Filtern
Erscheinungsjahr
Dokumenttyp
- Zeitschriftenartikel (104)
- Beitrag zu einem Tagungsband (23)
- Beitrag zu einem Sammelband (18)
- Vortrag (3)
- Buchkapitel (2)
- Forschungsbericht (2)
- Sonstiges (1)
Sprache
- Englisch (153) (entfernen)
Schlagworte
- Third body (13)
- Tribofilm (12)
- Friction (8)
- Nanoparticles (8)
- Friction layer (6)
- Sliding simulation (6)
- TEM (6)
- Movable cellular automata (5)
- Nanostructure (5)
- Automotive braking (4)
Organisationseinheit der BAM
Eingeladener Vortrag
- nein (3)
Optical and electron metallography have been used to investigate the development of different microstructures in Armco Fe after rolling reductions between 0 and 90%. Simultaneously, the orientation distribution functions have been calculated from pole figures obtained by X-ray diffraction. Different stages of texture development could be assigned to typical microstructures. Strain inhomogeneities, such as microbands and shear bands, caused some broadening of the texture and a slight deviation of one skeleton line from the predicted fibre texture component. The decomposition of orientations near {111} < 121 > , and the strengthening of {211} < 011 > after high rolling reductions, was not due to mechanical twinning but could rather be explained by assuming {211} < 111 > slip. 30 ref.--AA
The formation of a third body layer on a conventional friction material during braking tests was studied in some detail using TEM, SEM, and X-ray photoelectron spectroscopy (XPS) techniques. Plate shaped micro-contact areas representing a compositional mix of all components of the tribocouple and exhibiting a nanocry stalline microstructure were identified after a run-in period.
A rather new tool, the focused ion beam (FIB) technique, was used to characterise superficial layers at micro-contact areas of a commercial brake pad. The friction material was a polymer matrix composite (PMC) with approximately 50% metal content (semi-metallic) and the counter part was a cast iron rotor. Though the contact areas were not visible as topographic features, they could be identified with the aid of their increased secondary electron emission during FIB-scanning of the surface after tribological activation. Target preparation of micron-sized cross-sections with the FIB enabled the study of superficial layers at predetermined sites at high magnification.
Depending on the constituent of the pad, one, two or three layers were identified. The three layer structure comprised: (i) a 100 nm thick friction film containing nanocrystalline metal oxides and an amorphous phase which was enriched with sulphur, (ii) a nanocrystalline friction layer of compacted wear debris accommodating surface roughness and (iii) a severely deformed layer if the supporting constituent was a metal particle. Though the majority of loose wear particles was iron oxide, the friction film which adhered tightly to the pad surface contained a large amount of copper and sulphur, whereas zinc was transferred to the cast iron rotor.
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.
Patches of white etching layers on rail surfaces were investigated using sophisticated techniques like cross-sectional transmission electron microscopy (XTEM) and synchroton X-ray diffraction. Optical microscopy failed to resolve the microstructure, but in the TEM submicron grains with high dislocation densities and occasional twins, which are characteristic features of high carbon martensite, were observed. The martensitic structure was confirmed by evaluation of synchroton X-ray diffraction line profiles. The latter technique also allowed to determine dislocation densities of the order of 1012 cm-2 and residual compressive stresses of about 200 MPa.
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.
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.
The unique nanostructure formed during severe as well as moderate braking on the surface of brake discs was investigated by conventional and analytical Transmission Electron Microscopy. In both cases nanocrystalline magnetite mixed with carbon nanoinclusions and minor amounts of other pad constituents were identified. On the basis of these observations the friction performance of a single micro-contact was simulated with the method of Movable Cellular Automata. Inspite of a simplified nanostructure which was examined in two dimensions only, the calculated mean coefficient of friction fitted well to the value usually demanded for automotive braking. Furthermore, the model predicts that oxide films without soft nanoinclusions are not capable of providing smooth velocity accommodation at the pad–disc interface and thus lead to unstable friction behaviour.
Different, partly complementary and partly redundant characterization methods were applied to study the transition of magnetite, graphite and MoS2 powders to mechanically alloyed nanostructures. The applied methods were: Transmission electron microscopy (TEM), Mössbauer spectroscopy (MS), Raman spectroscopy (RS), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The main objective was to prepare a model material providing the essential features of a typical tribofilm forming during automotive braking, and to assess the impact of different constituents on sliding behaviour and friction level. Irrespective of the initial grain size, the raw materials were transferred to a nanocrystalline structure and mixed on a nanoscopic scale during high energy ball milling. Whereas magnetite remained almost unchanged, graphite and molybdenum disulphide were transformed to a nanocrystalline and highly disordered structure. The observed increase of the coefficient of friction was attributed to a loss of lubricity of the latter ingredient due to this transformation and subsequent oxidation.
The sliding behaviors of two simplified tribofilms with amorphous structure consisting either of SiO₂ molecules or C atoms were simulated by molecular dynamics modeling. The objective was to identify mechanisms explaining the experimentally observed lubricating properties of the two amorphous films. The impacts of layer thickness, normal pressure, temperature and different substrate materials were studied systematically, while the sliding velocity was kept constant at 30 m/s. While the layer thickness was not critical, all the other parameters showed special effects under certain conditions. Normal pressure impeded void formation and could even eliminate voids if applied at high temperature. Stick-slip sliding was changed to smooth sliding at high temperature due to void healing. Considering the carbon film, high friction forces and shearing of the entire film was observed with diamond substrates, whereas interface sliding at low friction forces and an amorphous layer of iron mixed with carbon was observed if the supporting substrates consisted of α-Fe. Both films show a decrease of friction forces and smooth sliding behavior at elevated temperature, corresponding well to the tribological behavior of and advanced nanocomposite sliding against a steel disc under severe stressing conditions when high flash temperatures can be expected.
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.
Residual stress depth profiles of a cast nickel-base superalloy were measured by regarding the deflections occurring in plate-shaped specimens while successively removing layers from the machined or treated surface by electropolishing. The results are in good agreement with previous findings showing (i) the influence of grinding parameters on the width of so-called white layers, which correspond to steep gradients of residual tensile stress, and (ii) a broad zone of compressive residual stress in the case of shot peening.
Mechanical and thermal response of a nickel-base superalloy upon grinding with high removal rates
(1997)
Turbine components from conventionally cast nickel-base alloy René 80 show different hot cracking susceptibilities depending on their heat treatment conditions leading to slightly different microstructures. Electron probe micro-analysis, focused ion beam technique and analytical transmission electron microscopy were applied to reveal and identify grain boundary precipitates and the γγ'-microstructure. The distribution of borides along grain boundaries was evaluated statistically by quantitative metallography. The following features could be correlated with an increase of cracking susceptibility: i) Increasing grain size, ii) increasing fraction of grain boundaries with densely spaced borides, iii) lack of secondary γ'-particles in matrix channels between the coarse cuboidal γ'-precipitates. The latter feature seems to be responsible for linking-up of cracked grain boundary precipitates which occurred as an additional cracking mechanism after one heat treatment, whereas decohesion at the boride-matrix-interface in the heat affected zone of laser-drilled holes was observed for both heat treatments.
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.
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.
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.
We applied a combination of Raman spectroscopy (RS) and cross-sectional transmission electron microscopy (X-TEM) to identify silicone oil residues and tribofilms at steel disc surfaces after tribological testing. Neither chemical cleaning nor mechanical removal of a 50 µm thick surface layer produced a surface without any silicone residue. Nevertheless, long-term tribological properties are not affected due to silicone degradation which has been proved by Raman spectroscopy. Excellent anti-wear and anti-friction properties of a nanocomposite at severe stressing conditions correlated with the formation of a silica-based tribofilm containing amorphous and graphite-like carbon nanoparticles. Since reliable carbon quantification by analytical TEM is difficult, RS is a useful complementary method for carbon identification at wear scars.
TEM study on the effect of machining on the microstructure of a soft magnetic Ni76Fe17Cu5CrMo2 alloy
(1991)
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.
Tribofilms formed during dry sliding usually exhibit a nanocrystalline structure and complicated composition. In the present study, tribofilms consisting mainly of a solid lubricant, namely graphite nanoparticles, are considered. Systems providing such tribofilms are candidates for anti-friction applications. Since sliding action always leads to mixing of the materials at both sides of the tribological interface, it was of major interest to study the impact of different amounts of a hard constituent, SiC in the considered case, within the soft matrix systematically. Furthermore, the impact of normal pressure was considered. A mechanically mixed layer was observed for the whole range of normal pressures and SiC volume fractions. The calculated coefficient of friction decreased significantly with increasing thickness of this layer but was only marginally affected by SiC volume fraction, which is good news for anti-friction applications.
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).
Automotive braking is based on dry friction between fixed pads and a rotating disc. Besides macroscopic thermo-physical properties, the development of topographic features on the mesoscopic scale and the nanostructure of the third body formed by wear processes, determine brake performance properties. Whereas modelling on the atomistic scale is suitable to understand mechanisms leading to nanocrystalline surface films, the properties of such films can be assessed best with a model based on movable cellular automata (MCA). It turned out that the presence of at least 10% of soft nanoinclusions is most essential in respect to smooth sliding conditions. It made no major difference whether graphite or copper particles were assumed as soft nanoinclusions. The third body material is not only the stuff which spreads over contact areas, but it also contributes to contact size by wear particle compaction and formation of secondary contact areas. The evolution of contact size is the major feature of mesoscopic modelling and thus it is capable to model and explain dynamic changes of the coefficient of friction (COF) during certain brake operations. Although it is still ambiguous in many cases which feature has the major impact on friction behaviour, the following conclusions can be drawn. The reinforcing ingredients of the pad material serve as primary contact sites and thus define the starting condition for mesoscopic simulations. A certain amount of wear is necessary to provide a third body which is capable to form secondary contact sites and friction layers screening the first body materials. The composition and nanostructure of the third body is important as well, because it determines the friction level and is responsible for smooth sliding conditions.
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.
Does ultra-mild wear play any role for dry friction applications, such as automotive braking?
(2012)
Nanostructured third body films and/or storage of wear debris at the surfaces of the first bodies are deemed as prerequisites of sliding under ultra-mild wear conditions. Since such features have been observed experimentally on brake pads and discs, attempts were undertaken to study their sliding behaviour by modelling on the nanoscopic scale with an approach based on Movable Cellular Automata (MCA). The model rendered the possibility to study the influence of different nanostructures systematically and to assess the impact of different brake pad ingredients on the sliding behaviour, velocity accommodation and friction force stabilization at a sliding contact. Besides providing a review on previously published modelling results, some additional new graphs enabling better visualization of dynamic processes are presented. Although ultra-mild wear conditions were considered to be essential for achieving the desired tribological properties, transitions to mesoscopic and macroscopic wear mechanisms were studied as well. The final conclusion is that ultra-mild wear and corresponding smooth sliding behaviour play an important role during automotive braking, even though temporarily and locally events of severe wear may cause friction instabilities, surface damage and release of coarse wear particles.
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.
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 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.
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.
In order to obtain a better understanding of the role of tribofilms during automotive braking, their structures were investigated and the essential features identified.
Next, different ingredient combinations were studied by preparing some model materials with simpler compositions than real tribofilms. A test method was developed for verifying the tribological properties of the model materials and for comparison with results obtained with numerical sliding simulations of such structures. Prerequisites of good brake Performance properties were identified. Although the coefficient of friction could be varied in a wide ränge, smooth sliding conditions could only be achieved with values smaller than 0.4. Tests with artificial third body powders turned out to be useful as screening method for the selection of raw materials for brake pad formulations.
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
The focused ion beam technique - eine interessante Alternative, auch für konventionelle Werkstoffe
(2002)
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.
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.
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.
The effect of steel counterface topography on the formation mechanisms of nanostructured tribofilms of polyetheretherketone (PEEK) hybrid nanocomposites was studied. Three types of surface finishes with mean roughness Ra ranging from nano- to micro-scale were investigated. Tribo-sintering of nanopartides, oxidation of counterface steel and compaction of wear debris are identified to be competing factors dominating the formation and function of the tribofilms. Counterface topography played an important role on the competing factors, and thereby influenced significantly the final structure, the load-carrying capability and the lubrication performance of the tribofilms. It was disclosed that a thin tribofilm, which mainly consists of silica nanoparticles and which forms on the counterface with a submicron roughness, benefits best the tribological performance of the composites
Formation and function mechanisms of nanostructured tribofilms of epoxy-based hybrid nanocomposites
(2015)
The nanostructures and properties of the tribofilms of epoxy (EP) composites filled with short carbon fibers (SCF) and different volume fractions of monodisperse silica nanoparticles were investigated. When the conventional composite filled only with SCF was considered under a high pv condition, an iron oxide layer is formed on the steel counterface. The addition of even only 0.05 vol% nano-silica leads to a significant change of the tribofilm's structure and the tribological behavior of the composite. With increasing silica content, the oxidation layer on the steel surface is gradually replaced by a silica-based tribofilm. A close relationship between the tribofilms structure and the tribological behavior of the composites was identified. Mixing, possible reactions and tribo-sintering of silica nanoparticles with other wear products are deemed to be main mechanisms inducing the formation and the lubricity of the silica-based tribofilm.
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.
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.
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.
Besides carbon, metal sulphides are used in every standard brake pad formulation as friction stabilisers. In order to investigate their impact, various powder mixtures were tribologically stressed in a pin-on-disc device in order to produce and test artificial third bodies. containing the three main components of a real friction film, namely magnetite, graphite and a metal sulphide of interest. Since the sliding behaviour is influenced by the relative humidity the powder mixtures are tested at low, medium and high moisture levels. The tests revealed that the presence of graphite dominates the friction behaviour as well as the humidity sensitivity.
The powders were prepared by either manual mixing or high energy ball-milling. Interestingly, all ball-milled blends provided coefficients of friction within the desired range for braking, which was attributed to the effect of zirconia particles from wear debris of the milling balls. The zirconia particles prevent the formation of solid lubricant films on the surfaces and support a homogeneous mixture of all constituents of the powder. Optimum brake performance is gained by an optimum combination of solid lubricants and abrasives.
The objective of the present work was to study the impact of Focused Ion Beam (FIB) machining parameters on the thickness of the damaged layer within a thin film PZT. Therefore, different Ga+- ion doses and ion energies were applied to a standard PZT film (80/20 lead zirconium titanate) under two beam incidence angles (90° and 1°). The thicknesses of the corresponding Ga+-implanted layers were then determined by cross-sectional TEM in combination with energy dispersive spectroscopic (EDS) line-scans and correlated with polarisation hysteresis loops. The results show a decrease of Ga+-implanted layer thickness with decreasing inclination angle, whereas ion energy and ion dose could be correlated with gallium concentration in the implanted layers.. Under the most unfavorable conditions the depth of the affected zone was 26 nm, it was only 2 nm for the most favorable conditions.
Determination of the elastic behavior of silicon nanowires within a scanning electron microscope
(2016)
Three-point bending tests were performed on double-anchored, <110> silicon nanowire samples inside a scanning electron microscope (SEM) via a micromanipulator equipped with a piezo-resistive force sensor. Representing the upper and lower boundaries achievable in a consistent manner, silicon nanowires with widths of 35 nm and 74 nm and a height of 168 nm were fabricated. The nanowires were obtained monolithically along with their 10-m-tall supports through a top-down fabrication approach involving a series of etching processes. Hence, no interface compliance was introduced between supports and nanowires. Exact nanowire dimensions and cross-sectional features were determined by transmission electron microscopy (TEM) following sample preparation through focused ion beam (FIB) machining. Conducting the experiments inside an SEM chamber further raised the opportunity of the direct observation of any deviation from ideal loading conditions such as twisting, which was taken into consideration in simulations. Measured force-displacement behavior was observed to exhibit close resemblance to simulation results obtained by finite element modeling, when the bulk value of 169 GPa was taken as the modulus of elasticity for <110> silicon. Hence, test results show neither any size effect nor evidence of residual stresses for the considered nanoscale objects. The increased effect of the native oxide with reduced nanowire dimensions was captured as well. Thus this very simple in-situ testing method was found to be an alternative to elaborate AFM measurements on geometrically formidable nanostructures. The results demonstrate the applicability of the developed fabrication approach to the incorporation of silicon nanowires in functional micromechanical devices.
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.
The tribological behaviour of MoS2/ta-C double layer coatings deposited by Laser-Arc technology was investigated in vacuum and air. In vacuum environment, the friction coefficient against steel balls varies between 0.005 and 0.02 depending on the contact pressure. At high contact pressures, the friction coefficient is as low as 0.005 and the life time between 340,000 and 500,000 cycles. Furthermore, it is shown that a ta-C base layer improves the performance of MoS2 coating.
Surface analyses were performed before and after the tribological tests by means of SEM, EDX, XRD, and TEM. They show that in the top layer beneath the sliding surface crystallization of the initially quasi-amorphous MoS2 took place. TEM images also verified an orientation of the basal MoS2-lattice planes parallel to the surface.
Introducing a single silicon nanowire with a known orientation and dimensions to a specific layout location constitutes a major challenge. The challenge becomes even more formidable, if one chooses to realize the task in a monolithic fashion with an extreme topography, a characteristic of microsystems. The need for such a monolithic integration is fueled by the recent surge in the use of silicon nanowires as functional building blocks in various electromechanical and optoelectronic applications. This challenge is addressed in this work by introducing a top-down, silicon-on-insulator technology. The technology provides a pathway for obtaining well-controlled silicon nanowires along with microstructures up to a three-order-of-magnitude scale difference. A two-step etching process is developed, where the first shallow etch defines a nanoscale protrusion on the wafer surface. After applying a conformal protection on the protrusion, a deep etch step is carried out forming the surrounding microscale features. A minimum nanowire cross-section of 35 nm by 168 nm is demonstrated in the presence of an etch depth of 10 m. All cross-sectional features are characterized via transmission electron microscopy and linked to specific process steps. The technology allows control on all dimensional aspects along with the exact location and orientation of the silicon nanowire.
A new type of test sample for the determination of lateral resolution in surface analysis is presented. The certified reference material BAM-L002 Nanoscale strip pattern for length calibration and testing of lateral resolution is an embedded cross-section of epitaxially grown layers of AlxGa1-xAs and InxGa1-xAs on GaAs substrate. The surface of the sample provides a flat pattern with strip widths of 0.4-500 nm. The combination of gratings, isolated narrow strips and sharp edges of wide strips offers improved possibilities for the calibration of a length scale, the determination of lateral resolution and the optimization of instrument settings. The feasibility of the reference material for an analysis of lateral resolution is demonstrated for SIMS.
The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1–xAs and InxGa1–xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface-analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013.
Results are reported from a pilot study under the Consultative Committee for Amount of Substance (CCQM) to compare measurements of and resolve any relevant measurement issues in, the amount of thermal SiO2 oxide on (100) and (111) orientation Si wafer substrates in the thickness range 1.5 - 8 nm. As a result of the invitation to participate in this activity, 45 sets of measurements have been made in different laboratories using 10 analytical methods: medium-energy ion scattering spectrometry (MEIS), nuclear reaction analysis (NRA), RBS, elastic backscattering spectrometry (EBS), XPS, SIMS, ellipsometry, grazing-incidence x-ray reflectrometry (GIXRR), neutron reflectometry and transmission electron microscopy (TEM). The measurements are made on separate sets of 10 carefully prepared samples, all of which have been characterised by a combination of ellipsometry and XPS using carefully established reference conditions and reference parameters.
The results have been assessed against the National Physical Laboratory (NPL) data and all show excellent linearity. The remaining data sets correlate with the NPL data with average root-mean-square scatters of 0.15 nm, half being better than 0.1 nm and a few at or better than 0.05 nm. Each set of data allows a relative scaling constant and a zero thickness offset to be determined. Each method has an inherent zero thickness offset between 0 nm and 1 nm and it is these offsets, measured here for the first time, that have caused many problems in the past. There are three basic classes of offset: water and carbonadeous contamination equivalent to ~1 nm as seen by ellipsometry; adsorbed oxygen mainly from water at an equivalent thickness of 0.5 nm as seen by MEIS, NRA, RBS and possibly GIXRR; and no offset as seen by XPS using the Si 2p peaks. Each technique has a different uncertainty for the scaling constant and consistent results have been achieved. X-Ray photoelectron spectroscopy has large uncertainties for the scaling constant but a high precision and, critically, if used correctly, has zero offset. Thus, a combination of XPS and the other methods allows the XPS scaling constant to be determined with low uncertainty, traceable via the other methods. XPS laboratories returning results early were invited to test a new reference procedure. All showed very significant improvements. The reference attenuation lengths thus need scaling by 0.986 ± 0.009 (at an expansion factor of 2) deduced from the data for the other methods. Several other methods have small offsets and, to the extent that these can be shown to be constant or measurable, then these methods will also show low uncertainty. Recommendations are provided for parameters for XPS, MEIS, RBS and NRA to improve their accuracy.
Copper, magnetite and graphite particles were mixed in order to observe their impact on the coefficient of friction (CoF) during pin-on-disc tests and on the tribofilm formation after testing. Pure magnetite powder provided a value of CoF of 0.4. Magnetite-copper mixtures tested at 400 °C revealed lower CoF values (~0.4) than those at room temperature (~0.6). Magnetite-graphite and magnetite-graphite-copper mixtures presented lower CoF values (~0.3). All systems formed a magnetite-based tribofilm and patches of metallic copper were found on the tribosurfaces of the mixtures containing copper. Carbon layers and graphite nanoinclusions were observed in the graphite mixtures. The incorporation of zirconia particles, a by-product of ball milling mixing, prevented the selective transfer of graphite and copper to the tribosurfaces of some of the samples.
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.
Transmission electron microscopy study of rapid thermally annealed Pd/Ge contacts on IN0.53Ga0.47As
(1996)
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 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.
Exploring the influence of counterpart materials on tribological behaviors of epoxy composites
(2016)
The dependence of the friction and wear of epoxy (EP) composites materials on counterpart materials, such as standard bearing steel, medium carbon steel and chrome-plating (Cr), was investigated. The conventional composite filled with short carbon fiber (SCF) and graphite shows the highest tribological performance when rubbing against Cr, whereas, the hybrid nanocomposite (EP filled with SCF, graphite and silica nanoparticles) exhibits the lowest friction and wear when sliding against the standard bearing steel. The role of nanoparticles in the tribological performance is distinctly different when sliding against with various counterpart materials. It is demonstrated that counterpart materials exert an important influence on material transfer, tribo-oxidation and mechanical mixing of wear products, resulting in the different formation mechanisms of transfer film.
The influence of the surface roughness of pearlitic grey cast iron discs on the formation of tribofilms and the evolution of the friction coefficient during a ring on disc tribotest with the addition of magnetite and magnetite–graphite nanopowders as interfacial media was investigated. The roughness parameters of the cast iron discs were varied by electro discharge machining (EDM) and grinding processes, producing four distinct surface roughness conditions. The evolution of the friction coefficient, however, did not reach the steady state for most of the samples and the role of the surface roughness on the friction coefficient could not be identified. Focused ion beam (FIB) microscopy on the cast iron discs was carried out to investigate the microstructure of the discs near the tribosurface. These results showed that the EDM process not only varied the surface roughness, but also changed the microstructure of the cast iron discs, promoting the incipient fusion of the cast iron surface, with the formation of ridges and casting defects (pores). As a result, a layer of rapidly solidified metal with a dendritic microstructure was formed near to the surface of the EDMed discs.
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.
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.
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.
The size, surface charge and agglomeration state of nanoparticles under physiological conditions are fundamental parameters to be determined prior to their application in toxicological studies. Although silica-based materials are among the most promising candidates for biomedical applications, more systematic studies concerning the characterisation before performing toxicological studies are necessary. This interest is based on the necessity to elucidate the mechanisms affecting its toxicity. We present here TEM, SAXS and SMPS as a combination of methods allowing an accurate determination of single nanoparticle sizes. For the commercial material, Ludox TM50 single particle sizes around 30 nm were found in solution. DLS measurements of single particles are rather affected by polydispersity and particles concentration but this technique is useful to monitor their agglomeration state. Here, the influence of nanoparticle concentration, ionic strength (IS), pH and bath sonication on the agglomeration behaviour of silica particles in solution has been systematically investigated. Moreover, the colloidal stability of silica particles in the presence of BSA has been investigated showing a correlation between silica and protein concentrations and the formation of agglomerates. Finally, the colloidal stability of silica particles in standard cell culture medium has been tested, concluding the necessity of surface modification in order to preserve silica as primary particles in the presence of serum. The results presented here have major implications on toxicity investigations because silica agglomeration will change the probability and uptake mechanisms and thereby may affect toxicity.
Analytical routines for a comprehensive in-depth morphological, structural, and chemical characterization of functionalized TiO2 films by using different state-of-the-art analytical techniques are presented and discussed with the main objective to identify potential reference TiO2 coating parameters able to be certified at a later stage. TiO2 films fabricated by two different synthetic procedures as representative for two main large-scale applications were selected: (i) pulsed d.c. magnetron sputtering for photocatalytic applications and (ii) screen printing from preformed anatase nanoparticles. The screen-printed films were further loaded with a sensitizing dye for application as a dye-sensitized solar cell. Film properties such as microstructure and crystallographic texture of pulsed d.c. magnetron sputtering synthesized films were systematically studied by means of scanning nanobeam electron diffraction in a transmission electron microscope and the surface and inner morphology by scanning electron microscopy. The dye distribution over the depth of screen-printed TiO2 layers was analyzed before and after dye-loading by means of energy dispersive X-ray spectroscopy at scanning electronmicroscope, Auger electron spectroscopy and time-of-flight secondary ion mass spectrometry. The long-term goal of the present study is the improvement of quality of the TiO2 film parameters as measured by using different types of reference TiO2 coatings having specific parameters certified.
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.
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.
Multi-layer ohmic contact systems such as Au/Pt/Ti/Pt on III-V double layers such as n-InGaP/p+-GaAs are of considerable technological relevance, e.g. for heterojunction bipolar transistors. The paper shows that such contacts can be effectively reacted through the InGaP layer and exhibit very good contact resistances (0.1 O mm) to the base layer if the thickness of the first Pt layer is properly matched to the thickness of the contacted InGaP layer. Interdiffusion and phase formation associated with the annealing processes are studied by cross-sectional analytical transmission electron microscopy, thin-film x-ray diffraction and Auger electron spectroscopy depth profiling. Thermal ageing experiments up to 400 °C show good electrical stability. Device related reliability tests do not show any degradation effect related to this novel base contact.
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.