TY - CONF A1 - Griepentrog, Michael A1 - Beck, Uwe ED - Schulte, J. ED - Niu, X. T1 - BAM certified reference materials for nano-metrology: Preparation, characterisation and certification T2 - Proceedings of the 3rd Annual Conference of the Asia Pacific Nanotechnology Forum T2 - 3rd Annual Conference of the Asia Pacific Nanotechnology Forum CY - Shanghai, China DA - 2004-12-09 KW - Certified reference materials KW - Film thickness KW - Mechanical properties KW - Surface acoustic waves KW - Naoindentation KW - Non-destructive testing KW - Destructive testing PY - 2005 SN - 0-97-57537-1-1 SP - 71 EP - 83 PB - Asia Pacific Nanotechnology Forum CY - Sydney AN - OPUS4-5482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dück, Alexander A1 - Gamer, Nadja A1 - Gesatzke, Wolfgang A1 - Griepentrog, Michael A1 - Österle, Werner A1 - Sahre, Mario A1 - Urban, Ingrid T1 - Ti/TiN multilayer coatings: deposition technique, characterization and mechanical properties JF - Surface and coatings technology N2 - Ti/TiN multilayer coatings with multilayer periods in the range 5–50 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 Hall–Petch 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. KW - Ti/TiN KW - Multilayer KW - Magnetron sputtering KW - Mechanical properties KW - Cross-sectional transmission electron microscopy (XTEM) PY - 2001 DO - https://doi.org/10.1016/S0257-8972(01)01171-9 SN - 0257-8972 VL - 142-144 SP - 579 EP - 584 PB - Elsevier Science CY - Lausanne AN - OPUS4-7646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Hattermann, Hilke A1 - Griepentrog, Michael T1 - Sol-gel-derived nanocomposite coatings filled with inorganic fullerene-like WS2 JF - Journal of sol gel science and technology N2 - Silica coatings filled with nanoscaled inorganic fullerene-like tungsten disulphide (IF-WS2) have been prepared through a sol–gel process on stainless steel substrates, and the structure and mechanical properties have been investigated. The precursor was prepared from a mixture of colloidal silica, 3-glycidoxypropyltrimethoxysilane (GLYMO), water and ethanol, adjusted to pH 4 with HNO3. In this solution WS2 is dispersed and in some cases immediately before coating ethylenediamine (ED) is added. The stainless steel substrates are dip-coated, dried in air and heat-treated in the temperature range of either 150–360 °C in air or up to 900 °C in vacuum. The solidification process is followed by differential thermal analysis (DTA). The resulting brown coloured coatings have a thickness of 1.5–4 µm. Scanning electron microscopy investigations (SEM) show that the WS2 nanoparticles are embedded as small aggregates in a hybrid silica matrix. X-ray diffraction (XRD) measurements prove that most of the tungsten disulphide embedded in the matrix can be protected against oxidation even after curing the samples at temperatures up to 900 °C. Hardness and modulus of the hybrid silica films were measured through an instrumented indentation test. Increasing the temperature of the heat treatment yields an increase of hardness from 0.3 to 1 GPa and of modulus from 3 to 17 GPa. The amount of up to 10 wt.% WS2 in the coatings has no remarkable influence on hardness and modulus of the samples. KW - Nanocomposites KW - Tungsten disulphide KW - Sol-gel KW - Mechanical properties PY - 2009 DO - https://doi.org/10.1007/s10971-009-1896-3 SN - 0928-0707 SN - 1573-4846 VL - 51 IS - 3 SP - 295 EP - 300 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-19713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griepentrog, Michael A1 - Krämer, Günther A1 - Cappella, Brunero T1 - Comparison of nanoindentation and AFM methods for the determination of mechanical properties of polymers JF - Polymer testing N2 - Force-deformation curves have been acquired using nanoindentation and atomic force microscopy on two amorphous polymer samples. The shape and size of the indenter tip was characterized using a white light interferometer and AFM. The measured nanoindentation curves were fitted with the Hertz equation to calculate the Young's modulus of the polymers. Once the Young's moduli of the polymers were known, AFM was used to acquire force-distance-curves on the same samples. We also used the Hertz theory for the analysis in this case. As a result, the tip radius of the AFM cantilever tip could be measured. This procedure is proposed as a method to determine the shape and size of AFM tips for the quantitative characterization of surface forces through force-distance curves. KW - Mechanical properties KW - Polymers KW - AFM KW - Nanoindenter PY - 2013 DO - https://doi.org/10.1016/j.polymertesting.2013.01.011 SN - 0142-9418 VL - 32 IS - 3 SP - 455 EP - 460 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-32073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krämer, Günther A1 - Griepentrog, Michael A1 - Bonaccurso, E. A1 - Cappella, Brunero T1 - Study of morphology and mechanical properties of polystyrene-polybutadiene blends with nanometre resolution using AFM and force-distance curves JF - European polymer journal N2 - Thin polybutadiene/polystyrene blend films were deposited on glass substrates by spin-coating. The two polymers were chosen, as they are immiscible and differ strongly in their mechanical properties. The blend was characterized with Tapping Mode and force–distance curves. Several advantages of force–distance curves measurements compared to Tapping Mode are shown, most of all the capability of yielding quantitative information about several properties, such as Young's modulus and adhesion. Also the aging behaviour of the blend exposed to air could be observed, in particular the increase of the Young's modulus due to cross-linking and dewetting processes. Additionally, the sample was used to improve the resolution of force–distance curves up to 6 nm, which is to date the best resolution achieved with force–distance curves. Such an improvement resolves the major disadvantage of force–distance curves, compared to other scanning mode, i.e. its inferior resolution. KW - Polymer blends KW - Mechanical properties KW - Atomic force microscopy KW - Force-distance curves KW - High-resolution force-volume PY - 2014 DO - https://doi.org/10.1016/j.eurpolymj.2014.03.026 SN - 0014-3057 SN - 1873-1945 VL - 55 SP - 123 EP - 134 PB - Elsevier CY - Oxford AN - OPUS4-30625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Instrumented Indentation Testing (IIT) - A critical journey from the very first steps to the modern state of the art N2 - Nowadays the Instrumented Indentation Testing (IIT), in the nano range often named as nano indention, is one of the most commonly used methods to determine the mechanical properties of materials in the micro and nano range. This method is already extensive standardized in DIN EN ISO 14577 part 1-4. In the past, the application of this standard in testing praxis shows that the established values have an excellent precision. On the other side, the trueness as comparability of obtained results with reference values is not so good. To improve accuracy of IIT the use of a variable ε and the consideration of the lateral displacement during indentation became normative requirements during the last revision of ISO 14577. Starting with the beginning of instrumented indentation testing in 1898 the historical background and the main assumption of the Oliver and Pharr method will be explained and critical discussed. It will be shown how to apply the use of a variable ε and the consideration of the lateral displacement during indentation in the daily testing work to improve accuracy of IIT. Finally, ongoing standardization projects in the field of IIT will be briefly presented. T2 - Advanced nano-mechanical techniques for academic and industrial research. MML Conference and Workshop CY - Warwick, UK DA - 13.12.2017 KW - ISO 14577 KW - Instrumented Indentation Testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Variable epsilon KW - Lateral displacement PY - 2017 AN - OPUS4-43466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Dynamic instrumented indentation test application and standardisation N2 - The draft of part 5 of ISO 14577 specifies verification and calibration of testing machines for carrying out the measurement of the dynamic material response when an oscillatory force or displacement, with amplitudes small in comparison to the prescribed target values, is imparted to the indenter while the indenter is continuously loaded to a prescribed target load or target depth or while the load or displacement is held constant at a prescribed target value. In case of a material showing plastic-elastic behavior, the measured dynamic response is used for continuous evaluation of the dynamic stiffness of the contact as a function of depth and frequency. Using the dynamic stiffness of the contact a reduced dynamic modulus will be calculated. In case of a material showing visco-elastic behavior from the measured dynamic response also the dynamic contact damping coefficient as function of depth and frequency is evaluated continuously. Using dynamic contact stiffness and dynamic contact damping coefficient reduced lost and storage modulus for visco-elastic materials will be calculated. The main normative requirements of the draft are discussed and their applications are illustrated by examples from daily experimental praxis. T2 - 13th Conference on Local Mechanical Properties CY - Košice, Slovak Republic DA - 06.11.2017 KW - ISO 14577 KW - Instrumented indentation testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Dynamic testing KW - Visco-elastic KW - Loss modul KW - Storage modul PY - 2017 AN - OPUS4-43468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Towards the standardization of dynamic instrumented indentation testing N2 - Nowadays the Instrumented Indentation Testing (IIT) is one of the most commonly used methods to determine the mechanical properties of materials in the nano range. This method is already extensive standardized in EN ISO 14577 part 1-4. Because of the great interest of researchers and industries in investigations of time depending material behavior mostly all suppliers of IIT equipment are offering the possibility of dynamic testing. Realizing this development ISO/TC 164/SC3 Hardness Testing has proposed to start the new standardization project “Linear elastic dynamic instrumented indentation testing DIIT”. The development of this standard is accompanied by the first international intercomparing exercise comparing results of dynamic instrumented indentation testing from testing machines using different hardware solutions and different models for data evaluation. The draft of part 5 of ISO 14577 “Linear elastic dynamic instrumented indentation testing DIIT” specifies verification and calibration of testing machines for carrying out the measurement of the dynamic material response when an oscillatory force or displacement, with amplitudes small in comparison to the prescribed target values, is imparted to the indenter while the indenter is continuously loaded to a prescribed target load or target depth or while the load or displacement is held constant at a prescribed target value. In case of a material showing plastic-elastic behavior, the measured dynamic response is used for continuous evaluation of the dynamic stiffness of the contact as a function of depth and frequency. Using the dynamic stiffness of the contact a reduced dynamic modulus will be calculated. In case of a material showing visco-elastic behavior from the measured dynamic response also the dynamic contact damping coefficient as function of depth and frequency is evaluated continuously. Using dynamic contact stiffness and dynamic contact damping coefficient reduced lost and storage modulus for visco-elastic materials will be calculated. The main normative requirements of the draft will be presented and discussed in the light of the first results of the intercomparing excise. T2 - IIW6, International Indentation Workshop 6 CY - Sapporo, Japan DA - 02.07.2018 KW - ISO 14577 KW - Instrumented indentation testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Dynamic testing KW - Visco-elastic KW - Loss module KW - Storage module PY - 2018 AN - OPUS4-45850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -