Low-temperature synthesis and photoluminescence of ZnO nanostructures by a facile hydrothermal process

We reported a facile route to large-scale ZnO nanostructures by a poly (styrene-alt-maleic acid sodium) (PSMA)-assisted hydrothermal process. Various nanostructures including nanowires, nanobelts and nanorod arrays were fabricated depending on the experimental conditions. The structural studies reveal that all the nanostructures are single crystal with hexagonal phase and preferentially grow along [0 0 0 1]. The organic additive PSMA offers a spatial template for the one-dimensional (1D) growth of ZnO. The photoluminescence (PL) spectra of these nanostructures exhibit coexistence properties of ultraviolet (UV) and green emission. The nanorod arrays and nanobelts exhibit the strongest UV performance and green emission, respectively. We deduce that quantity of surface defects should be responsible for the difference in PL properties of these nanostructures.     

Sintering of tungsten powder with and without tungsten carbide additive by field assisted sintering technology

Tungsten powder (0.6–0.9 μm) was sintered by field assisted sintering technology (FAST) at various processing conditions. The sample sintered with in-situ hydrogen reduction pretreatment and pulsed electric current during heating showed the lowest amount of oxygen. The maximum relative density achieved was 98.5%, which is from the sample sintered at 2000 °C, 85 MPa for 30 min. However, the corresponding sintered grain size was 22.2 μm. To minimize grain growth, nano tungsten carbide powder (0.1–0.2 μm) was used as sintering additive. By mixing 5 and 10 vol.% WC with W powder, densification was enhanced and finer grain size was obtained. Relative density above 99% with grain size around 3 μm was achieved in W–10 vol.% WC sintered at 1700 °C, 85 MPa, for 5 min.     

Abrasive slurry jet micro-machining of holes in brittle and ductile materials

This paper investigated the effects of elasticity and viscosity, induced by a dilute high-molecular-weight polymer solution, on the shape, depth, and diameter of micro-holes drilled in borosilicate glass and in plates of 6061-T6 aluminum alloy, 110 copper, and 316 stainless steel using low-pressure abrasive slurry jet micro-machining (ASJM). Holes were machined using aqueous jets with 1 wt% 10 μm Al₂O₃ particles. The 180 μm sapphire orifice produced a 140 μm diameter jet at pressures of 4 and 7 MPa. When the jet contained 50 wppm of dissolved 8 million molecular weight polyethylene oxide (PEO), the blind holes in glass were approximately 20% narrower and 30% shallower than holes drilled without the polymer, using the same abrasive concentration and pressure. The addition of PEO led to hole cross-sectional profiles that had a sharper edge at the glass surface and were more V-shaped compared with the U-shape of the holes produced without PEO. Hole symmetry in glass was maintained over depths ranging from about 80–900 μm by ensuring that the jets were aligned perpendicularly to within 0.2°. The changes in shape and size were brought about by normal stresses generated by the polymer. Jets containing this dissolved polymer were observed to oscillate laterally and non-periodically, with an amplitude reaching a value of 20 μm. For the first time, symmetric ASJM through-holes were drilled in a 3-mm-thick borosilicate glass plate without chipping around the exit edge.The depth of symmetric blind holes in metals was restricted to approximately 150 μm for jets with and without PEO. At greater depths, the holes became highly asymmetric, eroding in a specific direction to create a sub-surface slot. The asymmetry appeared to be caused by the extreme sensitivity of ductile materials to jet alignment. This sensitivity also caused the holes in metals to be less circular when PEO was included, apparently caused by the random jet oscillations induced by the polymer. Under identical conditions, hole depths increased in the order: borosilicate glass > 6061-T6 aluminum > 110 copper > 316 stainless steel. The edges of the holes in glass could be made sharper by machining through a sacrificial layer of glass or epoxy.     

Sintering behavior and non-linear properties of ZnO varistors processed in microwave electric and magnetic fields at 2.45 GHz

A study of the densification behavior and grain growth mechanisms of ZnO-based varistors composed of 98 mol.% ZnO–2 mol.% (Bi₂O₃, Sb₂O₃, Co₃O₄, MnO₂) has been carried out. The pressed samples were sintered in microwave electric (E) and magnetic (H) fields using a single-mode cavity of 2.45 GHz. The effect of the sintering temperature (900–1200 °C), holding time (5–120 min) and sintering mode (E, H) on the microstructure and electrical properties of the sintered varistor samples were investigated. The grain growth kinetics was studied using the simplified phenomenological equation Gⁿ = kte^(?Q/RT). The grain growth exponent (n) and apparent activation energy (Q) values were estimated for both electric and magnetic heating modes and were found to be n = 3.06–3.27, Q = 206–214 kJ mol^?1, respectively. The lower value of n estimated in the E field was attributed to a volume diffusion mechanism, whereas the higher n value in the H field sintering was correlated mainly to a combined effect of volume and surface diffusion processes. Samples sintered in the H and E fields showed high final densities. Moreover, the ones sintered in the H field presented slightly higher density values and bigger grains for all sintering temperatures than E field heated ones. The optimal sintering conditions were achieved at 1100 °C for a 5 min soaking time for both H and E field processed samples, where respectively densities of 99.2 ± 0.5% theoretical density (TD) and 98.3 ± 0.5% TD along with grain size values of G = 7.2 ± 0.36 μm and G = 6.6 ± 0.33 μm were obtained. Regarding the electrical properties, breakdown voltage values as high as 500–570 V mm^?1 were obtained, together with high non-linear coefficients α = 29–39 and low leakage currents (J_l ≈ 5 × 10^?3 mA cm^?2), respectively, for E and H field sintered varistor samples. Moreover, samples sintered in an H field systematically exhibited higher breakdown voltage values compared to the ones sintered in the E field. This was attributed to an improved coupling between the H field and the present dopants within the ZnO matrix, this latter being mostly semiconductive, thus leading to an enhanced reactivity and improved properties of the electrostatic barrier.     

Experimentation on MR fluid using a 2-axis wheel tool

This paper is focused on magnetorheological (MR) fluid assistive polishing of optical aspheric components. MR fluid is a functional mixture of non-colloidal magnetic particle of micrometer size suspended in a host fluid, with the special property that its viscosity can be varied by the application of a magnetic field. This paper introduces the basic principles of the methodology and presents experiment results on MR fluids using a 2-axis wheel-shaped tool supporting dual magnetic fields. Mathematical models taking into account the pressure and the tool velocity are derived. The experiments serve to evaluate the effects of process parameters on material removal and performance using a K9 glass parabolic lens of 60 mm diameter as work-piece. It is shown that surface roughness can be reduced from an initial value of 3.8–1.2 nm after 10 min of polishing. The form errors can also be improved from an initial 2.27 μm rms and 7.89 μm peak-to-valley to become 0.36 μm rms and 2.01 μm peak-to-valley after 60 min of polishing.     

Laser compression of monocrystalline tantalum

Monocrystalline tantalum with orientations [1 0 0] and [1 1 1] was subjected to laser-driven compression at energies of 350–684 J, generating shock amplitudes varying from 10 to 110 GPa. A stagnating reservoir driven by a laser beam with a spot radius of ～800 μm created a crater of significant depth (～80 to ～200 μm) on the drive side of the Ta sample. The defects generated by the laser pulse were characterized by transmission and scanning electron microscopy, and are composed of dislocations at low pressures, and mechanical twins and a displacive phase transformation at higher pressures. The defect substructure is a function of distance from the energy deposition surface and correlates directly with the pressure. Directly under the bottom of the crater is an isentropic layer, approximately 40 μm thick, which shows few deformation markings. Lattice rotation was observed immediately beneath this layer. Further below this regime, a high density of twins and dislocations was observed. As the shock amplitude decayed to below ～40 GPa, the incidence of twinning decreased dramatically, suggesting a critical threshold pressure. The twinning planes were primarily {1 1 2}, although some {1 2 3} twins were also observed. Body-centered cubic to hexagonal close-packed pressure induced-transformation was observed at high pressures (～68 GPa).The experimentally measured dislocation densities and threshold stress for twinning are compared with predictions using analyses based on the constitutive response, and the similarities and differences are discussed in terms of the mechanisms of defect generation.     

Effects of squeeze casting parameters on the microstructure of LM13 alloy

Effects of applied pressure and melt and die temperatures on the microstructure of squeeze cast LM13 alloy were examined. The results showed that application of pressure during solidification decreased the grain size and SDAS of the primary α phase and modified the eutectic silicon particles. With application of an external pressure of about 100 MPa, the average SDAS and the average aspect ratio of eutectic silicon particles were reduced from 47 μm and 5 to about 34 μm and 1.5, respectively. SDAS of the primary α phase and the average aspect ratio of eutectic silicon particles decreased slightly with a drop in the melt or die temperatures, reaching to 32 μm and 1.25, respectively, for the best conditions.     

An evaluation of the evolution of workpiece surface integrity in hole making operations for a nickel-based superalloy

White layers and extensive material drag introduced during rough machining are regarded as detrimental to surface integrity. As such a sensible method for determining the amount of material to be removed in a roughing process would be to understand the relationship and interaction between roughing (i.e. drilling) and finishing (i.e. plunge milling) operations. Within this work non-standard cutting parameters were employed during the roughing process to generate a white layer and material drag up to a depth of 20 μm. Various plunge milling cutting strategies followed, with radius removal ranging from 25 μm to 250 μm in order to identify the amount of material removal necessary to eliminate the anomalies previously generated from mistreated surface history. The results show that finishing with a depth of cut between 50 μm and 125 μm removes all anomalies from the roughing process, leaving behind a negligible amount of material drag (3–4 μm). X-ray diffraction demonstrates significant tensile residual stresses (1000–2000 MPa) were generated in the axial and hoop direction by abusive hole drilling while subsequent plunge milling operation leaves compressive surface stresses in the region of ?500 MPa in both the axial and hoop directions; in both cases the depth of the surface stresses extended to around 125 μm from the drilled surface. It was also found that a depth of cut of 25 μm was not sufficient to recover the abused surface; this was due to intense material drag accompanied by surface cracking (i.e. 2 μm depth). The research shows that understanding the interaction between successive cutting operations can provide a suitable machining route to fulfil the industrial quality requirements in terms of the machined surface mechanical/metallurgical properties.     

Residual stress and subsurface damage in machined alumina and alumina/silicon carbide nanocomposite ceramics

We have used TEM and Hertzian indentation to study the interrelation between subsurface damage and residual stress introduced by grinding and diamond polishing surfaces of polycrystalline alumina and 5%SiC/alumina nanocomposites. In all cases a layer of high dislocation density was found near the surface. This varied in thickness from about 300 nm for alumina polished with 1 μm diamond grit to greater than 6 μm for a nanocomposite surface wheel-ground with 150 μm diamond grit. For a given finishing process the nanocomposites showed a greater depth of dislocation activity than alumina. In alumina, extensive basal twinning was found beneath the ground surfaces. Hertzian indentation data indicates a residual compressive stress of about 1500 MPa confined to the dislocation-containing region. Mechanisms for the enhanced dislocation activity in the nanocomposites are discussed.     

Microstructure and growth mechanism of tin whiskers on RESn3 compounds

An exclusive method was developed to prepare intact tin whiskers as transmission electron microscope specimens, and with this technique in situ observation of tin whisker growth from RESn₃ (RE = Nd, La, Ce) film specimen was first achieved. Electron irradiation was discovered to have an effect on the growth of a tin whisker through its root. Large quantities of tin whiskers with diameters from 20 nm to 10 μm and lengths ranging from 50 nm to 500 μm were formed at a growth rate of 0.1–1.8 nm s^?1 on the surface of RESn₃ compounds. Most (>85%) of these tin whiskers have preferred growth directions of 〈1 0 0〉, 〈0 0 1〉, 〈1 0 1〉 and 〈1 0 3〉, as determined by statistics. This kind of tin whisker is single-crystal β-Sn even if it has growth striations, steps and kinks, and no dislocations or twin or grain boundaries were observed within the whisker body. RESn₃ compounds undergo selective oxidation during whisker growth, and the oxidation provides continuous tin atoms for tin whisker growth until they are exhausted. The driving force for whisker growth is the compressive stress resulting from the restriction of the massive volume expansion (38–43%) during the oxidation by the surface RE(OH)₃ layer. Tin atoms diffuse and flow to feed the continuous growth of tin whiskers under a compressive stress gradient formed from the extrusion of tin atoms/clusters at weak points on the surface RE(OH)₃ layers. A growth model was proposed to discuss the characteristics and growth mechanism of tin whiskers from RESn₃ compounds.     

Finite size effect on the piezoelectric properties of ZnO nanobelts: A molecular dynamics approach

The size scale effect on the piezoelectric response of bulk ZnO and ZnO nanobelts has been studied using molecular dynamics simulation. Six molecular dynamics models of ZnO nanobelts are constructed and simulated with lengths of 150.97 Å and lateral dimensions ranging between 8.13 and 37.37 Å. A molecular dynamics model of bulk ZnO has also been constructed and simulated using periodic boundary conditions. The piezoelectric constants of the bulk ZnO and each of the ZnO nanobelts are predicted. The predicted piezoelectric coefficient of bulk ZnO is 1.4 C m^?2, while the piezoelectric coefficient of ZnO nanobelts increases from 1.639 to 2.322 C m^?2 when the lateral dimension of the ZnO NBs is reduced from 37.37 to 8.13 Å. The changes in the piezoelectric constants are explained in the context of surface charge redistribution. The results give a key insight into the field of nanopiezotronics and energy scavenging because the piezoelectric response and voltage output scale with the piezoelectric coefficient.     

Amorphous magnetoelastic sensors for the detection of biological agents

Freestanding amorphous magnetoelastic (ME) biosensors were fabricated by two ways. One type with larger size, 2000 × 400 × 15 μm, 1000 × 200 × 15 μm and 500 × 100 × 15 μm, was made from an ME Fe40Ni38Mo4B18 ribbon, the other with smaller size 200 × 40 × 4 μm was manufactured by dual beam sputtering and non-traditional microelectronic fabrication techniques. Both platforms were immobilized with JRB7 phage and were developed for the real-time in vitro detection of Bacillus anthracis spores. The experimental results show that the measured sensitivity of the ME sensors agrees with theoretical predictions and the specificity of ME sensors coated with JRB7 phage for B. anthracis spore species is excellent. The 200 × 40 × 4 μm biosensor was found to have a detection limit of 10² cfu/ml and sensitivity of 13.1 kHz/decade.     

The role of beam dispersion in Raman and photo-stimulated luminescence piezo-spectroscopy of yttria-stabilized zirconia in multi-layered coatings

Laser beam dispersion affects the resolution of Raman and photo-stimulated luminescence piezo-spectroscopy measurements of transparent materials. In this paper, we investigate the lateral spreading of the laser beam and the axial sampling depth of Raman spectroscopy measurements within thermal sprayed yttria-stabilized zirconia (YSZ) thin coatings. The lateral diameters of the laser beams (λ = 632.8 nm and 514 nm) reach approximately ～160 μm after travelling through a thickness of 200 μm of air plasma sprayed (APS) YSZ and ～80 μm after travelling through 120 μm of electron beam physical vapour deposited YSZ. The Raman spectroscopy sampling depth was found to be between 30 and 40 μm in APS YSZ. The beam dispersions within these two coatings were simulated using the ray-tracing software ZEMAX to understand the observed scattering patterns. The results are discussed with respect to the application of these two spectroscopic techniques in multi-layered thermal barrier coating systems.     

Plastic deformation mechanism of crystalline polymer materials in the equal channel angular extrusion process

The plastic deformation mechanism of polymer materials was observed during the equal channel angular extrusion process with polypropylene as crystal polymer. The variations of the crystalline morphology, microstructure, and microhardness were discussed during the process. The extent of plastic deformation increased from the top surface to the bottom surface, and the maximum molecular orientation increased from R = 1 near the top surface to R = 2.2 near the bottom surface. The plastic deformation at the surface was small, especially in the range of 400 μm distance from the top surface, without definite change of the crystalline structure. The plastic deformation was obvious when the sample was pressed into the outer corner of die. The spherulitic structure extended to the ellipsoidal shape along the 45° direction of the diagonal line because of the shear strain. The plastic deformation led to the destruction of spherulites near the bottom surface. However, the spherulites were not destroyed at center part, so their refinement as metallic material could not be expected. The variation of internal structure and material orientation increased along the direction of the maximum molecular orientation.     

Effect of hot rolled grain size on the precipitation kinetics of nitrides in low carbon Al-killed steel

The precipitation of nitrides plays a general role in the industrial processing of deep drawing quality Al-killed low carbon steels. In this paper, the effect of hot rolled grain size on the precipitation of nitrides has been analysed. To evaluate the effect of grain size on the nitride precipitation kinetics, thermoelectric power based investigations have been performed on hot and cold rolled specimens.In the hot rolled state, the precipitation of nitrides occurs more intensively in the fine grain size microstructure (average grain size = 9 μm) than in the large grain size microstructure (average grain size = 23 μm) until the precipitated fraction of nitrides reaches about 70%. In the cold rolled state the effect of grain size is much less significant; probably the precipitation process occurs simultaneously at the grain boundaries and along dislocations. According to the simulation results, significant differences can be found between the precipitated fraction of nitrides in fine and large grain size sheets coiled in the temperature range 550–650 °C. In this interval, the precipitated nitride fraction is about two times larger in a fine grain microstructure (9 μm) than in sheets with 23 μm average grain size. The local position in the coil also affects significantly the precipitated fraction of nitrides. In the outer ring of the coil, less than 20% precipitated fraction is predicted in coiling temperature range 550–700 °C. However, in the middle ring of a hot rolled coil, the precipitated fraction changes from 5% to 85% with increasing coiling temperature from 550 to 700 °C.     

An innovative method to perform maskless plain waterjet milling for pocket generation: a case study in Ti-based superalloys

This paper presents an innovative methodology/jet path on which plain waterjet (PWJ) can generate pockets of good dimensional/geometrical definition (minimised under/over-erosion) while the proposed method leads to the avoidance of grit embedment on the target workpiece and the elimination of extra cost and time related to the use of mask.The novelty of the paper relies on the proposal of jet-path strategy that minimises the variations in jet dwell time by providing “continuous” relative movement during the jet-part interaction (through minimisation of accelerations/decelerations of the machine head) and by removing a controlled amount of material in a series of layers using special techniques. The proposed method is powerful in its approach from which it ensures (quasi)equal exposure time for each zone of material over which the jet passes, so that the jet path is “totally contained” within the form to be generated; hence, no masking is necessary to define the contour/shape.This approach has been employed for generating pockets on two Ti-based superalloys commonly used in aerospace industries, followed by dimensional, geometrical and surface quality analysis. The results proved that this approach can produce milled surfaces of straightness of the pocket bottom (<200 μm), tolerance on depth of cut per layer (<20 μm), tolerance on the radii at the bottom of the pockets (<100 μm), surface roughness (Ra=4–14 μm) and waviness (Wa=10–13 μm) characteristics in conditions of high surface integrity (no cracks, contaminations, etc.).     

Effect of initial particulate and sintering temperature on mechanical properties and microstructure of WC–ZrO2–VC ceramic composites

Owing to improving the mechanical properties of cemented carbides in high speed machining fields, a new composite tool material WC–ZrO₂–VC (WZV) is prepared from a mixture of yttria stabilized zirconia (YSZ) and micrometer VC particles by hot-press-sintering in nitrogenous atmosphere. Commercial WC, of which the initial particle sizes are 0.2 μm, 0.4 μm, 0.6 μm and 0.8 μm, is mixed with zirconia and VC powder in aqueous medium by following a ball mill process. The sintering behavior is investigated by isostatic pressing under different sintering temperature. The relative density and bending strength are measured by Archimedes methods and three-point bending mode, respectively. Hardness and fracture toughness are performed by Vickers indentation method. Microstructure of the composite is characterized by scanning electron microscopy (SEM). The correlations between initial particles, densification mechanism, sintering temperature, microstructure and mechanical properties are studied. Experimental results show that maximum densification 99.5% is achieved at 1650 °C and the initial particle size is 0.8 μm. When temperature is 1550 °C and particle size is 0.4 μm, the optimized bending strength (943 MPa) is obtained. The best hardness record is 19.2 GPa when sintering temperature is 1650 and particle size is 0.8 μm. The indention cracks propagate around the grain boundaries and the WC particles fracture, which is associated with particle and microcrack toughening mechanism.     

Attenuation of ultrasound in severely plastically deformed nickel

Ultrasound attenuation was measured in nickel specimens of about 30 mm diameter prepared using the high pressure torsion technique. The cold working process produced an equivalent shear strain increasing from zero at the center up to 1000% at the edge of the specimen. The fragmentation of the grains due to multiple dislocations led to an ultrafine microstructure with large angle grain boundaries. The mean value of the grain size distribution gradually decreased from ～50 μm at the center to 0.2 μm at the edge. Laser pulses of 5 ns were employed for the excitation of broadband ultrasound pulses covering the spectral range of 0.1–150 MHz. The ultrasound pulses were measured from the opposite side of the specimen by means of an optical interferometer and a piezoelectric foil transducer in two experimental setups. The features of the detected signal forms are discussed. The absolute value of the attenuation decreases from the center to the edge of the specimen showing nearly linear frequency dependence. The variation of the phase velocity was measured in a 6 mm-thick high pressure torsion nickel sample, revealing a velocity increase from the center to the edge.     

Mechanical and structural properties of multilayer c-BN coatings on cemented carbide cutting tools

Multilayer cubic boron nitride (c-BN) coatings represent a new deposition method that can improve adhesion on metal substrates. The multilayer c-BN system in this study consisted of a TiAlN interlayer (2– 3.5 μm), boron carbide (~ 1 μm), and a c-BN (~ 2 μm) gradient layer. This multilayer c-BN structure, exceeding 5 μm in thickness, showed outstanding adhesion in atmospheric conditions even with high residual stress. Compared to monolayer c-BN coatings, the multilayer c-BN films had lower elastic moduli, and their critical loads were twice as high. The adhesion of the multilayer c-BN system was significantly improved because of the induced stress relaxation.     

Effect of oxide scale on temperature-dependent interfacial heat transfer in hot stamping process

An optimization-based numerical procedure was developed to determine the temperature-dependent interfacial heat transfer coefficient (IHTC). The effects of temperature, pressure and oxide scale thickness were analyzed, for oxide thickness between 9 μm and 156 μm and pressure from 8 MPa to 42 MPa. Oxide scales and contact pressure both show distinctive effects on IHTC in the cooling process. The average IHTC decreases about 2461 W/(m² °C) with the increase of oxide scale thickness and increases 2620 W/(m² °C) with the increase of pressure. Based on the two-way ANOVA, the effect of contact pressure influences the IHTC most. Their mutual interaction is negligible. The IHTC decreases when the average temperature between the blank and die surface is above 250 °C and increases when the latent heat release.