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Instrumented indentation test for hardness and materials parameter from millinewtons to kilonewtons
(2002)
The ISO/DIS 14577 Metallic materials - Instrumented indentation test for hardness and
materials parameters Part 1-3 (IIT) concerns test forces up to 30 kN. The paper reports on
IIT at test forces ranging from 0.002 N to 1000 N on non magnetizable steel X8 CrMnN 18-
18 (1.386) with well polished surface using Vickers indenter and four hardness machines of
different design (Nano Indenter XP, Fischerscope H 100, Zwick Z005 with Universal
hardness head and a laboratory four-column set up materials testing machine) according to
the standard. Using mostly identical test parameters the results of the different machines are
almost in good agreement. Estimated small differences are caused by the different
uncertainties of the used machines and by different methods of mathematical analysis of the
detected raw data.
Ti/TiN multilayer coatings with multilayer periods in the range 550 nm and a final thickness of 2 µm were deposited on steel substrates by cyclic modulation of nitrogen gas flow into the chamber of a PVD sputtering device. Coating characterization was performed by cross-sectional transmission electron microscopy, glancing-angle X-ray diffraction and instrumental indentation testing. Individual a-titanium and titanium nitride layers were always observed, although for the finer microstructures, the TiN layers were thicker than the Ti layers by a factor three. The plastic hardness of the films increased steadily with decreasing layer spacing, following a HallPetch relationship. Finally, a hardness value of 42 GPa was reached, which is similar to that of a thick TiN monolayer, prepared under the same coating conditions.
A Round Robin (RR) exercise on selected coated materials has been carried out with the aim of finding the optimal conditions for the analysis of nitride layers with GD-OES. Such pre-normative work is necessary for the evaluation of parallel development of the production of nitride layers as certified reference materials (CRMs). Two types of samples, TiN layer and VN layer, respectively, with chemical compositions close to stoichiometry and a thickness of ~3 µm, deposited on a steel substrate, have been provided to the RR participants. Additionally, another type of sample, a (100 nm CrNi/100 nm Cu) multilayer (ML) stack deposited on silicon wafer has also been included in the RR. This sample can be used as a CRM for checking GD spectrometer conditions and it has been proved helpful in further development of GDS instrumentation and methodology. The RR exercise has been performed in the frame of the EC Thematic Network on Glow Discharge Spectroscopy for Spectrochemical Analysis (GDS-Net).