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Application Note

Depth Profiling of Hardness and Modulus

The Load-Partial Unload Technique

 

The NanoTest can be used to determine hardness and Young's modulus as a function of depth at a single point. This is achieved by producing a series of load-unload hysteresis curves with progressively increasing load, but where the indenter remains in contact with the point of interest throughout. This is significantly faster than producing a corresponding series of separate indentations since diamond-specimen contact has to occur only once. To ensure that contact is maintained, only partial unloading is performed. During reloading, the Depth vs. Load data is essentially superimposed on the previous unloading curve until the additional load increment is applied, when further plastic deformation takes place.

20 consecutive load-50% unload curves from a 2.5 µm TiN film deposited on a plasma nitrided steel substrate. Loading rate = 0.35 mN/s; dwell time at maximum load = 10 s. The slope change in the loading curves at a total depth of approximately 300 nm was due to substrate effects.

An Alternative Method


A possible alternative approach is known as Continuous Stiffness Measurement. Here, an extremely small sinusoidal oscillation is superimposed on the load ramp and the dynamic response of the contact is determined. Theoretically, this permits the instantaneous stiffness to be determined. However, this technique requires knowledge of 8 parameters, including the instrument damping coefficient. Contact damping and contact frictional effects should also be taken into account, but these parameters are not measurable. Clearly, implementation of the load-unload procedure is relatively straightforward.

 

In addition, to measure the mechanical properties of normal materials using indentation methods, it is necessary to hold the load periodically in order to allow time-dependent processes to occur. In such cases, continuous stiffness results still show discrete points in curves of Hardness vs. Depth and Modulus vs. Depth.