3.3.

1 The oscillating system

The pendulum consists of a suitable torsion wire, a pendulum linkage with mirror for oscillation
detection and the crucible holder. Two types of construction, the standing as well as the hanging
crucible, are conceivable for the technical implementation. The construction of the suspended crucible
is self-evident and is already shown in Figure 2.2. The pendulum is above the furnace and protrudes into
the latter with the crucible holder. With this construction, there is a risk that the torsion wire warms by
heat conduction in the pendulum and by gases rising from the furnace. A change in the temperature of
the torsion wire would directly change the parameters of the vibration. An effective interruption of heat
conduction and convection is therefore one of the challenges in the construction of a vibratory
viscometer.

The concept of the standing crucible [43] attempts to circumvent these disadvantages. Only the crucible
holder projects into the oven from below. The temperature-sensitive torsion wire is located under the
furnace and is protected against ascending hot gases. The heat conduction in the pendulum, however,
also takes place with this design. Because the crucible and specimen crucible is above the torsion wire, a
counterweight is required at the lower end of the pendulum to hold the center of mass in the lower half
of the pendulum. However, such a pendulum is generally more susceptible to disturbances than a
hanging pendulum. Furthermore, the great moment of inertia of such a pendulum proves to be
problematic for the measurement of the viscosity of metal melts. The damping of the oscillation caused
by a molten mass comparable to the suspended crucible is very small and thus more difficult to measure
due to the great moment of inertia.

The design of the suspended crucible is considered to be better suited with the requirement for smallest
possible specimens as defined in section 3.2.

The torsion pendulum is shown in Figure 3.1. At the lower end of the pendulum, the sample container is
made of graphite. This is shown half-transparent in the illustration, so that the crucible is visible inside
the container. The sample container is provided with an internal thread and is screwed to the container
head after installation of the sample. This is also made of graphite and has a step in the middle area.
This stage is required to center the insulating plug at the top of the furnace. This is necessary since the
insulating plug is pulled out of the furnace when the sample is changed with the pendulum and is
introduced into the furnace again when the sample is installed. The container and the head were also
made from BN, but proved to be not very practical, as the screw has always opened automatically
during the measurement. At the upper end of the head there is a bore of 4 mm diameter and 20 mm
depth on the cylinder axis. The pendulum rod is made of tungsten in this hole. The container head is
mounted on the pendulum bar with two crosswise arranged cotter pins made of tungsten wire. Both the
cotter pins and the pendulum rod irreversibly change to tungsten carbide (WC) at a temperature above
1400C. It is therefore advisable to process a new pendulum rod without a container head in the oven
and to use the rod for regular measurements. Since WC is very brittle (comparable to glass), the
pendulum rod must be handled with extreme caution. The slight brittleness of WC is also the reason
why the two wire pins for the attachment of the container head must be renewed after each
measurement.
The pendulum rod of W / WC reaches the middle of the upper insulation plug in the installed state.
There the pendulum stick is contained in a tube made of Al2O3 ceramic
4 mm inside diameter and 1 mm wall thickness. The connection is again made with wireplins. Because of
the lower temperatures in this area of the furnace, these do not change into WC and therefore do not
have to be replaced. For use as a pendulum rod, rods of ceramic materials were also tested. As a result
of the firing process, rods made of ceramic materials are never quite straight, which leads to
disturbances in the torsional vibrations. Furthermore, it was observed that Al2O3 ceramic rods began to
expand under temperatures of 1600C under the load of sample and container. In one case, this
elongation during a measurement resulted in fracture of the rod.

The ceramic tube is fitted at the top end to a stainless steel component. The two parts are also
connected by wireplins. The upper end of the component is inserted in a triangular disc made of
stainless steel and is fixed there with three clamping screws offset by 120 mm. The connection between
this disc and a disc of the same design, which is arranged parallel to each other at a distance of 40 mm,
is made by means of three radially arranged cylinders of stainless steel screwed to the discs. This
interruption in the course of the pendulum alone serves to disturb the heat conduction in the
pendulum. In order to keep the moment of inertia of the pendulum as small as possible with this
arrangement, the sides of the triangular disks were curved convexly as far as possible.

In the further course of the pendulum follows a support made of stainless steel, on the cylindrical axis of
which a silicon wafer is attached as a deflecting mirror for the laser beam for vibration detection. A
further distribution takes place after this mirror carrier. Instead of the stainless steel cylinders, identical
PTFE is used, which is characterized by a very poor heat conduction. In the disc at the upper end of the
manifold is attached to the torsion wire to terminate the connectors. The mounting is also carried out
with three clamping screws offset by 120 deg.

In contrast to many other viscometers, the torsion wire is not soldered to the pendulum. A soldering
connection always entails the risk that the elastic properties of the wire will change. Therefore, the wire
is fixed by means of a clamping mechanism. This is comparable in its function to a drill chuck, but was
correspondingly miniaturized.

The construction of the torsion pendulum permits the use of different crucibles. For this purpose, only a
suitable sample container has to be made, which is attached to the pendulum rod with two splints.
Containers for crucibles with an outside diameter of 30 mm as well as crucibles with a higher height
were successfully tested as part of the construction. A further advantage of the modular design of the
pendulum is the easy replacement of individual components in the event of damage.

3.3.5 Data acquisition, evaluation and control

A separate measuring and control program has been developed for the control of the viscometer as well
as the recording and processing of the measured values. To calculate the viscosity from the measured
vibration parameters the working equations of Roscoe (2.19) and Beckwith (2.20) were implemented. A
detailed description of the structure and functions of the program is not possible at this point for
reasons of space. However, such a description is given in the user manual of the viscometer, which is
attached to this work as an appendix (see chapter B.2).

The electrical acquisition of measured data and logic states takes place via an analog-to-digital converter
card, which is installed directly in the control computer. Measuring devices, which have internal signal
processing, transmit the measured data via serial interfaces to the control computer.

B.1.5 Completion of the frame

After the furnace and the vacuum system have been completed, the structure of the frame can be
continued as shown in figure B.9. For this purpose, four legs are mounted on the upper side of the
existing frame for receiving the displacement mechanism for the pendulum. On these feet, the
aluminum plate is fixed with four screws. The alignment of the plate must be observed: around the
circular cutout in the aluminum plate, three groups of tapped holes are arranged in the form of an
equilateral triangle. The tip of this triangle must point to the rear of the unit. In the holes around the
circular cutout in the aluminum plate, the three bearing rods of the sliding mechanism are attached.
Before the bearing rods are connected at their upper end to an aluminum ring and thus stabilized, two
linear bearings must be mounted on each bearing rod for the displacement of the pendulum tube.

Now the gibbet can be mounted on the back of the rack. Before attaching the gallows, the
counterweight for the pendulum tube must be installed from above into the quadrangle of the gallows.
To prevent the weight from slipping out of the pipe during the mounting, the weight must be secured by
means of a bolt in the holes provided for this purpose. After installing the weight, the two deflection
pulleys for the cable between the pendulum tube and the counterweight must be installed.

The completed gallows is attached to the frame, as shown in Figure B.10. First, the upper mounting
plate (1) is screwed to the frame. In a second step, the lower end of the gallows is screwed. Please note
that the screw connection is located at the lower end of the gallows in the interior of the square tube.

B.1.6 Installation of the pendulum tube

The pendulum pipe must now be installed in the sliding mechanism (see Figure B.11). The front halves of
the clamping plates (1) are attached to the linear bearings on the front bearing rods. Now, the
pendulum tube is placed on the still free flange of the upper double cross and is provisionally locked
there. If the pendulum tube already fits exactly into the semicircular sections of the holding plates, the
assembly can be continued. If the pendulum tube does not fit into the recesses, the oven and / or the
table may have to be aligned with the displacement mechanism.