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Eingeladener Vortrag
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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.
In the last years, a lot of research work has been performed in the field of surface coatings and thin films technology, often supported by governmental research programs, as i.e. in Germany, the Thin Film Technology and OSTec research programs. But up until now, there is still a lack in transfer of this large amount of knowledge created by research activities on to industrial application and commercialization. To overcome this problem, a new web based information system has been developed (http://www.schichttechnik.net), which in a first step will make the whole content of the German OSTec research program (approx. 180 research reports) of the last 10 years available. In further steps, data from products of coating suppliers and other research programs will be taken into account. The database contains the following sections: definition of the coating system, deposition equipment, deposition processes, application properties, test procedures and test equipment, information about standardization and base information about coating processes etc. It will be possible to search for coatings by material properties and functions of coatings, considering also restriction on the substrate. In addition, searching regarding combination of properties, e.g. for wear-resistant, conductive, decorative coatings etc. will also be possible.
TiN hard coatings have been prepared by unbalanced magnetron (UBM) sputtering and cathodic arc deposition using uni- and bipolar pulsed bias voltages. For UBM sputtering using a unipolar pulsed bias voltage the average substrate bulk temperature Ts was reduced to 220 °C without considerable loss of microhardness and adhesion by variation of the pulse parameters. Determination of the average energy Ep delivered to the growing film per deposited particle leads to values lower than the critical transition energy (150 eV atom-1) between open porous and dense coatings. Using a bipolar pulsed bias voltage Ts decreased with increasing duration ton+ of the positive bias pulse. It was found that Ep increased with increasing ton+ up to values found for d.c. bias voltage. The coatings prepared using a bipolar pulsed bias voltage at low Ts are dense and in compressive stress with acceptable microhardness and adhesion. First results of the investigation of TiN coatings prepared by cathodic arc deposition using unipolar pulsed bias are given.
An attempt was undertaken to obtain a better understanding of the tribological properties of two wear-resistant coatings on tool steel by structural and microchemical analysis of wear particles using a transmission electron microscope. Coatings were deposited by physical vapor deposition and plasma-assisted chemical vapor deposition techniques and tribological properties were derived from reciprocating sliding tests of the coatings against alumina balls. Three types of wear particles were identified by electron diffraction and energy dispersive X-ray spectroscopy: nanocrystalline rutile (TiO2), nanocrystalline graphite and microcrystalline graphite. Low coefficients of friction, of the order of 0.2, were attributed to the formation of solid lubricant films of sub-stoichiometric TiO2-x Magnéli phases and/or graphite.
The chemical and microstructural changes occurring during braking simulation tests at the surface of a conventional brake pad material were investigated mainly by scanning and transmission electron microscopy and surface analytical techniques. It can be shown that patches of a third body material develop, comprising a compositional mix of all constituents of the pad and iron oxides from the disk. Milled debris particles still have the crystal structure of barite, the major phase of the pad material, but the grain size is reduced drastically to the nanometer scale. The major wear mechanism is delamination of filler particles from the organic binder, supported by local degradation of the phenolic resin during asperity heating. Quartz crystals are preserved thereby adopting the function of primary contact areas.
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.
BAM Certified Reference Materials for Nano-metrology: Preparation, Charcterisation and Certification
(2004)
The irradiation of ~0.9-µm-thick hydrogenated amorphous carbon (a-C:H) layers deposited on silicon substrates with single femtosecond (fs) laser pulses (35 fs pulse duration, 790 nm centre wavelength) in air is studied experimentally. Irradiation spots have been generated with different peak fluences and subsequently investigated by optical topometry, micro Raman spectroscopy and microscale mechanical indentation in order to evaluate their microscopic, topographical, structural and mechanical properties (e.g. elastic modulus). By this multi-method approach, a clear separation of different effects (delamination and graphitisation) becomes possible. The joint application of mechanical and spectroscopic techniques provides unique insights into the effects of the fs-laser radiation on the carbon layer.
Tribological screening tests (simple, reciprocating ball-on-flat tests) were performed with the objective to identify an appropriate coating for the articulating surfaces of artificial hip joints whose acetabular cups and femoral stems are made from Ti6Al4V alloy, which is appreciated for its light weight, good biocompatibility and elastic properties similar to those of natural bone. Standard coatings like TiN or CrN performed better than more complicated multi-layer systems, though not as good as different types of amorphous carbon coatings, generally referred to as diamond-like carbon or DLC coatings. Among the latter, hydrogenated amorphous carbon (a-C:H) displayed the best properties, especially if the hydrogen content was increased by reducing the bias voltage during PA-CVD-deposition.
The optimised a-C:H coating revealed the most promising wear behaviour under the applied testing conditions, i.e. the increase of linear wear with the number of cycles was close to zero. Regarding the materials examined in this study, correlation of wear with mechanical properties obtained by nano-indentation revealed that high hardness was not an adequate criterion for selecting appropriate coatings. A high ratio of hardness and elastic modulus (H/E) proved to be more important. Microstructural and micro-analytical investigations revealed transformation of TiN and CrN to TiO2 and Cr2O3, respectively, and amorphous carbon was, at least partly, transformed to graphite. Furthermore, incorporation of Al2O3 from the ball was observed at a very fine scale. The wear debris of favourable coatings always formed agglomerates of nano-scale particles. It was shown that commercial nano-particles of Al2O3, Cr2O3 and carbon black are comparable to particles generated by the tribological tests. However, it is uncertain whether they are comparable to those formed during simulator studies or in vivo. Furthermore, the performance of the favourable coating has to be tested in a hip joint simulator before its potential for application in prostheses can be assessed.
Modified Yoldas sols can be used to prepare crack-free well adherent layers on different substrate materials such as sodalime glass, corundum and metal (IN-718). These layers having thicknesses of 0.6 µm are strain tolerant and withstand thermal cycling between 810 °C and room temperature. Introducing alpha-Al2O3 filler particles into modified Yoldas sols allows the preparation of thicker layers of 1.6 µm, which as well can be thermally cycled without noticeable delaminations. Chemical bonding seems to be the predominant layer bonding mechanism.
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).
A calibration procedure for the detection efficiency of energy dispersive X-ray spectrometers (EDS) used in combination with scanning electron microscopy (SEM) for standardless electron probe microanalysis (EPMA) is presented. The procedure is based on the comparison of X-ray spectra from a reference material (RM) measured with the EDS to be calibrated and a reference EDS. The RM is certified by the line intensities in the X-ray spectrum recorded with a reference EDS and by its composition. The calibration of the reference EDS is performed using synchrotron radiation at the radiometry laboratory of the Physikalisch-Technische Bundesanstalt. Measurement of RM spectra and comparison of the specified line intensities enables a rapid efficiency calibration on most SEMs. The article reports on studies to prepare such a RM and on EDS calibration and proposes a methodology that could be implemented in current spectrometer software to enable the calibration with a minimum of operator assistance.
Silica coatings filled with nanoscaled inorganic fullerene-like tungsten disulphide (IF-WS2) have been prepared through a solgel 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 150360 °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 1.54 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.
The accuracy and comparability of nanoindentation results depend significantly on the calibration of area function and instrument compliance. The area function results should not depend on the reference material used or on the calibration method (direct or indirect). This has been investigated for 18 different Berkovich tips. A novel calibration method is proposed that confirms the material independence of the area function and gives a force-dependent instrument compliance function. An agreement between direct and indirect calibration could only be achieved by considering a radial displacement correction. Further, it is shown that the transition range from a spherical cap to the correct face angle of the pyramid can extend to a depth of more than 250 nm. A better parameter for the indenter than the tip radius is the offset of the contact radius to the radius of an ideal tip at a depth where the correct face angle is reached.
An extensive comparison between the conventional Vickers hardness at 500 mN and indentation hardness measured with Vickers indenters at 500 mN is presented for up to 20 different materials and for three different instruments. Additionally, the indentation modulus is compared to Young’s modulus, which was measured with alternative methods or taken from the literature. It is shown that the agreement between the results from depth-sensing indentation and the reference values can be improved by additional corrections, for the calculation of the indentation area. With corrections the mean hardness difference to the Vickers hardness reference as average of all investigated materials can be reduced to about 10 % although disturbing pile-up or sink-in effects can still not be considered. For the modulus, the mean difference was only about 6 %.
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.
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.
Möglichkeiten und Grenzen der Bestimmung mechanischer Eigenschaften von Kombinationsschichten
(2011)
Der Vortrag widmet sich der Kratzbeständigkeit-Prüfmethoden und deren Bewertung und beschreibt Begriffe/Definitionen, Wirtschaftliche Bedeutung der Kratzbeständigkeit, Mess- und Prüfverfahren – allgemein (Anwendbarkeit, Messunsicherheit, Validierung), Mess- und Prüfverfahren – speziell die Erzeugung, Prüfverfahren von Einzel- und Vielfach-Kratzern, die Charakterisierung von Verkratzungen und eine zusammenfassende Bewertung im Einzelnen
Der Vortrag widmet sich dem „RITZ-TEST: EVALUIERUNG UND STAND DER NORMUNG“ und beschreibt die Komponenten, Ergebnis und Messgrößen, nicht registrierende Prüfgeräte, Evaluierung Ritz-Test (Makrobereich), den Atlas der Versagensformen, Geräte für den instrumentierten Ritz-Test und die Normung des Ritz-Tests (ASTM) zur Bewertung der Haftfestigkeit“ im Einzelnen.