Hardness is a useful measure of a material’s resistance to permanent indentation; but for viscoelastic polymers, hardness data are highly dependent on the test type and the parameter set chosen. Vickers microhardness testing is used to leave small indents (<150 µm) and is shown to be applicable to polymers. A detailed investigation of the required steps for microhardness testing in isotactic polypropylene (iPP) is provided. Samples should be mounted in epoxy resin in order to maintain curing temperatures at room temperature. Mounted samples can be ground and polished in a semi-automatic polisher using graduated SiC paper (wet grinding) but progressing onto alumina suspension for polishing. Final polishing should be performed with 0.05-µm alumina suspension. The hardness measured was shown to be dependent on load and dwell time with a much greater dependency on dwell time. Strain recovery was shown to be completed after a time period equal to the dwell time. This study shows that indents can be measured thereafter, and it is recommended that they be measured within a 24 h period after the indent was created. After data fitting, the equation for hardness was shown to follow a power law with load and dwell time as the main variables. Fitting parameters were compared to those found in the literature, and it was found that parameters were significantly different to those reported elsewhere. Therefore, this study highlights the importance of calibrating on a case-by-case basis. Finally, to show the usefulness of the Vickers micro-hardness testing method, the calibrated test method was applied on iPP with additions of carbon black up to 3 wt.%. Comparisons were made with data from the literature, but the hardness data generated in our work were found to be at least twice that reported in the literature. The testing parameters were not cited in the literature: specifically, the dwell time was not provided, and this generated doubt on the usefulness of the cited data. Hence, this work is intended to serve as an exemplar of how to prepare and proceed with hardness testing of polymers.
Keywords: Vickers hardness; carbon black addition; isotactic polypropylene.