A force-matching method for quantitative hardness measurements by atomic force microscopy with diamond-tipped sapphire cantilevers

We present a new method to improve the accuracy of force application and hardness measurements in hard surfaces by using low-force (<50 μN) nanoindentation technique with a cube-corner diamond tip mounted on an atomic force microscopy (AFM) sapphire cantilever. A force calibration procedure based on the force-matching method, which explicitly includes the tip geometry and the tip-substrate deformation during calibration, is proposed. A computer algorithm to automate this calibration procedure is also made available. The proposed methodology is verified experimentally by conducting AFM nanoindentations on fused quartz, Si(1 0 0) and a 100-nm-thick film of gold deposited on Si(1 0 0). Comparison of experimental results with finite element simulations and literature data yields excellent agreement. In particular, hardness measurements using AFM nanoindentation in fused quartz show a systematic error less than 2% when applying the force-matching method, as opposed to 37% with the standard protocol. Furthermore, the residual impressions left in the different substrates are examined in detail using non-contact AFM imaging with the same diamond probe. The uncertainty of method to measure the projected area of contact at maximum force due to elastic recovery effects is also discussed. -- Research Highlights: → A new method improves the accuracy of hardness measurements by AFM nanoindentation. → A computer algorithm is made available to automate this new method. → Comparison of experimental results with literature data yields excellent agreement. → Hardness measurements show a systematic error less than 2% when applying the new method. → Elastic recovery effects on measurements of contact area at maximum force are discussed.