2010 | A1 |
Number | Date | Country |
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508706 | Jun 2011 | AT |
1885005 | Dec 2006 | CN |
WO 2015069633 | May 2015 | WO |
Number | Date | Country | |
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20160341647 A1 | Nov 2016 | US |