Phase formation and physical properties of mechanically alloyed amorphous 55Mg35Ni1OSi

Amorphous 55Mg35Ni10Si alloy powder has been synthesized by mechanical alloying technique using pure Mg, Ni and Si elemental powders. The transformation of the crystalline powders into an amorphous one has been investigated by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and differential scanning calorimetry. The new material produced has a higher thermal stability than reported results, which is beneficial to the fabrication of Mg–Ni–Si bulk amorphous components through powder metallurgy.

One-step vapour-phase formation of patternable, electrically conductive, superamphiphobic coatings on fibrous materials

Patternable, electrically conductive coatings having a superhydrophobic and superoleophobic surface have been prepared by one-step vapour-phase polymerisation of polypyrrole in the presence of a fluorinated alkyl silane directly on fibrous substrates. The coated fabrics showed a surface resistance of 0.5-0.8 kΩ □^-1 with water and hexadecane contact angles of 165° and 154°, respectively.

Sol-gel derived hydroxyapatite/titania biocoatings on titanium substrate

A simple sol–gel method was successfully developed for a hydroxyapatite (HA)/TiO₂ double layer deposition on a pure titanium substrate. Phase formation, surface morphology, and interfacial microstructure were investigated by differential scanning calorimetry analysis (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The TiO₂ layer was coated by a spin coating method at a speed of 1500 rpm for 15 s, followed by a heat treatment at 560 °C for 20 min. The HA film was subsequently spin coated on the outer surface at the same speed and then heat-treated at difference temperatures. Results indicated that the HA phase began to crystallize after a heat treatment at 580 °C; and the crystallinity increased obviously at a temperature of 780 °C. The HA film showed a porous structure and a thickness of 5–7 μm after the heat treatment at 780 °C. SEM observations revealed no delamination and crack at the interfaces of HA/TiO₂ and TiO₂/Ti. The HA film with a porous structure is expected to be more susceptible to the natural remodeling processes when it is implanted in a living body.

Effects of process control agent on the microstructure and mechanical properties of Ti-Sn-Nb alloy prepared by mechanical alloying

In the present study, the influence of process control agent (PCA) on the characteristics of powder and bulk sintered Ti-16Sn-4Nb (wt. %) alloy prepared by mechanical alloying has been investigated. The elemental Ti, Sn and Nb powders were mechanically alloyed in a planetary ball mill for a short period of time using two types of PCA, namely stearic acid (SA) and ethylene bis-stearamide (EBS). The powder morphology, microstructural evolution of the bulk sintered alloy, phase formation and hardness of the alloy have been studied as a function of PCA. Results indicated that the addition of PCA leads to a delay in aIloy formation and introduces contaminations (mainly carbon and oxygen) into the material. The microstructural observation of the bulk alloy revealed a homogeneous distribution of fine Nb-rich colonies (ß-phase) within the a-Ti matrix for small amount of PCA. The hardness values of samples exhibited a significant increase with increasing amount of PCA, reaching a value of ~ 600 BV.

Novel sphene coatings on Ti–6Al–4V for orthopedic implants using sol–gel method

Hydroxyapatite (HAp) is commonly used to coat titanium alloys (Ti–6Al–4V) for orthopedic implants. However, their poor adhesion strength and insufficient long-term stability limit their application. Novel sphene (CaTiSiO₅) ceramics possess excellent chemical stability and cytocompatibility. The aim of this study is to use the novel sphene ceramics as coatings for Ti–6Al–4V. The sol–gel method was used to produce the coatings and the thermal properties, phase composition, microstructure, thickness, surface roughness and adhesion strength of sphene coatings were analyzed by differential thermal analysis–thermal gravity (DTA–TG), X-ray diffraction (XRD), scanning electron microscopy (SEM), atom force microscopy (AFM) and scratch test, respectively. DTA analysis confirmed that the temperature of the sphene phase formation is 875 °C and XRD analysis indicated pure sphene coatings were obtained. A uniform structure of the sphene coating was found across the Ti–6Al–4V surface, with a thickness and surface roughness of the coating of about 0.5–1 μm and 0.38 μm, respectively. Sphene-coated Ti–6Al–4V possessed a significantly improved adhesion strength compared to that for HAp coating and their chemical stability was evaluated by testing the profile element distribution and the dissolution kinetics of calcium (Ca) ions after soaking the sphene-coated Ti–6Al–4V in Tris–HCl solution. Sphene coatings had a significantly improved chemical stability compared to the HAp coatings. A layer of apatite formed on the sphene-coated Ti–6Al–4V after they were soaked in simulated body fluids (SBF). Our results indicate that sol–gel coating of novel sphene onto Ti–6Al–4V possessed improved adhesion strength and chemical stability, compared to HAp-coated Ti–6Al–4V prepared under the same conditions, suggesting their potential application as coatings for orthopedic implants.

Different thermal analysis technique application in determination of fold surface-free energy

In this work, the crystallization rates and spherulitic growth rate of miscible blends of poly(vinylidene fluoride) (PVDF) and acrylic rubber (ACM) were determined using differential scanning calorimetry (DSC), real-time FTIR, and optical microscopy. FTIR results suggest that blending does not induce the creation of polymorphic crystalline forms of PVDF. SAXS data demonstrate the formation of interlamellar structure after blending. The fold surface-free energy (σ e) was analyzed and compared using different thermal analysis techniques. The isothermal crystallization curves obtained using real-time FTIR and DSC explored in two different methods: t 1/2 or Avrami equation. While the Avrami equation is more widespread and precise, both analytical methods gave similar free energy of folding values. However, it was found that the direct optical method of measuring spherulitic growth rate yields σ e values 30-50 % lower than those obtained from the overall crystallization rate data. Conversely, the σ e values were found to increase with increasing amorphous ACM phase content regardless of the analytical methods.

Fluidized bed CrN coating formation on prenitrocarburized plain carbon steel

CrN coatings were formed on plain carbon steel by prenitrocarburizing, followed by thermoreactive deposition and diffusion (TRD) in a fluidized bed furnace at 570 °C. During TRD, Cr was transferred from Cr powder in the fluidized bed to the nitrocarburized substrates by gas-phase reactions initiated by reaction of HCl gas with the Cr. The microstructural processes occurring in the white layer, caused by N diffusion toward the surface during this stage were studied. This study compares TRD atmospheres employing inert gas and HCl or inert gas, H2, and HCl. Surface characterization was performed by scanning electron microscopy (SEM), x-ray diffraction (XRD), and glow-discharge optical-emission spectroscopy (GDOES).

Cr(N,C) diffusion coating formation on pre-nitrocarburised H13 tool steel

The microstructural processes of Cr(N,C) coating formation by thermoreactive deposition and diffusion (TRD) on pre-nitrocarburised H13 tool steel were studied. Both nitrocarburising and TRD were performed in fluidized bed furnaces at 570 °C. During TRD, chromium was transferred from chromium powder in the fluidized bed, to the nitrocarburised substrates by gas-phase reactions initiated by reaction of HCl gas with the chromium. Addition of 30% H2 to the input inert gas was found to increase the rate of coating formation, although hydrogen reduction resulted in rapid loss of nitrogen to the surface. The reason for the increased rate of coating formation could not be established without further investigation, although several possible explanations have been proposed. It was found that porosity and the formation of an iron nitride ‘cover layer’ during nitrocarburising were the biggest influences on the microstructure of the Cr(N,C) coating. Microstructural characterization of the coatings was performed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and glow discharge optical emission spectroscopy (GDOES).

Effect of thermomechanical parameters on the critical strain for ultrafine ferrite formation through hot torsion testing

A C–Mn–V steel was used to study ultrafine ferrite formation (1–3 μm) through dynamic strain-induced transformation (DSIT) using hot torsion experiments. A systematic study determined the critical strain for the start of DSIT (C,DSIT), although this may not lead to a fully ultrafine microstructure. Therefore, the strain to produce an ultrafine ferrite (UFF) as final microstructure (C,UFF) during deformation was also determined. In addition, the effect of thermomechanical parameters such as deformation temperature, prior austenite grain size, strain rate and cooling rate on C,DSIT and C,UFF has been evaluated. DSIT ferrite nucleated on prior austenite grain boundaries at an early stage of straining followed by intragranular nucleation at higher strains. The prior austenite grain size affected the distribution of DSIT ferrite nucleation sites at an early stage of transformation and the subsequent coarsening behaviour of the grain boundary and intragranular ferrite grains during post-deformation cooling. Also, C,DSIT and C,UFF increased with an increase in the prior austenite grain size and deformation temperature. The post-deformation cooling had a strong effect not only on C,UFF but also the UFF microstructure (i.e. final ferrite grain size and second phase characteristics).

Ultrafine grained structure formation in steels using dynamic strain induced transformation processing

The refinement of ferrite grain size is the most generally accepted approach to simultaneously improve the strength and toughness in steels. Historically, the level of ferrite refinement is limited to 5-10 μm using conventional industrial approaches. Nowadays, though, several thermomechanical processes have been developed to produce ferrite grain sizes of 1-3 μm or less, ranging from extreme thermal and deformation cycles to more typical thermomechanical processes. The present paper reviews the status of the production of ultrafine grained steels through relatively simple thermomechanical processing. This requires deformation within the Ae3 to Ar3 temperature range for a given alloy. Here, the formation of ultrafine ferrite (UFF) involves the dynamic transformation of a significant volume fraction of the austenite to ferrite. This dynamic strain induced transformation (DSIT) arises from the introduction of extensive intragranular nucleation sites that are not present in conventional controlled rolling. The DSIT route has the potential to be adjusted to suit current industrial infrastructure. However, there are a number of significant issues that have been raised, both as gaps in our understanding and as obstacles to industrial implementation. One of the critical issues is that it appears that very large strains are required. Combined with this concern is the issue of whether a combination of dynamic and static transformation can be used to achieve an adequate level of refinement. Another issue that has also become apparent is that grain sizes of 1 μm can lead to low levels of ductility and hence many workers are attempting to obtain 2-3 μm grains, or to introduce a second phase to provide the required ductility. There are also a number of areas of disagreement between authors including the role of dynamic recrystallisation of ferrite in the production of UFF by DSIT, the reasons for the low coarsening rate of UFF grains, the role of microalloying elements and the effects of austenite grain size and strain rate. The present review discusses these areas of controversy and highlights cases where experimental results do not agree.

Transmission electron microscopy characterization of the bake-hardening behavior of transformation-induced plasticity and dual-phase steels

The effect of prestraining (PS) and bake hardening (BH) on the microstructures and mechanical properties has been studied in transformation-induced plasticity (TRIP) and dual-phase (DP) steels after intercritical annealing. The DP steel showed an increase in the yield strength and the appearance of the upper and lower yield points after a single BH treatment as compared with the as-received condition, whereas the mechanical properties of the TRIP steel remained unchanged. This difference appears to be because of the formation of plastic deformation zones with high dislocation density around the “as-quenched” martensite in the DP steel, which allowed carbon to pin these dislocations, which, in turn, increased the yield strength. It was found for both steels that the BH behavior depends on the dislocation rearrangement in ferrite with the formation of cell, microbands, and shear band structures after PS. The strain-induced transformation of retained austenite to martensite in the TRIP steel contributes to the formation of a complex dislocation structure.

Prevalence of the thioamide {···H-N-C=S}2 synthon-solid-state (X-ray crystallography), solution (NMR) and gas-phase (theoretical) structures of O-methyl-N-aryl-thiocarbamides

Structural investigations, i.e. solid-state (X-ray), solution (¹H NMR) and gas-phase (theoretical), on molecules with the general formula MeOC(S)N(H)C₆H₄-4-Y: Y = H (1), NO₂ (2), C(O)Me (3), Cl (4) have shown a general preference for the adoption of an E-conformation about the central C–N bond. Such a conformation allows for the formation of a dimeric hydrogen-bonded {H–N–C=S}₂ synthon as the building block. In the cases of 1–3, additional C–H^...O interactions give rise to the formation of tapes of varying topology. A theoretical analysis shows that the preference for the E-conformation is about the same as the crystal packing stabilisation energy and consistent with this, the compound with Y = C(O)OMe, (5), adopts a Z-conformation in the solid-state that facilitates the formation of N–H^...O, C–H^...O and C–H^...S interactions, leading to a layer structure. Global crystal packing considerations are shown to be imperative in dictating the conformational form of molecules 1–5.

In situ formation of BN nanotubes during nitriding reactions

High-yield multiwalled boron nitride (BN) nanotubes have been produced using a ball milling-annealing method. The BN nanotubes with a diameter less than 10 nm and a well-crystallized multiwalled structure were formed via an in situ nitriding reaction. The systematic investigation of the formation process at different annealing temperatures and for different times suggested that the formation of the unique multiwalled structure was attributed by a two-dimensional growth of the BN phase and a nonmetal catalytic growth.