Examples of nanoindentation data ================================== .. include:: includes.rst Please look at the experimental procedure proposed by Jennett N. M. and Bushby A. J. [#Jennett_2001]_, to perform nanoindentation tests on bulk, coatings or multilayer systems, and to the ISO standard (ISO 14577 - 1 to 4). Type of data - Pre-Requirements ################################## Only data from Continuous Stiffness Measurement (CSM), given as a function of the indentation depth are accepted in the NIMS toolbox (e.g.: CSM mode for Agilent - MTS nanoindenter or DMA - CMX algorithm for Hysitron nanoindenter). You data must only have the loading part from the load-displacement curves of your (nano)indentation results. In the case of data saved in a 'Sample' or 'Analyst Project' sheet of a .xls file obtained with 'Analyst' (MTS software) (containing at least a 'Hold Segment Type' or a 'END' segment), the toolbox is able to consider only the loading part of your results. Please, check if the surface detection is well done, especially if the substrate is compliant [#Kaufman_2009]_ and [#Piccarolo_2010]_. For more explanations about the surface detection, look into the `NIMS documentation `_. It is advised to use average results from at least 10 indentation tests to avoid artefacts (e.g. pop-in, roughness, local impurities or dust on the sample's surface...). .. note:: To analyze pop-in distribution, the Matlab PopIn toolbox was developed. The `Matlab code `_ is available on GitHub with `the documentation `_. Agilent - MTS example files ############################### * Both .txt or .xls files are accepted. * 3 columns (Displacement / Load / Stiffness) * 6 columns (Disp. / SD (Disp.) / Load / SD (Load.) / Stiff. / SD (Stiff.)) (SD for Standard Deviation) * It is possible to get directly these type of average sheet in your .xls file, using the 'Analyst' Excel macro provided by MTS. * `MTS_0film_Si_CSM-2nm_noSD.txt `_ - Data for a bulk Silicon sample. - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 2nm) (no standard deviation). * `MTS_1film_SiO2_Si_CSM-2nm.xls `_ - Data for a thin film of Silicon thermal oxide (500nm) on a bulk Silicon sample. - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 2nm). * `MTS_1film_SiO2_Si_CSM-2nm_noSD.xls `_ - Data for a thin film of Silicon thermal oxide (500nm) on a bulk Silicon sample. - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 2nm) (no standard deviation). * `MTS_2films_Al_SiO2_Si_CSM-2nm.xls `_ - Data for a thin film of PVD Aluminum (500nm) deposited on a bulk Silicon sample with a Silicon thermal oxide (500nm). - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 2nm). * `MTS_3films_Au-Ti-SiO2-Si_CSM-1nm.txt `_ - Data for a thin film of PVD Gold (500nm) deposited on thin film of PVD Titanium (500nm) on a bulk Silicon sample with a Silicon thermal oxide (500nm). - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 1nm). * `MTS_3films_Au-Ti-SiO2-Si_CSM-1nm.xls `_ - Data for a thin film of PVD Gold (500nm) deposited on thin film of PVD Titanium (500nm) on a bulk Silicon sample with a Silicon thermal oxide (500nm). - Data obtained by Berkovich indentation with CSM mode (75Hz / amplitude 1nm). The last example (2 files for Au-Ti-SiO2-Si sample) is used to validate the elastic multilayer model of Mercier et al. [#Mercier_2010]_. A micrograph of this sample is given :numref:`multilayer_sem`. .. figure:: ./_pictures/multilayerSEM.png :name: multilayer_sem :scale: 60 % :align: center *SEM cross-sectional observation of a multilayer sample.* Hysitron example files ########################## * Both .txt or .dat files are accepted. * `Hysitron_dma.txt `_ - Data obtained by Berkovich indentation with DMA mode (205Hz / amplitude 0.65nm) - Courtesy of `Dr. Igor Zlotnikov `_ from `Max Planck Institute of Colloids and Interfaces `_ in Potsdam, Germany. References ############ .. [#Jennett_2001] `Jennett N. M. and Bushby A. J., "Adaptive Protocol for Robust Estimates of Coatings Properties by Nanoindentation" (2001). `_ .. [#Kaufman_2009] `Kaufman J. D. and Klapperich C. M., "Surface detection errors cause overestimation of the modulus in nanoindentation on soft materials" (2009). `_ .. [#Mercier_2010] `Mercier D. et al., "Young's modulus measurement of a thin film from experimental nanoindentation performed on multilayer systems" (2010). `_ .. [#Piccarolo_2010] `Piccarolo S. et al., "Improving surface detection on nanoindentation of compliant materials" (2010). `_ - `ISO 14577 - 1 , "Metallic materials -- Instrumented indentation test for hardness and materials parameters -- Part 1: Test method", (2002). `_ - `ISO 14577 - 2 , "Metallic materials -- Instrumented indentation test for hardness and materials parameters -- Part 2: Verification and calibration of testing machines", (2002). `_ - `ISO 14577 - 3 , "Metallic materials -- Instrumented indentation test for hardness and materials parameters -- Part 3: Calibration of reference blocks", (2002). `_ - `ISO 14577 - 4 , "Metallic materials -- Instrumented indentation test for hardness and materials parameters -- Part 4: Test method for metallic and non-metallic coatings", (2007). `_ - `Agilent website `_ - `Hysitron website `_