The effect of magnesium additions on the microstructure and cut edge corrosion resistance of zinc aluminium alloy galvanised steel

The magnesium levels in 20 μm thick 4.5% Al/Zn galvanising coatings applied to 0.7 mm gauge steel under continuous galvanising conditions were altered from 0.0% to 0.05%. The additions result in an increase in the zinc dendrites (volume fraction from 6% to 22% and number from 150 to 325 mm⁻²) since magnesium depresses the eutectic temperature increasing the freezing range. The microstructural modification results in increasing cut edge corrosion determined using a scanning vibrating electrode technique for 24 h exposure to 5% NaCl. The Mg additions result in an increase in zinc loss (from 80 to 185 μg), an increase in active anode numbers (from 600 to 1700 m⁻¹ cut edge) and an increase in the number of long lived anodes.     

Production of rapidly solidified Cu-Sn ribbons by water jet cooled rotating disc method

In order to obtain rapidly solidified ribbons, it is important to control and understand the mechanism of ribbon formation. In this study, rapidly solidified Cu-Sn ribbons were produced by water jet cooled rotating disc method. The produced ribbons had typically 15-95 μm thickness, 3-6 mm width and 45-72 mm length depending on process parameters. Increasing the disc speed from 50 to 75 m s⁻¹ resulted in a decrease of ribbon thickness from 75 to 34 μm. From the disc-side to the air-side surface of the ribbons, the microstructure of the ribbons consisted of three distinct zones: fine grained microstructure (chill region), columnar zone and cellular/equiaxed region. The columnar zone/ribbon thickness ratio decreased with increasing ribbon thickness. The estimated cooling rates of 20 and 90 μm thick ribbons were 1.98 × 10⁶ and 5.49 × 10³ K s⁻¹, respectively.     

Investigation into the effects of metallic coating thickness on the corrosion properties of Zn-Al alloy galvanising coatings

Galvalloy (4.5% Al 95.5% Zn) coatings were produced on a continuous coil coating line at Corus Colors’ Shotton works with varying metallic coating thickness from 7.8 μm (120 g m⁻²) to 48 μm (325 g m⁻²) controlled using air knives. An overall decrease in aluminium content from 5.1% to 4.5 wt% and a primary zinc volume fraction increase from 16.2% to 32.8% occurred as the coating thickness is decreased. This reflects greater nucleation in thinner coatings and some removal of Al enriched molten phases. The scanning vibrating electrode technique (SVET) was used to show that increasing the coating thickness from 7.8 to 48 μm resulted in a decrease in the level of zinc removed during corrosion from a 20 mm exposed cut edge from 530 to 220 μg in the 24 h exposure to 5% NaCl solution. The same trend was also observed when external zinc runoff measurements were made at the Port Talbot weathering site. The increasing corrosion observed at lower coating weights results from greater undercutting of these coatings that are further away from a eutectic composition and an increasing tendency for crevice driven corrosion brought about through primary zinc dendrite interconnectivity.     

Small scale resistance spot welding of Cu47Ti34Zr11Ni8 (Vitreloy 101) bulk metallic glass

The resistance spot welding of Vitreloy 101 (Cu₄₇Ti₃₄Zr₁₁Ni₈) metallic glass ribbons was studied by mechanical testing, scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Material was expelled along the weld interface and around the electrode contact points on the alloy surface. There were no significant changes in composition between the melted and native alloy although minor (∼8%) crystallization was observed in DSC data. Failure during peel and tensile-shear tests of the welds was observed to occur at the periphery of the weld (pullout failure), where slower melting and cooling occurred away from the heat sink effects of the welding electrodes. Measurements of lap welds indicated a maximum shear strength of 810 ± 77 MPa, about 75% of the predicted shear strength of the monolithic alloy. Embrittlement and crystallization around the weld likely contributed to failure. A finite element analysis (FEA) model was developed to explore the temperature–time relation inside the metallic glass during and following welding and it confirmed the main features observed experimentally. The model indicated rapid melting as temperatures reached ∼2000 K followed by cooling of the center of the weld nugget at rates up to ∼48,000 K s⁻¹, greatly exceeding the critical cooling rate for this material of 250 K s⁻¹. A torus of material around the weld nugget remained molten for longer and cooled more slowly than the center of the weld nugget.     

Preparation and characterization of graphene nanosheets/poly(3-hexylthiophene) thermoelectric composite materials

Graphene nanosheets/poly(3-hexylthiophene) (GNs/P3HT) composites were prepared by oxidative polymerization of 3-hexylthiophene in a GNs dispersed chloroform solution. The phase composition of the composite materials was analyzed by X-ray diffraction and Fourier transform infrared spectra. The thermoelectric properties of the cold pressed composite pellets with different GNs loadings were measured at room temperature. As the GNs loading increased from 0 to 30 wt.%, the electrical conductivity of the composites dramatically increased from ∼10⁻⁶ to ∼1.2 S/cm while the Seebeck coefficient slightly increased from 33.15 to 35.46 μV/K. The highest power factor (∼0.16 μW m⁻¹ K⁻²) was obtained in the 30 wt.% GNs/P3HT composite material.     

Structure and properties of nanostructured A357 alloy produced by melt spinning compared with direct chill ingot

The properties of nanostructured A357 ribbons produced by melt spinning were investigated using field emission gun scanning electron microscope, X-ray diffraction pattern, differential scanning calorimetry and microhardness testing in comparison with those fabricated by direct-chill (DC) casting. The solidification time and cooling rate of 46 μm thick melt-spun ribbon were estimated to be 9.13 × 10⁻⁶ s and 1.17 × 10⁷ K s⁻¹, respectively. The results show that the nanostructure of A357 ribbons exhibits the enhanced solid-solubility of Si in Al matrix to 2.00 wt.% and the existence of ultra-fine and homogenous dendritic structure having a dendrite arm spacing of about 200 nm. The nano-sized spherical eutectic Si crystals having a size of 50 nm were also observed. All these structural factors increase the microhardness of the ribbon which is twice as high as that of DC casting.     

Growth of ZnO nanorods by air annealing of ZnO films with an applied electric field

A novel method of ZnO nanorods growth is presented based on low temperature (300 °C) air annealing of ZnO film while applying an electric field (∼ 10 V/cm) parallel to the film. The films were deposited on glass substrates using a filtered vacuum arc deposition system equipped with a Zn cathode, at an arc current of 160 A, oxygen pressure of 3.2 mTorr, and deposition time of 30 s. Cu tape electrodes were applied on each end of the coated sample, and used to apply the electric field. The samples were annealed in a quartz furnace at 200, 300, 400 °C for 20 or 60 min. Each sample surface was examined using a Scanning Electron Microscope (SEM) and a High Resolution SEM (HRSEM) to study its micro- and nano-structure. The film crystallographic structure was studied using X-ray diffractometry (XRD). ZnO rods with lengths of ∼ 3 μm were observed on the samples annealed at 300 °C for 20 min with an electric field of ∼ 10³ V/m, while separated conical forms with lengths of ∼ 0.5 μm and base width of ∼ 150 nm were observed after annealing under the same conditions but without any electric field. The rod growth rate and area density were ∼ 2.0-2.5 nm/s, and ∼ 3 × 10⁷ cm^− 2, respectively.     

High rate deposition of thick CrN and Cr2N coatings using modulated pulse power (MPP) magnetron sputtering

As a variation of high power pulsed magnetron sputtering technique, modulated pulse power (MPP) magnetron sputtering can achieve a high deposition rate while at the same time achieving a high degree of ionization of the sputtered material with low ion energies. These advantages of the MPP technique can be utilized to obtain dense coatings with a small incorporation of the residual stress and defect density for the thick coating growth. In this study, the MPP technique has been utilized to reactively deposit thick Cr₂N and CrN coatings (up to 55 μm) on AISI 440C steel and cemented carbide substrates in a closed field unbalanced magnetron sputtering system. High deposition rates of 15 and 10 μm per hour have been measured for the Cr₂N and CrN coating depositions, respectively, using a 3 kW average target power (16.7 W/cm² average target power density), a 50 mm substrate to target distance and an Ar/N₂ gas flow ratio of 3:1 and 1:1. The CrN coatings showed a denser microstructure than the Cr₂N coatings, whereas the Cr₂N coatings exhibited a smaller grain size and surface roughness than those of the CrN coatings for the same coating thickness. The compressive residual stresses in the CrN and Cr₂N coatings increased as the coating thickness increased to 30 μm and 20 μm, respectively, but for thicker coatings, the stress gradually decreased as the coating thickness increased. The CrN coatings exhibited an increase in the scratch test critical load as the thickness was increased. Both CrN and Cr₂N coatings showed a decrease in the hardness and an increase in the sliding coefficient of friction as the coating thickness increased from 2.5 to 55 μm. However, the wear rate of the CrN coatings decreased significantly as the coating thickness was increased to 10 μm or higher. The 10-55 μm CrN coating exhibited low wear rates in the range of 3.5-5 × 10⁻⁷ mm³ N⁻¹ m⁻¹. To the contrary, the Cr₂N coating exhibited relatively low wear resistance in that high wear rates in the range of 3.5 to 7.5 × 10⁻⁶ mm³ N⁻¹ m⁻¹ were observed for different thicknesses.     

Grain refinement and mechanical properties of asymmetrically rolled low carbon steel

The formation of fine ferrite grains by the asymmetric rolling of low carbon steel and their mechanical properties were studied. Super-cooled low carbon austenite was deformed by asymmetric rolling at 750 °C with a roll size ratio of 1.5 and immediately cooled at various cooling rates ranging from 3 °C/s to 15 °C/s. Fine ferrite grains (∼2 μm) were formed after asymmetric rolling, preferentially at the prior austenite grain boundaries. The volume fraction of the fine ferrite grains increased with increasing rolling reduction. A ferrite plus pearlite microstructure was obtained at smaller strains and slower cooling rates. However, after heavy deformation, a fine ferrite grain structure with carbide particles dispersed at the ferrite grain boundaries was obtained and the pearlite structure was not observed even after very slow cooling, which implies that most of the ferrite grains were formed dynamically, i.e. during deformation. The yield strength of the asymmetrically rolled steel plates increased with increasing deformation; however, the yield ratio also increased with increasing rolling reduction. The best combination of strength and yield ratio was obtained by using a low level of deformation and a high cooling rate, in which case a portion of the untransformed austenite transformed to martensite.     

Thin films of thermoelectric compound Mg2Sn deposited by co-sputtering assisted by multi-dipolar microwave plasma

Magnesium stannide (Mg₂Sn) thin films doped with Ag intended for thermoelectric applications are deposited on both silicon and glass substrates at room temperature by plasma assisted co-sputtering. Characterization by scanning electron microscopy, energy-dispersive X-ray spectroscopy and X-ray diffraction confirms the formation of fine-grained polycrystalline thin films with thickness of 1-3 μm. Stoichiometry, microstructure and crystal structure of thin films are found to vary with target biasing and the distance from targets to substrate. Measurements of electrical resistivity and Seebeck coefficient at room temperature show the maximum power factor of ∼5.0 × 10⁻³ W K⁻² m⁻¹ for stoichiometric Mg₂Sn thin films doped with ∼1 at.% Ag.     

Synthesis of diamond-like carbon coatings on aluminum 6061 T-91 substrates by laser sintering of ultra-nanocrystalline diamond powders

Diamond-like carbon (DLC) coatings have been prepared on aluminum 6061 T-91 substrates with the aid of electrostatic spray deposition (ESD) of ultra-nanocrystalline diamond powders (2-8 nm) followed by direct laser sintering technique. A continuous-wave CO₂ laser was utilized, producing a dense, adherent DLC coating with a nominal thickness of 10 μm under optimal laser parameters that included laser power of 200 W, spot size of 1 mm by 0.1 mm and scanning speed of 254 mm/s. The evidence of DLC formation and its purity was obtained by characterizing the samples with Raman spectroscopy, X-ray diffraction and scanning electron microscopy/energy dispersive spectroscopy. Functional evaluation of DLC coatings was performed using scratch, micro-hardness, fracture toughness and surface roughness tests. Raman measurements showed the presence of a broader peak at around 1332 cm^− 1 (characteristic of pure diamond) for electrostatically deposited samples and the presence of DLC with a broad asymmetric hump in the region of 1000 to 1600 cm^− 1 for laser-sintered samples. X-ray diffraction and energy dispersive spectroscopy confirmed the presence of carbon phases in the coatings. Scanning electron microscopy examination showed a fairly uniform and dense coating with a nominal thickness of 10 μm and a heat affected zone of 60-80 μm. These coatings exhibited micro-hardness in the range of 2150 to 2350 kg/mm² when measured using a Vickers diamond pyramid indenter at a load of 0.5 N. In some localized regions, hardness of 9000 kg/mm² was obtained. Scratch tests revealed a fairly homogenous coating with strong adhesive nature having almost four times the average critical force when compared against the electrostatically deposited sample. Fracture toughness and surface roughness are well within the acceptable ranges of DLC coatings. The capability of laser sintering to produce thick DLC coatings with outstanding mechanical and tribological properties and excellent bonding with aluminum offers the possibility to tailor an extreme lightweight, strong and wear-resistant material.     

Deformation induced thermoremanent magnetisation in an FeMnNiCr antiferromagnetic alloy

In an austenitic Fe_61.5Mn₂₃Ni₇Cr_8.5 antiferromagnetic (afm) alloy deformation results in a splitting between magnetisation-vs.-temperature curves measured during field cooling (FC) below the Néel temperature and those measured at the same field after zero-field cooling (ZFC). Furthermore, a thermoremanent magnetisation (TRM) appears that corresponds to the splitting between zero-field and field cooled thermomagnetic measurements for a given cooling field and scales with the degree of deformation. This TRM is attributed to the deformation induced defects which act as a source of uncompensated magnetic moments and interact with the bulk afm moments. This interpretation is also supported by the fact that the net magnetic moments vanish above the Néel temperature. The TRM does not saturate in fields of up to 7 T, applied during cooling, and cannot be switched by fields up to 7 T. Within the investigated field range of −7 T to 7 T the magnetisation-vs.-field curves show a stable shift along the magnetisation axis. Thus, the uncompensated moments appear to be strongly exchange coupled to the afm matrix surrounding them. Within the series of experiments the maximum TRM reached after FC in 7 T corresponds to about 4 × 10⁻⁴μ_B/atom (Bohr magneton) of the maximum deformed afm sample. The Néel temperature decreases due to deformation.     

Microstructure and wear studies of laser clad Al-Si/SiC(p) composite coatings

Coatings of a composite material consisting of an Al-Si matrix reinforced with SiC particles were produced by laser cladding on UNS A03560 cast Al-alloy substrates from mixtures of powders of Al-12 wt.% Si alloy and SiC. The influence of the processing parameters on the microstructure and abrasive wear resistance of the coatings was studied. For an interaction time of 0.08 s and a power density of 330 MW/m², corresponding to a specific energy of 26 MJ/m², the interaction between SiC and liquid Al is limited and the reinforcement particles remain essentially undissolved. The coating's microstructure is formed of SiC particles dispersed in a matrix consisting of primary α-Al dendrites and interdendritic α-Al + Si eutectic. For interaction times of 0.3 and 0.45 s and a power density of 193 MW/m², corresponding to specific energies of 58 and 87 MJ/m², SiC reacts with molten Al and partially dissolves. The resulting microstructure consists of undissolved SiC particles, found mainly at the bottom of the clad tracks, where the maximum temperature reached during processing is lower, and Al₄SiC₄ and Si particles dispersed in a matrix of α-Al + Si eutectic. The coatings prepared with higher specific energy (58 MJ/m²) present a hardness of 250 V and an abrasive wear rate in three-body abrasion tests with SiC as abrasive of 1.7 × 10^− 4 mm³/m, while those produced with 26 MJ/m² present a hardness of 120 V and a wear rate of 0.43 × 10^− 4 mm³/m. These results show that Al₄SiC₄ and Si increase the hardness of the material by dispersion hardening but do not contribute to its abrasive wear resistance, because they are softer than the abrasive particles, and confirm that the parameters used to prepare Al-Si-SiC composite coatings by laser cladding must be selected so that only minimal reactions occur between SiC and molten Al.     

Microstructure and properties of Ni-Mn-Ga alloys produced by rapid solidification and pulsed electric current sintering

Ni-Mn-Ga alloys were compacted using pulsed electric current sintering (PECS) at 850-875 °C (50 MPa, 8 min) of flake-like powders made from the rapidly quenched melt-spun ribbons. Two kinds of ribbons were used: one made with a relatively slow wheel speed (6 m/s; average grain size ∼14 μm), and another with a faster wheel speed (23 m/s; average grain size ∼5 μm). Both sets of flake-like powders consisted of a mixture of non-modulated martensite (NM) and seven-layered modulated martensite (7M) structure. The amount of NM was greater in the slower speed material, while the other one exhibited mostly the 7M structure. These crystal structures were inherited by the sintered samples. In the compacts having the NM structure the multi-step martensitic reaction overlapped with the magnetic transition, and the Curie temperatures during heating and cooling differed from each other. In the compacts having mainly 7M structure the Curie point was about 100 °C and the martensitic transition took place in the paramagnetic state, while the intermartensitic one occurred in the region of 60-85 °C. This material demonstrated good magnetic properties and saturation magnetization, at best ∼50 emu/g. Mechanical properties of the compacts were good, and comparable to those of the polycrystalline Ni-Mn-Ga samples in compression.     

Effect of nitrogen addition on the stress corrosion cracking behavior of 904 L stainless steel welds in 288 °C deaerated water

This paper concerns with the effect of nitrogen addition to 904 L stainless steel (SS) welds on their stress corrosion cracking (SCC) behavior in high temperature (288 °C) and high pressure (1050 psi) water of high oxygen content (100 ppb) and high conductivity (2.5 μS/cm). For this study, 316 L SS base plate TIG welded with 904 L SS filler wire and with nitrogen contents of 0.027, 0.058 and 0.095 wt.% were used. Flat pin-loaded tensile specimens were fabricated from transverse welds, with the weld in the gauge length. Slow strain rate tests (SSRT) were carried out at a strain rate of 2.2 × 10⁻⁶ s⁻¹. The study shows that the samples, when tested in air, failed at the weld fusion zone for 0.027 and 0.058 wt.% N and at the base metal for 0.095 wt.% N. In the environment, the samples failed in the base metal except the one with least nitrogen content (0.027 wt.%). With nitrogen addition, as the failure location shifted to the base alloy, the weld seemed to acquire SCC resistance and became even more resistant than the base alloy.     

Effect of solubility on strengthening of Ag-Cu ultrafine eutectic composites

A series of binary Ag_80−xCu_20+x ultrafine eutectic composites with x = 0, 10, 20, 30 and 40 is prepared by copper mold casting in order to systematically investigate an influence of asymmetrical solubility between Ag and Cu solid solutions on the strengthening of ultrafine eutectic composites. The asymmetrical solubility of the ultrafine eutectic composites determined by the effective solubility index derived from rule of mixtures plays an important role to maintain the strength even with increasing the volume fraction of the micron-scale dendrites. Based on the results, the control of the strengthening of the ultrafine eutectic composites is governed by not only well-known volume fraction of the micron-scale dendrites but also the solubility in the micron-scale dendrites.     

Mullite-rich plasma electrolytic oxide coatings for thermal barrier applications

A study has been undertaken of the characteristics exhibited by mullite-rich plasma electrolytic oxide coatings grown on aluminium alloys by using silicate-rich electrolytes. It is found that they can be grown at a higher rate, and to a greater thickness, than alumina PEO coatings on aluminium. The thermal conductivity of these coatings has been measured using a steady-state method. It is shown to be of the order of 0.5 W m^− 1 K^− 1, which may be compared with ∼ 1.5 W m^− 1 K^− 1 for pure alumina PEO coatings and ∼ 10-15 W m^− 1 K^− 1 for dense polycrystalline mullite. Coupled with excellent substrate adhesion and good mechanical properties, this relatively low conductivity makes these coatings attractive for thermal barrier applications. Furthermore, they are shown to exhibit a relatively low global stiffness (∼ 40 GPa), which will reduce the magnitude of thermally-induced stresses and improve the resistance to spallation during temperature changes.     

Solution-phase chemical route to branched single-crystalline CdS nanoarchitectures and their field emission property

A facile solution chemical method is developed to prepare hierarchical branched single-crystalline CdS architectures. A mechanism of “nucleate-aggregate-grow-ripen-separate” process is proposed to illustrate the growth of the CdS architectures. The obtained branched CdS architectures exhibit superior FE properties with the lower turn-on field (Eto) of 7.1 V μm⁻¹ at a current density of 10 μA cm⁻², and threshold field (Ethr) of 8.3 V μm⁻¹ at a current density of 100 μA cm⁻², which shows that the obtained products have greatly potential application as FE devices.     

Room temperature ferromagnetism in Mn-doped zinc oxide nanorods prepared by hybrid wet chemical route

Mn-doped (2.6-4.8 at%) aligned zinc oxide (Mn:ZnO) nanorod-films were synthesized by hybrid wet chemical route onto glass substrates. The chemical composition, structural, microstructural and magnetic studies were performed to investigate the origin of observed room temperature ferromagnetism (∼0.11 μ_B/Mn) in these Mn doped ZnO nanorod-films. XPS studies indicated that incorporated Mn was in Mn²⁺ and Mn⁴⁺ states. Mn²⁺ atomic concentration was found to be significantly larger than Mn⁴⁺ concentration in all the samples. Disappearance of the Raman peak at ∼577 cm⁻¹ arising due to the Zn interstitials may be related to the substitution of Mn²⁺ in the Zn²⁺ site with annealing. Thus, Mn metal inclusions as Mn²⁺ in the ZnO lattice are possibly responsible for such large magnetic moment in the films.     

Workpiece surface integrity when slot milling γ-TiAl intermetallic alloy

Slot milling is presented as a potential manufacturing route for aerospace component feature production when machining γ-TiAl intermetallic alloy Ti–45Al–2Mn–2Nb + 0.8 vol.% TiB₂XD using 2 mm diameter AlTiN coated WC ball nose end milling cutters. When operating with flood cutting fluid at v = 88 m/min, f = 0.05 mm/tooth, d = 0.2 mm, maximum flank wear was ∼65 μm after 25 min. SEM micrographs of slot surfaces show re-deposited/adhered and smeared workpiece material to a length of ∼50 μm. Brittle fracture of the slot edges was restricted to <10 μm with sporadic top burr formation observed up to ∼20 μm. Cross sectional micrographs of the slot sidewalls showed bending of the lamellae limited to within 5 μm.