Characteristic features of slip bands in submicron single-crystal gold component produced by fatigue

In order to investigate the fatigue behavior of submicron metal components, a resonant fatigue experiment is conducted using a single-crystal gold specimen that possesses a test section with a submicron width. Crystallographic slip bands appear on the test section surface due to fatigue when the resonant frequency of the specimen decreases abruptly. These slip bands form due to activation of a slip system with the maximum resolved shear stress amplitude. The critical value for slip band formation is evaluated to be over 150 MPa, which is over six times larger than that of persistent slip bands (PSBs) in the bulk counterpart. Cross-sectional field-emission scanning electron microscopy observations reveal that extrusions/intrusions that are ～15 nm wide form on the surface at slip bands. Although the slip bands have similar morphologies to those of PSBs, they are much narrower (bulk width is larger than 1 μm). The high fatigue strength may be attributed to the narrow slips required. Strain localization at the slip bands is revealed by cyclic deformation in the surface-polished specimen after fatigue. This suggests that there may be a certain fatigue understructure at the slip bands.     

Fatigue testing and microstructural characterization of tungsten heavy alloy Densimet 185

A rotating target consisting of helium-cooled tungsten has been chosen for the European Spallation Source (ESS) facility to be built in Lund. Thermo-mechanical cycling due to the incidence of the proton beam every 2 s on any given tungsten slab in the rotating wheel could lead to crack formation and failure over the lifetime of the target. This work reports tensile and fatigue data obtained at room temperature for the Densimet 185 alloy in the non-irradiated condition. Methods for extracting relevant parameters from fatigue curves with small sets of data are discussed. Fatigue results show a large spread of data for which the application of such methods is challenging.Stress controlled fatigue testing was carried out in this study with mean stress approaching zero and amplitudes in the range 250 to 450 MPa, with 50 MPa increments. A frequency of 25Hz was employed and the fatigue tests lasted until failure was registered or until the upper limit of 2 × 10⁶ cycles was reached. No failure due to fatigue occurred in specimens subjected to stress amplitudes below 300 MPa. Microstructural and fractographic studies on the fatigue samples using Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) showed that the samples had low porosity, large and nearly spherical tungsten grains, and with a fairly uniform distribution of the ductile phase rich in nickel and iron. However, bonding between tungsten grains in some areas was found to be inadequate. Intergranular fracture was predominant in the specimens at room temperature. Data for the D185 alloy are compared to those for IT180 and D176 alloys obtained in a previous study and strategies for improving the fatigue strength are discussed.     

The influence of SDS and CTAB surfactants on the surface morphology and surface topography of electroless Ni–P deposits

The effect of surfactants sodium dodecyl sulphate (SDS) and cetyltrimethyl ammonium bromide (CTAB) on the surface roughness, surface morphology and surface topography of electroless nickel (EN)–phosphorus surface protective coating obtained from an alkaline bath is presented in this paper. In this study the influence of surfactant concentrations on the surface roughness of coated samples were investigated. It was observed that the surface roughness, surface morphology and surface topography of Ni–P coating were clearly influenced by the addition of surfactants SDS and CTAB. EN deposits with addition of surfactant SDS and CTAB at a concentration of 0.6 g/l produce a smooth surface and the average roughness (R_a) value is 1.715 μm for SDS and 1.607 μm for CTAB which is less than the R_a value of EN deposit without surfactant addition (1.885 μm). The mean average roughness (R_a) value with addition of surfactant is 1.796 μm.EN deposit with addition of surfactants consists of a significant fraction of particles of nickel. In the presence of SDS, fine nickel particles have dispersed uniformly on the substrate surface resulting in smoother surface finish of the deposited layers. In the presence of CTAB, at lower concentrations (upto 0.6 g/l) coalescence of nickel particles have been deposited on the substrate surface and at the higher concentration (above 0.6 g/l) uniformly improved surface finish of the deposited layer is resulted. The complete experimental details, results obtained and their analysis are presented in this paper.     

Enhanced fatigue resistance in 316L austenitic stainless steel due to low-temperature paraequilibrium carburization

Fully reversed fatigue tests have been performed on wrought 316L stainless steel samples after low-temperature carburization. The resulting 25 μm case depth, with a surface hardness three times that of the core and a surface compressive stress greater than 2 GPa, leads to significantly enhanced fatigue performance. The so-called endurance limit (defined as the stress at which the fatigue life is 10⁷ cycles) increased from about one-third to about one-half the yield stress (from ∼200 to ∼325 MPa). Fractographic investigations reveal that the surface stresses change the preferred site of fatigue crack nucleation from the surface for noncarburized samples to the interior for carburized samples.     

On-chip laboratory suite for testing of free-standing metal film mechanical properties,Part II – Experiments

In this paper, we demonstrate the fabrication of electrostatically loaded, free-standing Al–0.5 wt.%Cu thin-film samples, realizing a near-zero compliance support post. We measure Young’s modulus E = 74 GPa using cantilevers, in good agreement with grain texture measurements. We measure residual stress σ_R ranging from 30 to 60 MPa using fixed–fixed beams and find that processing induces significant plastic straining, which leads to residual stress values significantly less than the as-deposited value. Strength of this alloy is at least 172 MPa if the film is not severely strained, and the material exhibits no room-temperature fatigue up to 1 billion cycles at this stress level. Notched devices that have been subjected to process-induced plastic straining of ∼4% are weaker and fatigue logarithmically with the number of cycles. We compare deformation processes on the samples using ex situ TEM. The mechanism for the high strength value is attributed to the grain size and the thin surface oxide which constrain dislocation glide, while fatigue of the highly strained material is associated with the appearance of persistent slip bands.     

The fatigue behavior of I-phase containing as-cast Mg–Zn–Y–Zr alloy

The fatigue behavior of as-cast Mg–12%Zn–1.2%Y–0.4%Zr alloy has been investigated. The S–N curve showed that the fatigue strength at 10⁷ cycles was 45 MPa. Scanning electron microscopy observations on the surfaces of the failed and unfailed specimens (after up to 1 × 10⁷ cycles) suggested that the slip bands could act as preferential sites for non-propagating fatigue crack initiation, and the I-phase could effectively retard fatigue crack propagation (FCP). The macro fracture morphology clearly indicated that the overall fracture surface was composed of three regions, i.e. a fatigue crack initiation region (Region 1), a steady crack propagation region (Region 2) and a tearing region (Region 3). High-magnification fractographs showed that only porosities can act as the crack initiation sites for all specimens. Moreover, for specimens with fatigue lifetimes lower than 2 × 10⁵ cycles, the cracks mostly initiated at the subsurface or surface of the specimen. However, when the fatigue lifetime was equal to or higher than 2 × 10⁵ cycles, the fatigue crack initiation sites transferred to the interior of the specimen. The maximum stress intensity factors corresponding to the transition sites between Regions 1, 2 and 3 were 2 and 4.2 MPa m^1/2, respectively. When the maximum stress intensity factor K_max was lower than 4.2 MPa m^1/2, in the steady crack propagation region, due to the retarding effect of I-phase/α-Mg matrix interfaces, the fatigue cracks tended to pass the I-phase/α-Mg matrix eutectic pockets directly and propagated through the grain cells, resulting in the formation of many flat facets on the fracture surface. However, when the maximum stress intensity factor was higher than 4.2 MPa m^1/2, in the sudden failure region, the rigid bonding of I-phase/α-Mg matrix interfaces was destroyed and the cracks preferentially propagated along the interfaces, which resulted in the fracture surface being almost completely composed of cracked I-phase/α-Mg matrix eutectic pockets. Based on microstructural observation and the fracture characteristics of the two regions, it is suggested that with an increase in crack tip driving force, the FCP mode changes from transgranular propagation to intergranular propagation.     

Investigation of the low-cycle fatigue mechanism for micron-scale monocrystalline silicon films

This study investigated the cyclic and static fatigue properties of 10 μm thick, deep reactive ion etched, monocrystalline silicon films. Stress–life fatigue curves and fatigue degradation rates vs. stress curves were generated at both 4 and 40 kHz, at 30 °C, 50% relative humidity (RH). A significant frequency effect was observed, with shorter fatigue lives and faster damage accumulation rates at 4 kHz. Static fatigue was also observed with shorter static lifetimes at 80 °C, 90% RH than at 30 °C, 50% RH. Fracture surface evaluation did not reveal any major difference between cyclically and statically fatigued devices. These experimental results confirm that the fatigue of micron-scale silicon is not purely mechanical. The study also proposes a fatigue scenario based on time-dependent subcritical crack growth to account for the low-cycle fatigue regime.     

Titanium-supported Ce-, Zr-containing oxide coatings modified by platinum or nickel and copper oxides and their catalytic activity in CO oxidation

A combination of plasma electrolytic oxidation (PEO) and impregnation techniques followed by annealing in air has been used to obtain composites Pt/nZrO₂ + pTiO₂/Ti, Pt/nZrO₂ + pTiO₂ + zCeO_x/Ti, NiO + CuO/nZrO₂ + pTiO₂/Ti, NiO + CuO/nZrO₂ + pTiO₂ + zCeO_x/Ti with different zirconium and titanium contents and ZrO₂/TiO₂ phase ratio. The composites have been investigated by means of XRD, XPS and SEM/XSA methods. According to the XPS data, the platinum content on the coating surface is ~ 0.4 at.%, whereas the XSA measurements have shown that the nickel and copper contents in coatings attain 16 and 8 at.%, respectively, depending on the initial oxide coatings composition. Nickel and copper oxides form either extended islets or solid layers (“crusts”) on the coating surface. Both the composites promoted with platinum and those with the “crust” built from nickel and copper oxides are active in CO oxidation at the temperatures above 200 °C and 300 °C, respectively.     

Preparation of self-organized porous anodic niobium oxide microcones and their surface wettability

Porous anodic niobium oxide with a pore size of ～10 nm was formed at 10 V in glycerol electrolyte containing 0.6 mol dm^?3 K₂HPO₄ and 0.2 mol dm^?3 K₃PO₄ at 433 K. After prolonged anodizing for 5.4 ks, niobium oxide microcones develop on the surface. X-ray diffraction patterns of the anodized specimens revealed that the initially formed anodic oxide is amorphous, but an amorphous-to-crystalline transition occurs during anodizing. As a consequence of the preferential chemical dissolution of the initially formed amorphous oxide, due to different solubility of the amorphous and crystalline oxides, crystalline oxide microcones appear on the film surface after prolonged anodizing. The surface is superhydrophilic. After coating with fluorinated alkylsilane, the surface becomes superhydrophobic with a contact angle of 158° for water. The surface is also oil repellent, with a contact angle as high as 140° for salad oil.     

Corrosion of a stainless steel and nickel-based alloys in high temperature supercritical carbon dioxide environment

Corrosion of four alloys has been studied in supercritical carbon dioxide at 650 °C and 20 MPa, specifically AL-6XN stainless steel and three nickel-based alloys, PE-16, Haynes 230, and Alloy 625. The tests were performed for exposure durations of up to 3000 h with samples being removed for analyses at 500 h intervals. The corrosion performance of the alloys was evaluated by weight change measurements, and the surface oxide layers were characterized by scanning electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy. Weight gain measurements showed that the Al-6XN stainless steel exhibited the least corrosion resistance while the weight gains were nearly similar for the other alloys. The oxide layer in AL-6XN stainless steel was composed of large equiaxed grained outer layer of Fe₃O₄ (magnetite) and an inner layer of FeCr₂O₄. Oxide spallation was observed in this stainless steel even after 500 h exposure. In all alloys, Cr-rich oxides phases of Cr₂O₃ and Cr_1.4Fe_0.7O₃ were identified as the protective layers. In alloy PE-16 a thin layer of aluminum oxide formed that promoted the corrosion resistance of the alloy. Cr₂O₃ was identified as the main protective oxide layer in nickel base alloys Haynes 230 and 625.     

Pulse current plasma assisted electrolytic cleaning of AISI 4340 steel

An electrolytic plasma process (EPP) for cleaning AISI 4340 steel was performed in a 10% solution of sodium bicarbonate operated at 70 °C. The effects of the pulse frequency (f) and duty cycle (δ) on the surface morphology, microstructure, mechanical and corrosion properties were investigated. Compared to the conventional DC process, the pulsed EPP cleaning resulted in reduced surface roughness and compressive residual stress at the surface. Minimal reduction in hardness and no reduction in toughness due to hydrogen embrittlement (ASTM F519) were found. At the same time, rotating bending beam fatigue tests indicated a noticeable reduction in fatigue life, which could be offset by a shot peening treatment prior to EPP cleaning at 10 kHz and δ = 0.8. Glow discharge optical emission spectroscopy indicated minimal changes in the surface composition and potentiodynamic corrosion studies revealed a slight ennoblement of the surface attributable to an increased rate of cathodic processes. Optimal process parameters were identified for δ = 0.8 and f = 100–10,000 Hz.     

Composition and annealing effects in solution-processable functionalized graphene oxide/P3HT based solar cells

Characterization of a solution-processable functionalized graphene oxide (SPFGraphene oxide) was investigated by FT-IR spectroscopy and the result of elemental analysis showed that the isocyanate treatment results in the functionalization groups in SPFGraphene oxide. Doping SPFGraphene oxide to P3HT based solar cells induces absorbing spectra more strongly and a great quenching of the photoluminescence of the P3HT. With an increase in the SPFGraphene oxide content, the overall performances of the hybrid devices increases first, reaching the peak efficiency for the 10 wt% SPFGraphene oxide content, and then decreases. After annealing at 160 °C for different time durations, the device containing 10 wt% of SPFGraphene oxide for 10 min shows the best performance with a power conversion efficiency of 1.046%, an open-circuit voltage of 0.73 V, a short-circuit current density of 3.98 mA cm^?2 and a fill factor of 0.36 under simulated AM1.5G conditions at 100 mW cm^?2; The similar content one for 20 min shows η value of 1.013%, which is lower than the former one to a small extent for longer annealing duration. The graphene has the potential to act as the next-generation material in the photovoltaic devices and other applications for ease of preparation, low price, large surface area, high conductivity and excellent transparency.     

Structural changes during the reaction of Ni thin films with (1 0 0) silicon substrates

Ultrathin films of nickel deposited onto (1 0 0) Si substrates were found to form kinetically constrained multilayered interface structures characterized by structural and compositional gradients. The presence of a native SiO₂ on the substrate surface in tandem with thickness-dependent intrinsic stress of the metal film limits the solid-state reaction between Ni and Si. A roughly 6.5 nm thick Ni film on top of the native oxide was observed regardless of the initial nominal film thickness of either 5 or 15 nm. The thickness of the silicide layer that formed by Ni diffusion into the Si substrate, however, scales with the nominal film thickness. Cross-sectional in situ annealing experiments in the transmission electron microscope elucidate the kinetics of interface transformation towards thermodynamic equilibrium. Two competing mechanisms are active during thermal annealing: thermally activated diffusion of Ni through the native oxide layer and subsequent transformation of the observed compositional gradient into a thick reaction layer of NiSi₂ with an epitaxial orientation relationship to the Si substrate; and, secondly, metal film dispersion and subsequent formation of faceted Ni islands on top of the native oxide layer.     

Supercapacitive behavior of electrosynthesized marygold-like structured nickel doped iron hydroxide thin film

Herein, we report the electrosynthesized marygold-like structured nickel doped (5 at.%) iron hydroxide thin film from the aqueous solution of 0.1 M iron sulphate using galavanostatic mode of electrodeposition method for supercapacitor application. The compositional analysis of film was studied by AAS. Amorphous structure of nickel doped iron hydroxide film revealed from XRD analysis. The formation of elemental bands of iron hydroxide was confirmed from FTIR study. The SEM images and surface wettability showed marygold-like structure with contact angle 79° with surface of film. The supercapacitive properties of film using cyclic voltammetry and galvanostatic charge–discharge showed the highest specific capacitance 287 F g^?1 in 1 M Na₂SO₃ electrolyte at the scan rate of 10 mV s^?1. The supercapacitive parameters such as, specific energy (S.E.), specific power (S.P.) and coulomb efficiency (η%) are 8.32 Wh kg^?1, 2.5 kW kg^?1 and 92%, respectively.     

Effect of superimposed uniaxial stress on rumpling of platinum-modified nickel aluminide coatings

Thermal cycling of a platinum modified, nickel aluminide (Ni,Pt)Al coated single crystal superalloy, between 1000 and 1150 °C with 10 min holds at each temperature, and subject to a compressive uniaxial stress is reported. There are two major effects of the superimposed compressive stress not observed in the absence of the stress. One is that the rumpling pattern exhibits an asymmetry with an increase of the bond coat surface roughness perpendicular to the applied loading axis. The other is the formation of cracks in the thermally grown oxide aligned parallel to the stress axis.     

Tunable surface metal morphologies and electrical properties of monodispersed polystyrene beads coated with metal multilayers via electroless deposition

Conducting core–shell beads are composed of a polystyrene (PS) core and a metallic shell of nickel/gold, regardless of their method of preparation. This study examined conducting core–shell beads to identify the metal–polymer interface and the electromechanical response under large deformation. Firstly, monodispersed PS beads, 4.4 μm in diameter, were synthesized by dispersion polymerization. After sequential electroless deposition, the nickel content decreased after gold plating because the nickel deposit oxidized and dissolved into solution while the gold in solution was reduced to the metal on the nickel surface. When the beads were prepared using three different methods, the core–shell beads had a raspberry-like morphology, a smooth surface and an onion-like structure. The electromechanical indentation test of a single conducting core–shell bead (route 1, route 2 and route 3) showed an electrical resistance of 5.0 Ω, 5.1 Ω and 5.8 Ω, respectively. Without a sulfonation process, a noisy response of the electrical signals was observed over the entire range of stain due to the delamination of the metal–polymer interface and mechanical buckling of the metallic layer.     

Fatigue crack growth behavior of a Zr58.5Cu15.6Ni12.8Al10.3Nb2.8 bulk metallic glass-forming alloy

Fatigue crack growth behavior was studied for a Zr_58.5Cu_15.6Ni_12.8Al_10.3Nb_2.8 bulk metallic glass in ambient air, demonstrating a fatigue threshold of ΔK_TH = 1.4 MPa√m and a Paris law exponent of 1.7. A nearly stress intensity-independent crack growth regime occurred at 2.5 × 10^?8 m cycle^–1, suggesting an environmental influence of ambient air on the fatigue crack growth, as has been observed for Zr–Ti–Ni–Cu–Be bulk metallic glasses. However, this environmental fatigue effect was shifted to 25× higher growth rates due to the different chemistry.     

Application of a novel microwave plasma treatment for the sintering of nickel oxide coatings for use in dye-sensitized solar cells

In this study the use of microwave plasma sintering of nickel oxide (NiO_x) particles for use as p-type photoelectrode coatings in dye-sensitized solar cells (DSSCs) is investigated. NiO_x was chosen as the photocathode for this application due to its stability, wide band gap and p-type nature. For high light conversion efficiency DSSCs require a mesoporous structure exhibiting a high surface area. This can be achieved by sintering particles of NiO_x onto a conductive substrate. In this study the use of both 2.45 GHz microwave plasma and conventional furnace sintering were compared for the sintering of the NiO_x particles. Coatings 1 to 2.5 μm thick were obtained from the sintered particles (mean particle size of 50 nm) on 3 mm thick fluorine-doped tin oxide (FTO) coated glass substrates. Both the furnace and microwave plasma sintering treatments were carried out at ~ 450 °C over a 5 min period. Dye sensitization was carried out using Erythrosin B and the UV–vis absorption spectra of the NiO_x coatings were compared. A 44% increase in the level of dye adsorption was obtained for the microwave plasma sintered samples as compared to that obtained through furnace treatments. While the photovoltaic performance of the DSSC fabricated using the microwave plasma treated NiO_x coatings exhibited a tenfold increase in the conversion efficiency in comparison to the furnace treated samples. This enhanced performance was associated with the difference in the mesoporous structure of the sintered NiO_x coatings.     

Cyclic deformation of ultrafine-grained aluminum

Cyclic deformation of ultrafine-grained (UFG) Al with different grain sizes has been studied. It was found that UFG Al had shorter fatigue life than its coarse-grained counterparts. For UFG Al, the fatigue life decreases with decreasing grain size. Shear bands (SBs) shorten fatigue life. SBs are always inclined at 45° to the loading axis, and extend across the whole specimen. A SB is a thin sheet of tangled dislocations that have different Burgers vectors; its thickness is much less than the grain size. The strain–stress field inside a SB is very high. SBs produce shear steps, but not surface extrusions/intrusions, on the specimen surface. Thick shear bands (TSBs), about 200–300 μm, were found in the 6.36 μm grain size specimens, which also inclined 45° to the loading axis. TSBs consist of dislocation cells. The formation of TSBs does not reduce the fatigue life.     

The time behaviour of surface applied fluorine inducing the formation of an alumina scale on gamma-TiAl during oxidation at 900 °C in air

Recently the target temperature of components manufactured from gamma-TiAl alloys like turbine blades, turbocharger rotors or automotive valves has been increased to 900 °C. However, there is an insufficient oxidation resistance above 750 °C. One method used to improve the gamma-TiAl oxidation behaviour is the so-called fluorine microalloying effect. After application of fluorine to the TiAl surface by ion implantation or treatment with diluted HF and oxidation at 900 °C in air a dense alumina layer is formed. The aim of this work was firstly to study the short time development of the fluorine concentration during heating up to 400–1000 °C (1 h/air) in steps of 100 °C. Using ion beam analysis the depth profiles of F, Al, Ti and O were obtained simultaneously and non-destructive. A distinct loss of fluorine was found between 400 °C and 500 °C. At temperatures above 800 °C an alumina layer was formed with fluorine maximum located at the metal/oxide interface. Secondly the long time behaviour during oxidation of up to 500 h/900 °C/air was investigated showing a slow fluorine decrease. The alumina layer acts as a diffusion barrier for fluorine, whereas fluorine diffuses into the metal. The diffusion coefficient was calculated. The results fit into the theoretical model assuming a selective transport of gaseous aluminium fluorides at the metal/oxide interface.