USE OF RHEOMETERS

FOR RUBBER
COMPOUNDS CONTROL

The preparation of rubber

compound is influenced by
several factors that influence the
results obtained:

Variability in the quality of the ingredients:

Polymer
Vulcanizing agent
Cure activator
Cure accelerator
Fillers ( reinforcing, diluents.)
Softener/ process acid /tackifier
Plasticizer
Protective agent (s)
Miscellaneous ingredients ( pigments, blowing agent, etc.)

Variability originated by the weighing system (automatic or manual)

used for the ingredients
Variability originated by the environmental conditions (temperature
and Humidity) which influence the dispersion and the activity level
of the ingredients.
Variability originated by the mixing parameters (time and
temperature)
In addition, the characteristics of the compound change
significantly when the product is stored.

All the influence factors described above has a considerable effect

on the characteristics of the compound produced
In many cases the variations are small and dont have a significant
effect on the results obtained after the transformation of the
compound into finished products.
In any case, compound producers, even with automatic weighing
system, statistically produce between 1% and 5% of nonconforming compounds that require additional rework activity to
correct the defects.

It is very important that the non-conforming compounds are

identified as quickly as possible in order to:

- remove the reason of the defect and avoid the production of more
non-conforming products
- prevent the non-conforming products from being transferred to the
next production stage
One of the biggest differences between rubber and other products
is the fact that many of the defects in the compound (ex. Dispersion
problems or mistakes in the dosage of accelerators) can be
invisible during the transformation process and be detected only
when the final product is used. For this reason, the final cost for a
non-detected defect can be very high.

Normally a test of the compound made with a Rheometer permits

to identify most of the possible problems in a rubber compound.
The test only takes a few minutes (generally between 3 and 5) and
is normally done on 100% of the batches.
This instrument permits to measure the change of the properties of
a rubber compound during the course of vulcanization.
Rheometers permit to apply a cyclic strain to a test piece and the
associated force is measured.
The test is carried out at a predetermined constant temperature
and the measure of stiffness is recorded continuously as a function
of time

MOVING DIE RHEOMETER

Moving Die Rheometer is considered the most
modern version of Rheometer.
The sample is placed between two dies.
The lower dies oscillates with 0.5 degrees
The upped die is connected to a torque sensor to
measure the torque response of the rubber at the
deformation.
Typically the working temperature is set between
170C and 190C (100 120C for platinum cured
silicon)
Plastic film (typically Polyamide or Polyester) is
placed between the dies and the samples to
prevent contamination of the dies during the test of
different products.
Thermal recovery is very fast
The instrument has very high repeatability and
reproducibility.

OSCILLATING DISK RHEOMETER

Oscillating Disk Rheometer is the most traditional kind of
rheometer.
The sample is placed between the two dies.
A rotor, placed in the middle of the dies oscillates with 3
degrees (or 1 degree)
The rotor is connected to a torque sensor to measure the
torque response of the rubber at the deformation.
Typically the working temperature is set between 170C
and 190C (100 120C for platinum cured silicon)
Test time required for complete curing of the sample is
slightly bigger then the one required for Moving die
Rheometer.
It is not possible to use plastic film between the rotor and
the sample. When different kind of rubber are used, a
blank test to clean the rotor is required.
Opening time between one test and the other must be
limited to obtain repeatable results.
This kind of instrument requires very little maintenance
and has extremely stable calibration

WHICH KIND OF RHEOMETER ?

The Moving Die Rheometer and the Oscillating Disk
Rheometer produce different test curves and results.
Even if the results are numerically different, they are
strongly correlated and provide the same information
about the sample tested.
Useful indication for the choice of the rheometer are:
-in case you need to compare your results with your
supplier or your customer it is useful to have the same
kind of instrument
-In case you need to test different kind of polymer it is
useful to use plastic film to prevent contamination (MD
Rheometer)
-Oscillating Disk Rheometer are normally slightly cheeper
both for purchase and for maintenance.
-Moving Die Rheometer have higher repeatability and the
influence of the operator is lower
-Moving die Rheometer can be combined with automatic
sample loading systems.

RESULTS OBTAINED WITH A RHEOMETER

PROCESSING
PHASE

The PROCESSING phase, during which the viscous (plastic) behaviour

of the compound is dominating shows rubber procesability and
therefore furnish useful indications about the fluency in the moulds.
Meaningful results are:
ML, (least torque)
tS1, tS2: Scorch time: time required for the increase of 1 (ts1) or 2 (ts2)
points from Minimum Torque. This number is an indication of the time
required for the beginning of the process of cross linking

RESULTS OBTAINED WITH A RHEOMETER

CURING PHASE

During the curing phase of the curve, the cross-linking process evolutes.
The shape and the slope of the curve are very important because the
curing curve must be designed according to the thickness of the finished
part to produce and to the kind of transformation process.
Typical data that can be obtained from the curve are:
t10: time corresponding to 10% curing
t50: time corresponding to 50% curing
t90: time corresponding to 90% curing. This result is considered the
optimum vulcanization time
Note: more data about the slope of the curve can be obtained.

RESULTS OBTAINED WITH A RHEOMETER

PHYSICAL
PROPERTIES

The last part of the curve is an indication of the physical proprieties of the
compound.
The maximum value of torque obtained is related with:
-the final level of cross-linking,
-The quality of the polymer used
-The filler used
-The compounding process.
The typical result is:
- MH: Maximum Torque
After the Maximum Torque has been reached the degradation of the compound can
be measured: the reversion is an indication of the resistance of the compound at
high temperature and can be useful for the design of the transformation process
-TR_x: Time for the torque reduction of x points

SCREENSHOT OF RHEOMETER SOFTWARE

Gibitre rheometers permit to:

- Store data and curves of the products tested
- Prepare a statistic of the results stored and create tolerance limits for future tests
- Compare each results with the expected tolerance limits for the product