TEM investigation of MoSeC films

Transition metal dichalcogenides (TMD) are widely used as self-lubricating material either as oil additive or directly as thin films. Magnetron sputtering is a deposition method allowing depositing such films with high density and adhesion. However, their spread use in practical applications is still hindered since their excellent sliding properties are deteriorated in the presence of humidity and under high contact pressures. MoSe2, one of the members of TMD family recently studied, has been co-sputtered with carbon in order to improve the mechanical and tribological properties when compared to pure MoSe2 films

Large-scale fabrication of titanium-rich perovskite PZT submicro/nano wires and their electromechanical properties

We report a 2-step approach to prepare tetragonal perovskite PbZr0.1Ti0.9O3 submicro/nano wires in gram scale and with over 95% wire content. Non-perovskite precursor wires were first fabricated by hydrothermal processing. A subsequent annealing in a PbO atmosphere at 600degC converted these wires into perovskite structures which retain the one-dimensional shape. Binding of the perovksite nanowires to a conductive substrate could be achieved by a similar heat treatment of the non-perovskite precursor wires on a flat Pt coated substrate. Taking advantage of the strong mechanical attachment and good electrical contact between the wires and the metallic layer, piezoresponse force microscopy (PFM) was used to measure the local piezoelectric and ferroelectric properties of the individual wires. Enhanced piezoelectric response relative to sputtered epitaxial PbZr0.2Ti0.8O3 film and squared hysterisis loop with sharp switching indicate pronounced electro- mechanical and ferroelectric behavior. The 90deg domain structure of the as-prepared perovskite PZT wires was confirmed by both PFM and transmission electron microscopy investigations

Control of morphology (ZrN crystallite size and SiNx layer thickness) in Zr-Si-N nanocomposite thin films

DC reactive magnetron sputtering was used for the deposition of Zr–Si–N thin films. Four series of samples have been deposited at various substrate temperatures TS: 300 K, 510 K, 710 K and 910 K. Depending on TS, different N2 partial pressures pN2 were required to obtain nearly stoichiometric ZrN films. Si content (CSi) was varied in each series by changing the power applied on the Si target, whereas the power on the Zr target was kept constant. The microstructure of the coatings was examined by XRD and in cross-section by transmission electron microscopy (TEM). Depending on TS and pN2, the deposition rate showed significant variations from 0.04 to 0.18 nm/s. The correlation between film morphology (preferential orientation of crystallites, grain size, column dimensions, thickness of the SiNx layer covering ZrN crystallites) and the deposition conditions (power applied on Si target, temperature, nitrogen partial pressure and deposition rate) provides useful information for optimizing the deposition process

Precise control of multilayered structures of Nb–O–N thin films by the use of reactive gas pulsing process in DC magnetron sputtering

Multilayered niobium oxynitride films were deposited onto (100) Si using DC magnetron sputtering with a reactive gas pulsing process. The argon and nitrogen flows were kept constant during sputtering of a pure niobium target and the oxygen flow was pulsed during deposition. Pulse durations of T = 10, 40 and 100 s and duty cycles α = tON / T of 0.3, 0.6 and 0.9 were chosen (tON = injection time of high oxygen flow). A mounting triangle was used as the pulse shape for the oxygen injection. During thin film deposition the cathode voltage, Ucath, the O2 and N2 partial pressures, p(O2) and p(N2), were recorded. A delay of both parameters (Ucath, p(O2)) was observed after each pulse, for the return to the values during tOFF = T − tON (off-time of oxygen injection with high flow). High resolution scanning electron microscopy revealed a multilayered structure for coatings deposited with T = 40 and 100 s. Transmission electron microscopy was used to verify that also the coatings with T = 10 s possess a multilayered structure with a period of λ = 10 nm. Despite this low period small crystallites (< 7 nm) were present in these layers. The indentation hardness and the Youngs modulus were in the range of 8.3–16.5 GPa and 154–180 GPa, respectively

A unique approach to reveal the nanocomposite nc-MN/SiN-layer architecture of thin films via electrical measurements

By addition of Si to a binary transition metal nitride MN (e.g. TiN, ZrN, NbN, CrN), the hardness, thermal stability and chemical inertness of films have been considerably improved. The formation of a ternary M–Si–N ternary phase is possible under specific conditions such as low temperature, high deposition rate and low nitrogen pressure. The formation of nanocomposite materials (e.g. crystallites of MN + a thin layer of SiNx) is also possible under a wide range of deposition conditions. In such nanocomposite thin films the crystallite sizes are on the order of a few nanometers. The grain surfaces and boundaries have an important effect on the physical properties. The arrangement and chemical composition of the so-called “amorphous” minority phase (SiNx) are crucial for electrical and mechanical properties. The location, composition and thickness of the amorphous phase must therefore be known precisely. Their experimental determination is challenging due to the small concentration and in particular the geometry of the “amorphous” phase: approximately one monolayer either completely or partially covering the MN nanocrystallites. TEM investigations on such composites are known to have their limitations. It will be shown that the electrical resistivity, measured as a function of temperature, provides an experimental means for following the thickness evolution of the SiNx coverage layer, in such nanocomposite films

Nanoscale triboactivity: The response of Mo–Se–C coatings to sliding

Mo–Se–C films were deposited by sputtering from a carbon target with pellets of MoSe2. In addition to the standard evaluation of their chemical composition, structure, morphology, hardness and cohesion/adhesion, the core objective of this paper was to analyze the tribological behavior of these films, particularly in the high-load regime. The carbon content varied from 29 to 68 at.% which led to a progressive increase of the Se/Mo ratio and the hardness. The friction coefficient of Mo–Se–C coatings clearly decreased with load from 0.15 to 0.05. The excellent friction properties were attributed to the formation of a thin molybdenum diselenide film on the top of the wear track of the coating and on the counterpart surface, while the role of the carbon in the sliding process is only secondary by increasing the coating hardness and thus its wear resistance

Influence of bias voltage on the microstructure and physical properties of magnetron sputtered Zr–Si–N nanocomposite thin films

e report an investigation concerning the influence of ion bombardment on the nanostructure and physical properties of Zr–Si–N nanocomposite thin films. The films were deposited by reactive magnetron sputtering from individual Zr and Si targets. The Si content was varied by changing the power applied to the Si target. The increase of ion bombardment energy was obtained by applying a negative potential Ub = − 150 V to the substrate. The evolution of the film texture, grain size and lattice constant was mapped out using X-ray diffraction measurements. Zr–Si–N films deposited at a substrate temperature Ts = 510 K with a bias voltage of Ub = − 150 V exhibit less pronounced columnar structure with small crystallites having various orientations. The maximum nanohardness of 39 GPa is reached for the films at about 2.5 at.% Si, 8 nm grain size and 0.3 Si surface coverage. The increased energy of ionic species reaching the substrate when a negative bias voltage is applied seems to have the opposite effect to that of increasing substrate temperature: reduced SiNx coverage on the ZrN nanocrystallites

Post-deposition control of ferroelestic stripe domains and internal electric field by thermal treatment

International audienceThe dependence of the formation of ferroelastic stripe domain patternes on the thermal history is investigated be detailed piezoresponse force microscopy and X-ray diffraction expeiments after and during annealing of tensile strained tetragonal Pb(Ti,Zr)O3 epitaxial thin films on DyScO3 substates. In particular, the ferroelastic pattern is reversibly interchanged between a cross-hatched and a stripe domain patterne if the films are cooled at different rates after annealing above the formation temperature of a-domains. Different types of 180° and non-180° patterns can be created, depending on the thermal treatment. The changes in the 180° domain structure and lattice parameters are attributed to a change of oxygen vacancy concentration, which results in a modification of the internal electric fiels and unit cell size, causing also a shift of Tc. Thermal treatment is done on rhombohedral La:BiFeO3 thin films as well. It is observed that also in these films, appropriate heat treatment modifies the domain pattern and films with a stripe domain pattern can be created, confirming the general validity of the developed model

A Simple Synthesis of an N-Doped Carbon ORR Catalyst: Hierarchical Micro/Meso/Macro Porosity and Graphitic Shells

Replacing platinum as an oxygen reduction catalyst is an important scientific and technological challenge. Herein we report a simple synthesis of a complex carbon with very good oxygen reduction reaction (ORR) activity at pH 13. Pyrolysis of magnesium nitrilotriacetate yields a carbon with hierarchical micro/meso/macro porosity, resulting from in situ templating by spontaneously forming MgO nanoparticles and from etching by pyrolysis gases. The mesopores are lined with highly graphitic shells. The high ORR activity is attributed to a good balance between high specific surface area and mass transport through the hierarchical porosity, and to improved electronic conductivity through the graphitic shells. This novel carbon has a high surface area (1320 m2g−1), and high nitrogen content for a single precursor synthesis (∼6 %). Importantly, its synthesis is both cheap and easily scalable