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Organisationseinheit der BAM
Eingeladener Vortrag
- nein (6)
In the past few years, it has been discussed with increasing frequency, whether cube slip does occur in gamma' hardened nickel-base superalloys. Occurrence of cube slip has consequences for the modeling of orientation dependence of the CRSS. Until now, there are only few experimental investigations.
In principle, cube slip should be possible in primitive cubic lattices (e.g. L12 ordered gamma' phase) but not in face centered cubic ones (e.g. Ni solid solution). The most favourable specimen orientations are near [111], where the Schmid factors for this type of glide exceed those for octahedral systems.
There are two basic methods to detect cube slip: macroscopic slip trace analysis and Transmission electron microscopy (TEM) investigation of the dislocation structure. Few observations of cube slip by macroscopic slip traces are reported in the literature. But it is still uncertain under which test conditions cube slip occurs and what the dislocation mechanisms are. Cube slip was observed during tensile or compression tests of several first generation superalloys, but it seems not to occur during shear creep deformation (e.g. CMSX-4 at 980°C), and it is also lacking under conventional tensile or compression loading, if the gmma' particles are small. No observations were ever reported of dislocations gliding on {001} planes in matrix channels.
Cross-sectional transmission electron microscopy, in combination with energy dispersive X-ray spectroscopy and focused beam microdiffraction, was applied to study the solid-state reactions taking place during contact formation of the system Ge(115 nm)/Pd(50 nm)In0.53Ga0.47As. In order to get information about the sequence of the different processes, rapid thermal, annealing experiments in the range 225400 °C were performed. The following features were observed: at 225 °C Pd reacted with the substrate forming the quaternary phase PdxIn0.53Ga0.47As (x 4), and with the Ge-layer forming mainly PdGe and Pd2Ge. Between PdxIn0.53Ga0.47As and In0.53Ga0.47As, a 5 nm thick amorphous Pd-In-Ga-As layer remained, indicating that the first reaction step was solid-state amorphization. After annealing at 350 °C, PdxIn0.53Ga0.47As disappeared and regrowth of In0.53Ga0.47As occured. Finally, at 400 °C, residual Ge from the amorphous top layer diffused to the interface and grew epitaxially on the regrown In0.53Ga0.47As, thus separating the IIIV compound semiconductor from the Pd-Ge reaction products. The interface remained flat, while only about 10 nm of the active In0.53Ga0.47As layer had been modified during the annealing processes.
XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems
(2002)
The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction. For two typical rapid thermal annealing steps at 750 °C (non-ohmic behaviour) and 850 °C (ohmic behaviour) the intermetallic phases at the metal-semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed.
XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems
(2002)
The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction.
For two typical rapid thermal annealing steps at 750 ◦C (non-ohmic behaviour) and 850 ◦C (ohmic behaviour) the intermetallic phases at the metal–semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed.
X-ray photoelectron spectroscopy (XPS) and cross-sectional transmission electron microscopy (XTEM) were used to study the formation of AlN films by N+2 ion implantation of aluminium at energies of 3 keV and 100 keV. In both cases, a two-stage mechanism was found, comprising first the oriented precipitation of small particles of the hexagonal AlN-phase, followed by growth and coalescence finally forming a continuous AlN-layer while increasing the implantation dose from 1×1017 cm-2 to 2×1017 cm-2. The results of both methods are in excellent agreement and furthermore provide complementary information concerning chemical composition and binding energies as well as microstructural details.
A model based on movable cellular automata has been applied to study the sliding behaviour of tribofilms formed during automotive braking. Since it is not possible yet to determine the composition of real tribofilms quantitatively, final verification of modelling results is needed. This was done by preparing artificial third bodies with compositions and nanostructures matching the ones assumed for modelling. Pin-on-disc tests were performed while applying the artificial third bodies to the contact. The results revealed that not only the structure of the third body but also the amount of the applied normal pressure determines the COF obtained by modelling and that much better correlation between experimental and modelling results was obtained while assuming high normal pressures at asperity contacts.
Untersuchung der Mikrostruktur asbesthaltiger Bremsbeläge und Möglichkeiten der Asbestsubstitution
(2002)
A facile and versatile synthetic route for controlling the size and surface potential of organic–inorganic hybrid silica nanoparticles (NPs) is introduced in this paper. For polymer-grafted NPs, the density of polymer chains on the surface is strongly affected by the concentration of precursor. Nevertheless, for condensed NPs, the precursor concentration determines the particle size but not the density of polymer chains on the surface or the adsorption of bovine serum albumin (BSA). Results presented here may have Major implications in biomedical and colloidal chemistry since interfacial and colloidal properties are known to drive several processes associated with nanoparticles in biological media.
A modified pin-on-disc test was applied to determine tribological properties of typical brake pad constituents. Ball-milling of these ingredients together with iron oxide and graphite provided model materials displaying the main features of real third bodies. Solid lubricants like graphite affected the friction and wear behaviour of Fe3O4 powders considerably whereas further addition of hard nanoparticles induced only minor effects. This was corroborated by comparison with modelling results. MoS2 played a dual role. Depending on special conditions, this ingredient either reduced or increased friction. The latter could be explained, after nanoscopic characterization, by oxidation and destruction of the wear-protecting tribofilm.
The tribological performance of short glass fibers (SGF),solid lubricants and silica nanoparticles filled epoxy (EP) composites was investigated under oil lubrication conditions. It is demonstrated that the addition of SGF greatly reduces the friction and wear of EP. However, further addition of solid lubricants and silica nanoparticles does not change obviously the friction and wear. It is identified that the high tribological performance of SGF reinforced EP is related to the high load carrying capacity and abrasion resistance of SGF. The nanostructure of the tribofilm was comprehensively characterized. It is deemed that the tribofilm plays an important role in the tribological performance by avoiding the direct rubbing of the sliding pairs exposed to boundary and mixed lubrication conditions.
Transmission electron microscopy study of rapid thermally annealed Pd/Ge contacts on IN0.53Ga0.47As
(1996)
Transmission electron microscopy study of rapid thermally annealed Pd/Ge contacts on In0.53Ga0.47As
(1996)
Phase formation in rapid thermally annealed Pd/Ge contacts on In0.53Ga0.47As has been investigated by means of cross-sectional transmission electron microscopy, convergent-beam electron diffraction, and energy-dispersive x-ray analysis. Solid-phase regrowth is observed to occur similarly as in Pd/Ge contacts on GaAs or InP. The reaction starts at low temperatures with the formation of an amorphous Pd–In–Ga–As layer, which crystallizes at elevated temperatures yielding hexagonal Pd4In0.53Ga0.47As being first described in this work. At temperatures .250 °C, this phase decomposes due to epitaxial solid-phase regrowth of In0.53Ga0.47As and formation of Pd–Ge phases. The stable composition is reached at temperatures .350 °C with excess Ge diffused through top Pd–Ge to the contact interface and growing epitaxially on the semiconductor.
Cell cultures form the basis of most biological assays conducted to assess the cytotoxicity of nanomaterials.
Since the molecular environment of nanoparticles exerts influence on their physicochemical properties, it can have an impact on nanotoxicity. Here, toxicity of silica nanoparticles upon delivery by fluid-phase uptake is studied in a 3T3 fibroblast cell line. Based on XTT viability assay, cytotoxicity is shown to be a function of (1) particle concentration and (2) of fetal calf serum (FCS) content in the cell culture medium.
Application of dynamic light scattering shows that both parameters affect particle agglomeration. The DLS Experiments verify the stability of the nanoparticles in culture medium without FCS over a wide range of particle concentrations.
The related toxicity can be mainly accounted for by single silica nanoparticles and small agglomerates. In contrast, agglomeration of silica nanoparticles in all FCS-containing media is observed, resulting in a decrease of the associated toxicity. This result has implications for the evaluation of the cytotoxic potential of silica nanoparticles and possibly also other nanomaterials in standard cell culture.
This work focuses on surface changes induced by repeated brake applications and tries to provide explanations, how such material modifications might affect friction and wear properties of automotive disc brakes. Surface films were investigated locally by transmission electron microscopy (TEM) after having prepared thin cross-sections with a focused ion beam instrument (FIB). Since the observed friction layers revealed a nanocrystalline structure, modelling with the method of movable cellular automata (MCA) was performed by assuming an array of linked nanometer-sized particles. In spite of complicated material combinations at the pad surface, two very characteristic features were always observed at both the pad and disc surface, namely a steel constituenteither ferritic (pad) or pearlitic (disc), partly covered with patches of nanocrystalline iron oxide, on a zone of severe plastic deformation with fragmented grain structure. When using an automata size of 10 nm, reasonable values for the mean coefficient of friction (COF) were obtained, namely 0.35 and 0.85 for oxide-on-oxide and metal-on-metal contacts, respectively. Immediately after brake application mass-mixing and bond-breaking was observed within a narrow zone at both surfaces.
Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales.
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.
The surfaces of a brake pad and rotor were investigated after a run-in period during which a stable coefficient of friction had developed. The Focused Ion Beam Technique (FIB) was used to reveal tribologically induced surface films and for cross-sectional preparation of superficial layers. Additional information was obtained by TEM/EDS of thin lamellae prepared with the FIB and by surface analytical methods (GDOS, XPS and RS). Microscopic contact areas of the pad showed bright contrast in Scanning Ion Microscopy (SIM). This was attributed to severe plastic deformation finally leading to a nanocrystalline microstructure. Metallic particles of the pad, the so-called primary contact areas, were mostly covered with a smooth oxide layer of less than 1 µm thickness. Above this layer a thin (100 nm) partly amorphous film was often observed. The film was not only restricted to the metal particles, but also spread over adjacent regions, suggesting that secondary plateaus had formed. Similar layers and films, although with slightly different composition and structure, were also observed at the surface of the rotor.
The topographic effect of steel counterface, finished by mechanical grinding with Ra ranging from 0.01 to 0.95 µm, on the structure and functionality of the tribofilm of a hybrid nanocomposite, i.e. epoxy matrix filled with monodisperse silica nanoparticles, carbon fibers and graphite, was systematically investigated. The nanostructure of the tribofilm was comprehensively characterized by using combined focused ion beam and transmission electron microscope analyses. It was identified that oxidation of the steel surface, release, compaction and tribosintering of silica nanoparticles and deposition of an epoxy-like degradation product as well as fragmentation of carbon fibers are main mechanisms determining the structure and functionality of the tribofilm. The size of roughness grooves determines the type and size class of wear particles to be trapped at the surface. An optimum groove size leading to a maximum of surface coverage with a nanostructured tribofilm formed mainly from released silica nanoparticles was identified.
This review article comprises of three parts. Firstly, reports of brake manufacturers on the beneficial impact of solid lubricants for pad formulations are surveyed. Secondly, since tribofilms were identified to play a crucial role in friction stabilization and wear reduction, the knowledge about tribofilm structures formed during automotive braking was reviewed comprehensively. Finally, a model for simulating the sliding behavior of tribofilms is suggested and a review on modelling efforts with different model structures related to real tribofilms will be presented. Although the variety of friction composites involved in commercial brake systems is very broad, striking similarities were observed in respect to tribofilm nanostructures. Thus a generalization of the tribofilm nanostructure is suggested and prerequisites for smooth sliding performance and minimal wear rates have been identified. A minimum of 13 vol.% of soft inclusions embedded in an iron oxide based tribofilm is crucial for obtaining the desired properties. As long as the solid lubricants or their reaction products are softer than magnetite, the main constituent of the tribofilm, the model predicts smooth sliding and a minimum of wear.
The role of grain size and ferrite substructure in respect to mechanical properties of an HSLA steel
(1986)
Several heat treatments were applied to an HSLA steel on type StE460 (German standard) to produce four ferrite substructures of different strength and at least two different grain sizes respectively. Whereas the ferrite substructure has a strong influence on yield strength the effect of grain size was negligible though probably to some extent masked by different pearlite volume fractions. The different strength levels could be explained by regarding the arrangement of dislocations and vanadium carbonitride particles and their mutual interaction. Increasing both grain size and pearlite volume fraction leads to a remarkable shift of transition temperature T sub 27J which was further enhanced by increasing ferrite strength. 16 ref.--AA
Excellent tribological properties of an advanced polymer matrix composite were obtained by a combination of micro- and nano-sized fillers. Surface features and the nanostructure of tribofilms were characterized by advanced microscopic techniques, and correlated with the macroscopic behavior in terms of wear rate and friction evolution. A model based on movable cellular automata was applied for obtaining a better understanding of the sliding behavior of the nanostructured tribofilms. The failure of the conventional composite without silica nanoparticles could be attributed to severe oxidational wear after degradation of an initially formed polymer transfer film. The hybrid composite preserves its antiwear and antifriction properties because flash temperatures at micron-sized carbon fibers, lead to polymer degradation and subsequent release of nanoparticles. It has been shown that the released particles are mixed with other wear products and form stable films at the disc surface thus preventing further severe oxidational wear. Furthermore, the released wear product also is embedding carbon fibers at the composite surface thus preventing fiber fragmentation and subsequent third body abrasion. With nanoscale modelling we were able to show that low friction and wear can be expected if the nanostructured silica films contain at least 10 vol.% of a soft ingredient.
The focused ion beam technique - eine interessante Alternative, auch für konventionelle Werkstoffe
(2002)
TEM study on the effect of machining on the microstructure of a soft magnetic Ni76Fe17Cu5CrMo2 alloy
(1991)
Synthesis and characterisation of highly fluorescent core-shell nanoparticles based on Alexa dyes
(2012)
Current and future developments in the
emerging field of nanobiotechnology are closely
linked to the rational design of novel fluorescent
nanomaterials, e.g. for biosensing and imaging applications.
Here, the synthesis of bright near infrared
(NIR)-emissive nanoparticles based on the grafting
of silica nanoparticles (SNPs) with 3-aminopropyl
triethoxysilane (APTES) followed by covalent attachment
of Alexa dyes and their subsequent shielding by an
additional silica shell are presented. These nanoparticles
were investigated by dynamic light scattering (DLS),
transmission electron microscopy (TEM) and fluorescence
spectroscopy. TEM studies revealed the monodispersity
of the initially prepared and fluorophorelabelled
silica particles and the subsequent formation of
raspberry-like structures after addition of a silica
precursor.Measurements of absolute fluorescence quantum
yields of these scattering particle suspensions with
an integrating sphere setup demonstrated the influence
of dye labelling density-dependent fluorophore aggregation
on the signaling behaviour of such nanoparticles.
Silver nanoparticles were generated based on citrate reduction in the ultrastructure of the sporopollenin biopolymer of Ambrosia artemisiifolia (ragweed) and Secale cereale (rye). The nanoparticles enable the acquisition of SERS spectra and thereby a vibrational characterization of the local molecular structure of sporopollenin.
Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity.
Many performance properties of devices or interacting machine parts are related to superficial layers which often show completely different or at least modified microstructures compared to the bulk materials. A quasi non-destructive technique will be described which enables us to obtain detailed information of a material's state at a certain site of interest down to a depth of 10 µm from the surface with nanometre or even atomistic resolution.
Third bodies, also termed friction layers, tribofilms or secondary contact patches, are layers of more or less compacted wear debris between pads and rotor of a disc brake. Our approach of assessing the sliding behavior and friction properties induced by third bodies has been: i) structural characterization after AK-master test procedure, ii) sliding simulation of model structures similar to the observed ones but with simpler and well defined compositions, and iii) verification of simulation results by pin-on-disc tests with artificial third bodies showing the same microstructures and compositions as the model structures. The idea was to simulate structure formation during real braking conditions by high energy ball milling of appropriate powder blends. The final outcome of numerous parameter studies was that a third body containing 15 vol% soft ingredients and 0-20 vol % hard ingredients, both distributed homogeneously in a nanocrystalline iron oxide matrix, should be most desirable for braking. This general description of the optimum third body structure and several parameter studies performed by modelling enabled us to interpret a number of features of the AK-master test procedure, such as i) friction evolution during bedding, ii) the role of solid lubricants in respect to the initiation of smooth sliding behavior, and iii) friction evolution during a single braking event (in-stop behavior).
Copper is one of the most important components in brake pads and its amount can reach up to 14%. In spite of a number of positive features copper usage in brake pad formulations has recently become the subject of considerable discussions, primarily due to concerns about potential risks related to environmental impacts of copper particles. So, for developing new pad formulations with possible replacements of copper content, it is very important to understand the functionality of copper additions to brake friction materials. In the paper theoretical investigation of the role of copper as a pad ingredient was carried out on the basis of modelling by the method of movable cellular automata (MCA). Our previous studies show that copper as a constituent of the tribofilm formed during braking provides smooth sliding by forming a granular layer of mechanically mixed materials from the friction layers. In the present study the concentration of copper particles in a Fe3O4-matrix was varied systematically in the range 5.5-28 vol. % and compared to mixtures with the same amount of graphite nanoparticles. The sliding simulations were performed while assuming material properties at 500°C in order to assess the beneficial role of copper during severe braking conditions corresponding to fading cycles during dynamometer testing.
Copper is one of the most important components in brake pads and its amount can reach up to 14%. In spite of a number of positive features copper usage in brake pad formulations has recently become the subject of considerable discussions, primarily due to concerns about potential risks related to environmental impacts of copper particles. So, for developing new pad formulations with possible replacements of copper content, it is very important to understand the functionality of copper additions to brake friction materials. In the paper theoretical investigation of the role of copper as a pad ingredient was carried out on the basis of modelling by the method of movable cellular automata (MCA). In the study the concentration of copper particles in a Fe3O4-matrix was varied. The sliding simulations were performed while assuming material properties at 500 degrees C in order to assess the beneficial role of copper during severe braking conditions corresponding to fading cycles during dynamometer testing.
The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale.
REM-Untersuchung des Oxidschichtwachstums auf der einkristallinen Nickelbasis-Superlegierung SRR 99
(2001)
Recent progress in the development of A1GaN/GaN heterostructure field effect transistors (HFETs) Shows the great potential towards high temperature / high power electronics. Nevertheless investigations on reliability properties of GaN-based devices are still at the beginning. The frequently used Ti/A1 based ohmic and Pt based Schottky contacts suffer from strong Degradation after aging at elevated temperatures. Therefore new contact systems have to be employed. Concerning the source and drain metallization we used an amorphous WSiN barrier layer as applied for GaAs on top of the Ti/Al-based ohmic contact. This technique significantly reduces the in-diffusion of the Au-containing overlayer, furthermore the barrier layer guaranties smooth contact morphology after RTA and aging, respectively. For the Schottky metallization the Ir/Au system was used. Reliability studies performed on HFET devices containing refractory Ti/A1/Ti/Au/WSiN ohmic and Ir/Au Schottky contacts demonstrate stable conditions during 120h aging at 500°C.
Reference nanomaterials
(2016)
This chapter reviews relevant aspects of the still less explored field of RNMs. In the first part, definition of RMs according to different metrological levels was presented as well as the general strategy on their development. In the second part, the importance of RNMs in material science and nanotoxicology is explained and considerations on the use of silica nano-objects as potential future reference material was discussed. Overall, several points should be highlighted from this chapter: Definition of a reference material depends on the level of standardization. Certified reference material represents the highest level of traceability. Different types of reference materials, standard materials and certified reference materials are available, as shown in Table 3.1. The preparation of nano-objects with well-defined mechanical properties is still an unsolved issue and thus needs further R&D activities. Nevertheless, amorphous silica seems to be a promising candidate for reaching this objective. Traceable properties of nanomaterials are still limited to few cases such as primary particle size and thickness measurements of very thin films. In general, developed RMs are monoparametric thus, only one characteristic of the nano-objects is reported. In nanotoxicology, the challenge is in the development of suitable RNM that bears similarities to the measurements made on the sample analysed.
The tribological performance of a hydrogenated amorphous carbon coating on Ti6Al4V against ceramic balls was checked by simple reciprocating sliding tests and by more complicated tests in a hip joint simulator. 3 of 4 joints failed during hip simulator testing already after approximately 100 × 10³ cycles and possibly due to coating failures caused by insufficient polishing of the metallic acetabular cups prior to coating deposition. Since such failures occurred only occasionally, the problem was not revealed by reciprocating sliding tests which are stressing a much smaller surface area compared to the tests in the hip joint simulator. Another type of failure, pits of 12 µm in diameter distributed randomly at the coating surface, was frequently observed by Scanning Electron Microscopy and analyzed comprehensively by Focused Ion Beam technique in combination with Transmission Electron Microscopy in one case. Although not necessarily affecting wear, such small failures might cause long-term problems in vivo, by providing access of body fluid to the substratecoating interface making it susceptible to corrosion.
The resistance of structural steels against corrosion in CO2-H2O and CO2-H2O-O2
atmospheres at temperatures above 550°C was observed with high magnification methods.
The test atmosphere is the basic composition of an oxyfuel coal combustion atmosphere. The
analytical information base was applied to develop reaction schemes for the oxidation of
steels. It was demonstrated that the formation of phases and the kinetics of oxidation reactions
in this atmospheres is affected by the formation of intermediate iron hydroxide and a high
carbon activity. In the temperature regime above 550°C the thermal equilibrium between H2O,
CO2 and Fe reacted and formed CO. CO triggers the formation of FeO and carbides and
increases the reaction kinetics. Porosity at the interface is established by gaseous phases
such as Fe(OH)2 or H2O. H2 formation is not limited to the steel - oxide interface but can occur
in the whole oxide scale. Examples of the experimental results were compared with a
thermodynamic approach. The objective of the work was to derive qualitative rules of the basic
corrosion reactions.
8 wt% Y2O3-ZrO2 spray powder and thermally sprayed as thermal barrier coatings on outer air seals were characterized by Raman microprobe spectroscopy (RMS) and transmission electron microscopy to investigate the lateral distribution, composition, structure and grain size of ZrO2 phases and to separate ZrO2 and Y2O3. RMS of transfer layers on ZrO2-coated shrouds after rub tests against SiC laser-tipped metallic blades showed the formation of metallic oxides MeIMeII2O4 of spinel type. Wear tracks were partly covered by graphite and spinel-type oxides. In some cases, the latter were better detectable after laser enhanced cleaning by burning off the covering carbon layer.
Platinum does not form any adherent oxides and can be easily wetted by tin-based solders. Platinum is also an available metallization in semiconductor laboratories. Therefore we investigated the diffusion of platinum thin-film metallizations into eutectic tin–lead solder by using a high-resolution secondary ion mass spectroscopy (SIMS) profiling from the back side. It is shown that an intermetallic phase (PtSn4) is formed during soldering, which controls the consumption of platinum during soldering and in operation. The consumption of platinum follows the well-known parabolic diffusion law. The activation energy of this process is 0.63 eV. Even at extended heating cycles of 2 min at 250°C, 190 nm from the original 300 nm of the platinum film remain undissolved. This high stability makes platinum a very attractive thin-film metallization for flip-chip (FC) bonding of new microsystems.
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.
The tribological properties of nanostructured surface films formed during dry sliding, for example during
automotive braking, were determined by modelling using the method of movable cellular automata.
Starting from a basic model structure, consisting of magnetite with 13% graphite inclusions, the impact of
additional soft and hard particles of different size and volume fraction was studied systematically. It was
revealed that agglomerates of soft particles decomposed and finally mixed with the oxide in the same
way as single nanoparticles. On the other hand, agglomerates of hard particles mixed with the other
components without decomposing. Whereas increasing the amount of soft components in the third body
lowered the coefficient of friction, the opposite occurred with the hard particles. The boundary conditions
for obtaining smooth sliding conditions with minor fluctuations between friction forces at successive time
steps could be defined. In addition to features of the nanostructure, the applied normal pressure
impacted modelling results. Within the parameter range of smooth sliding behaviour, increasing pressure
induced thicker granular interface layers, which lead to a slight decrease of the coefficient of friction.
Changing the amount of soft or hard particles did not change this pressure dependency but only the
friction level.
NM 105, Ti02 (P25) could not be ignited as dust layer and dispersed in air as dust/air-mixture as well. This dust is not dust explosible and the burning behaviour corresponds to Burning Class 1 (no Ignition). The results have shown that the tested sample is thus not combustible at all, because it is already oxidized completely.
Phasenbildung in Metall-Halbleiterkontaktschichten und Präparationstechnik für TEM-Untersuchung
(1995)
Weld metal microstructure for alloy 6060 aluminum welds, made using the gas-tungsten arc process and alloy 4043 filler metal, has been characterized using optical metallography, EPMA microprobe analysis, SEM/EBSD and STEM/EDX electron microscopy, and single-sensor differential thermal analysis (SS-DTA). In addition, alloy 6060 castings were solidified at variable cooling rates approaching that of welding, to provide a reference for comparison with weld microstructure. It was found that a major change in cast microstructure occurs at cooling rates higher than 27 K/s resulting in a structure similar to that observed in weld metal. Rapid cooling is believed to favor low temperature solidification reactions that normally would be achieved only at higher silicon content. Accordingly, additions of 4043 filler metal that increase the weld metal silicon content have only limited affect on weld solidification range and microstructure. This has direct implications regarding how 4043 filler additions improve weldability and weld quality.
The development of two metallizations based on the solid-phase regrowth principle is presented, namely Pd/Sb(Zn) and Pd/Ge(Zn) on moderately doped In0.53Ga0.47As (p=4×1018 cm-3). Contact resistivities of 23×10-7 and 67×10-7 ?cm2, respectively, have been achieved, where both systems exhibit an effective contact reaction depth of zero and a Zn diffusion depth below 50 nm. Exhibiting resistivities equivalent to the lowest values of Au-based systems in this doping range, especially Pd/Sb(Zn) contacts are superior to them concerning metallurgical stability and contact penetration. Both metallizations have been successfully applied for contacting the base layer of InP/In0.53Ga0.47As heterojunction bipolar transistors.
The need for a better understanding of nanoparticleprotein interactions and the mechanisms governing the resulting colloidal stability has been emphasised in recent years. In the present contribution, the short and long term colloidal stability of silica nanoparticles (SNPs) and silica–poly(ethylene glycol) nanohybrids (Sil–PEG) have been scrutinised in a protein model system. Well-defined silica nanoparticles are rapidly covered by bovine serum albumin (BSA) and form small clusters after 20 min while large agglomerates are detected after 10 h depending on both particle size and nanoparticle–protein ratio. Oppositely, Sil–PEG hybrids present suppressive protein adsorption and enhanced short and long term colloidal stability in protein solution. No critical agglomeration was found for either system in the absence of protein, proving that instability found for SNPs must arise as a consequence of protein adsorption and not to high ionic environment. Analysis of the small angle X-ray scattering (SAXS) structure factor indicates a short-range attractive potential between particles in the silica-BSA system, which is in good agreement with a protein bridging agglomeration mechanism. The results presented here point out the importance of the nanoparticle surface properties on the ability to adsorb proteins and how the induced or depressed adsorption may potentially drive the resulting colloidal stability.
Copper is a major ingredient in friction materials used for automotive braking. The purpose of this study was to find out how copper contributes to good brake performance properties in addition to providing good thermal conductivity. Microstructural investigations of copper chips at the surfaces of brake pads revealed a zone of severe plastic deformation which provides high hardness, but there is also evidence of recrystallized copper nano-particles which are incorporated into friction layers as soft ingredient once detached from the pad surface. Thus copper seems to play a dual role, firstly as reinforcing element of the brake pad providing primary contact sites, and secondly as solid lubricant by contributing to the formation of a layer of granular material providing velocity accommodation between the rotating disc and fixed pad. Confirmation for this hypothesis was obtained by modelling contact sites on the nanometre scale with the method of movable cellular automata. Results show both, the similarity of steel fibres and copper macro-particles in respect to providing primary contact sites, as well as similar sliding behaviours of friction layers containing either copper or graphite as soft inclusions. Furthermore, it is shown that not only material properties, but also the concentration of solid lubricant particles in the friction layers, determine conditions for friction force stabilization and smooth sliding behaviour.
In the paper, a model typical for contact situations of automotive brakes is established based on the method of movable cellular automata. The processes taking place at local contacts in an automotive brake system are analysed. Based on microscopic and micro-analytical observations, the following contact situations were simulated: (i) a couple of ferritic steel against pearlitic steel, both covered by an oxide layer mixed with graphite nanoparticles and (ii) the same situation but without oxide layers. The results of calculated mean coefficients of friction of the oxide-on-oxide contact correspond well to expected values for a real braking system, whereas steel-on-steel contact are twice as high. This allows one to make some conclusions; for example, oxide formation will take place more quickly than friction layer elimination, and finally this is responsible for the stabilisation of the coefficient of friction.
The formation of AlN films prepared by N+2 ion implantation into aluminium was investigated using X-ray and Auger photoelectron spectroscopy ( XPS, AES) as well as cross-sectional transmission electron microscopy (XTEM). After 100-keV N+2 implantation of low doses (1×1017 cm−2), the formation of hexagonal AlN nanocrystals (crystal size <5 nm, Ncrystal=1017 cm−3) was observed. Their orientation is strongly correlated with the aluminium matrix. With the dose increasing to 3×1017 cm−2, crystal growth follows, finally forming a homogeneous AlN-layer. Furthermore, the diffraction patterns show an increasing amount of misorientation with increasing dose. From the crystal size distribution, we conclude that continuous nucleation takes place. Samples implanted with an energy of 3 keV exhibit analogous behaviour. Nitride growth was further investigated using microstructured AlN formed by 3-keV implantation through movable TEM-masks (structure size: 15–150 mm).
In the case of high N+2 doses (D&5×1017 cm−2), AlN is detected by AES in the shielded area at a distance of up to 10 mm from the exposed region. The Diffusion coefficient was calculated to be 10−10 cm2 s−1. The formation of AlN proceeds in two steps.
After a continuous nucleation, diffusion-assisted Crystal growth takes place until a homogeneous AlN layer results.
The method of movable cellular automata (MCA) and method of molecular dynamics (MD) were applied to simulate the friction and sliding behavior of model-tribofilms formed from a nanocomposite consisting of an epoxy matrix, 10 vol % micron-sized carbon fibers and 5 vol. % silica nanoparticles. Whereas MCA considered the tribofilm as an agglomerate of silica nanoparticles released from the composite and mixed with graphite particles, MD simulated the sliding behavior of an amorphous silica layer supported by stiff crystalline substrates on both sides. The MCA model provided reasonable quantitative results which corroborate experimental findings at moderate stressing conditions. The very low coefficient of friction observed experimentally under severe stressing conditions was not explained by this model. This could be attributed to the lack of mechanical data at the high temperature expected under these conditions. Although based on a simpler assumption of the tribofilm composition, MD-modelling could be easily applied to the expected high flash temperature and was able to predict friction reduction and smooth sliding under these conditions.
A major requirement for the validation of methods assessing the risk associated with engineered nanoparticles (ENPs) is the use of reference materials (RMs). In the present contribution we review available RMs, ongoing projects and characterisation trends in the field. The conclusion is that actual approaches to RMs mostly deal with metrological considerations about single properties of the ENPs, typically their primary size, which can hardly be representative of nanoparticles characteristics in real testing media and therefore, not valid for reliable and comparable toxicological studies. As an alternative, we discussed the convenience and feasibility of establishing multi-parametric RMs for a series of ENPs, focusing on silica nanoparticles (SNPs). As a future perspective, the need to develop RMs based on hybrid nanoparticles is also discussed.
In the paper by using molecular dynamics method we investigate behavior of nickel-phosphorus compound in amorphous-like state under conditions of shear loading at the constant velocity. Samples with an amorphous layer of pure nickel and nickel-phosphorus compound were considered. The analysis showed that forces of shear resistance in the sample with an amorphous layer containing phosphorus in about 3 times less than the sample with a layer of pure nickel. Thus, it was shown that nickel-phosphorous coating in amorphous-like state may exhibit low friction properties, and, therefore, serve as the solid lubricant material.
The sliding behavior of an amorphous silica sample between two rigid surfaces is in the focus of the present paper. Molecular Dynamics using a classical Tersoff’s potential and a recently developed ReaxFF potential was applied for simulating sliding within a thin film corresponding to a tribofilm formed from silica nanoparticles. The simulations were performed at different temperatures corresponding to moderate and severe tribological stressing conditions. Simulations with both potentials revealed the need of considering different temperatures in order to obtain a sound interpretation of experimental findings. The results show the striking differences between the two potentials not only in terms of magnitude of the resistance stress (about one order of magnitude) but also in terms of friction mechanisms. The expected smooth sliding regime under high temperature conditions was predicted by both simulations, although with Tersoff’s potential smooth sliding was obtained only at the highest temperature. On the other hand, at room temperature Tersoff-style calculations demonstrate stick-slip behavior, which corresponds qualitatively with our experimental findings. Nevertheless, comparison with a macroscopic coefficient of friction is not possible because simulated resistance stresses do not depend on the applied normal pressure.
The impact of pressure, sliding velocity and property variation of constituents on the sliding behaviour of a model tribofilm was studied with the method of movable cellular automata (MCA). Whereas a clear pressure dependency of the coefficient of friction (COF) was always observed and could be correlated with the structure formation in terms of varying thickness of a mechanically mixed layer, the impact of the other parameters was either negligible or rather weak. Only if a brittle-to-ductile Transition of the oxide-based tribofilm was assumed, a significant decrease in the COF level was predicted.
Temperature-dependent property changes can be neglected during MCA modelling, unless this transition takes place. For magnetite-based tribofilms, the transition temperature is beyond 800 °C, i.e. a temperature leading to fading effects during braking anyway. Thus, it could be concluded that, except for very severe braking conditions, sliding simulations with the MCA method yield meaningful results without considering temperature-dependent mechanical properties.
In the mechanical friction and wear process, normal and tangential (shear) forces cause elastic and plastic deformations, generate cracks and form loose wear particles through fracture processes. Depending on the working conditions, the material properties and the real contact Situation (topography), a third body is formed as a mechanical ly mixed layer, which determines different running-in and steady-state behaviours.
Two dimensional (2D) MCA Simulation results will be described via empirical equations, which are related to the incubation time (period without wear) and the following running-in wear rate (kinetic concept of strength, fatigue wear model).
In order to understand the running-in and steady-state wear, kinetic model equations for mass balance of the third body are useful and are therefore to be included in the investigation.
For a more complex material behaviour, numerical Simulation results are also presented for friction at the pad-disk interface of automotive brakes.
The method of movable cellular automata (MCA) was applied to simulate the stress-strain behavior of a nano composite consisting of an epoxy matrix and 6 vol. % silica nano particles. The size of the elements used for modelling was fixed at 10 nm, corresponding approximately to the diameter of the filler particles. Since not only the stress-strain response of the two constituents but also debonding of neighboring particles and granular flow was taken into account, plastic deformation as well as crack initiation and propagation could be simulated with the model. Modelling results were compared with tensile test results of both, pure epoxy as well as the epoxy-6 vol. % SiO2 composite. Since assuming bulk properties of the two constituents did not yield satisfactory results, slight modifications of the nanoparticle response functions and nanostructures were tested numerically. Finally, it was observed that only the assumption of slightly increased strength properties of the epoxy yielded good correlation between experimental and modelling results. This was attributed to an increased cross linking of the epoxy caused by the presence of silica nano particles.
The frictional behavior at local contacts in an automotive brake system was analysed on the basis of computer simulation by movable cellular automata method. The boundary conditions of the model were adjusted to experimental observations obtained by TEM. The model proved to be adequate for simulating mechanical mixing and velocity accommodation at the pad-disc interface. Dynamics of particle interaction were visualized by showing rotation angles and velocity vectors. The model provided information on the development of plastic deformation for metal-on-metal contacts and on crack formation at graphite lamellae of cast iron disc. Results are in agreement with conventional friction theories.
The microstructures of two samples of a Zr(C,N) coating on steel, which unexpectedly differed in their tribological properties, were investigated by analytical transmission electron microscopy. The samples were produced by a cathodic arc evaporation process in two commercial coating devices under similar coating conditions with the exception of the number of Zr targets.
The source of the differing tribological properties of the samples was detected by analytical transmission electron microscopy (TEM) methods energy-dispersive X-ray spectroscopy (EDX), energy filtering TEM (EFTEM), electron diffraction, high resolution electron microscopy, and high angel annular dark field. The TEM preparation and the results of the TEM investigations are shown in detail. The origin of the unexpected behavior was determined to be a nano-scale multilayer structure that existed only in the tribologically superior specimen. EDX and EFTEM investigations indicated enrichment in oxygen at the interface between coating and steel substrate in the tribologically inferior sample. Findings of the microstructural configuration were obtained by taking a closer look at the structure and comparing the results of the several analytical TEM techniques. This allows the allocation of the concentration fluctuations in N, C, and Zr to the two thickness fractions of the nano multilayers and a local correlation of the identified minority phase Zr3(C,N)4 to the higher N content in the narrower type of the multilayer fraction of the sample with the excellent tribological properties. The minority phase Zr3(C,N)4 is randomly distributed in the sample with the defective tribological properties.
Coating conditions are not topic of this work, but after discussion of the TEM results, the fact that one of the coating devices worked with one Zr target and the other one with two, could be identified as cause for the formation of the nano multilayer structure in the sample with the superior tribological properties.