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