Processing, physico-chemical characterisation and in vitro evaluation of silicon containing β-tricalcium phosphate ceramics

For bone grafting applications, the elaboration of silicon containing beta-tricalcium phosphate (β-TCP) was studied. The synthesis was performed using a wet precipitation method according to the hypothetical theoretical formula Ca_3 − x(PO₄)_2 − 2x(SiO₄)_x. Two silicon loaded materials (0.46 wt.% and 0.95 wt.%) were investigated and compared to a pure β-TCP. The maturation time of the synthesis required in order to obtain β-TCP decreased with the amount of silicon. Only restrictive synthesis conditions allow preparing silicon containing β-TCP with controlled composition. To obtain dense ceramics, the sintering behaviour of the powders was evaluated. The addition of silicon slowed the densification process and decreased the grain size of the dense ceramics. Rietveld refinement may indicate a partial incorporation of silicon in the β-TCP lattice. X-ray photoelectron spectroscopy and transmission electron microscopy analyses revealed that the remaining silicon formed amorphous clusters of silicon rich phase. The in vitro biological behaviour was investigated with MC3T3-E1 osteoblast-like cells. After the addition of silicon, the ceramics remained cytocompatible, highlighting the high potential of silicon containing β-TCP as optimised bone graft material.     

Microstructural characterisation and mechanical properties of Ni–Ge alloys containing Ni3Ge

Abstract

Six Ni–Ge alloys were prepared and equilibrated at 1000°C. The microstructures, compositions of phases, solubilities in various phases, volume fractions of phases, lattice parameters of Ni₃ Ge, and microhardness values of phases were determined. Two alloys contained Ni₃Ge and α, one alloy was single phase Ni₃Ge, and three alloys contained Ni₃Ge and Ni₅Ge₃. The volume fractions of second phase were 6 and 33%α and 37 and 54%Ni₅Ge₃. The amount of second phase in the third Ni₃Ge–Ni₅Ge₃ alloy was too low to be determined accurately. The two phase alloys containing 6%α, 37%Ni₅Ge₃, or 54%Ni₅Ge₃ were tested in compression. A yield strength maximum was observed in the three alloys. The deformation behaviour of the alloy containing 6%α was similar to that of single phase Ni₃Ge: crack formation along Ni₃Ge grain boundaries and very low plastic strain were revealed. In alloys containing Ni₃Ge and an appreciable percentage of Ni₅Ge₃, crack formation was not observed along Ni₃Ge grain boundaries. Instead, at low temperatures, deformation and crack growth occurred within Ni₅Ge₃ grains and, at high temperatures, decohesion occurred along the Ni₃Ge/Ni₅Ge₃ interphase. The plastic strain in the alloy containing 54%Ni₅Ge₃ increased to about 40%.

MST/1724     

An investigation on the precipitated phases and mechanical properties of cerium modified 2024 aluminum alloy

The effects of the addition of rare earth cerium on the cast microstructure and mechanical properties of 2024-T6 aluminum alloy were investigated in this work. The specimens for room-temperature tensile tests were prepared with a T6 heat treatment. Experimental results indicated that the cerium modified alloys showed refined grains, higher hardness, and strength values at room temperature. The hardness and the strength of the cerium modified alloys initially increased and then decreased as the cerium content increased. The maximum tensile strength was obtained at the 0.6 wt.% cerium modified 2024 aluminum alloy. This was improved from 464 MPa to 612 MPa. Simultaneous increases in the tensile strength and hardness were proposed to result from the refined α-aluminum dendrites, the formation of aluminum-rare earth intermetallic compounds at the grain boundaries and the grains, the more homogeneously distributed nano-scale S precipitates, and the smaller T diffusion phase.     

Microstructural investigation and indentation response of pressureless-sintered α- and β-SiC

The microstructure and indentation response of pressureless-sintered - and -SiC were studied using a high-resolution electron microscope and analytical electron microscopy. The materials were manufactured with boron and carbon as sintering aids. It was found that the overall porosity of the materials was very low but a large number of carbon inclusions were present. X-ray diffraction revealed the fabricated -SiC material was of the same 3C polytype as the initial starting powder; however, electron microscope observations indicated that the material contained a high density of faulting of the -forms. High-resolution imaging of grain boundaries in these materials indicated that the boundaries were very clean, and when they contained an amorphous intergranular film it was at most 0.5 to 1 nm thick. The presence of boron was not detected. Deformation due to identation took several forms. Firstly, radial cracks extending from the corners of the indent suffered little hindrance from the matrix microstructure, such that transgranular fracture was the dominant mode. Secondly, the deformation zone beneath the indentations showed copious lattice microcracks with some preferred orientation during crack formation and propagation.     

Chromium removal on chitosan-based sorbents – An EXAFS/XANES investigation of mechanism

Chitosan is known to be a good sorbent for metal-containing ions as the presence of amino groups and hydroxyl functions act as effective binding sites. Its crosslinking, employing glutaraldehyde or epichlorohydrin, may change the sorption properties (sorption capacity or diffusion properties) of this biopolymer, since the available functional groups are different in each case. X-ray absorption spectroscopy (XAS), including extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES), Fourier-transformed infrared spectroscopy with attenuated total reflectance device (FTIR-ATR) was used along with speciation diagrams, in order to identify the binding groups involved in chromate sorption and its mechanisms. In pristine chitosan and epichlorohydrin-crosslinked chitosan membranes, amino groups are most likely responsible for adsorption, although the contribution of hydroxyl groups cannot be excluded (especially for metal-sorbent stabilization). In this case, when adsorbed about 70% of chromate ions remain in the Cr(VI) oxidation state. In the case of glutaraldehyde-crosslinked membranes, the functional groups involved are different. Carbonyl groups and imino bonds – resulting from the reaction of the crosslinking agent and amino groups – may be involved in the adsorption mechanism. Additionally, a higher fraction of chromate anions, around 44% are reduced to Cr(III) oxidation state in loaded sorbent. The presence of free aldehyde groups may explain this partial reduction.     

Polypropylene-blended organoclay nanocomposites – preparation,characterisation and properties

Intercalated/exfoliated nanocomposites of thermoplastic polyolefin (TPO) blended nanoclay (Cloisite 20?A and Cloisite 30B) were fabricated using melt extrusion process. Polypropylene grafted maleic anhydride (PP-g-MA) was used as a compatibiliser to improve the dispersibility of clay. TPO/nanoclay composites were prepared with different percentages of clay loading (3, 5 and 7?wt%) by adding PP-g-MA as a compatibiliser. The nanocomposites having 5?wt%C20A/5?wt% compatibiliser exhibited a remarkable improvement in mechanical (tensile modulus, flexural modulus and impact strength) and thermal (heat distortion temperature, HDT) properties. The thermal measurements have been carried out by differential scanning calorimetry, thermogravimetric analysis and HDT methods. Dynamic mechanical analysis studies indicated that PP macromolecules were intercalated or exfoliated between the interlayer of silicates. The morphology of nanocomposites was characterised by scanning electron microscopy (SEM) and X-ray diffraction (XRD) was used to find out the arrangement of crystals in the nanocomposites. The SEM and XRD clearly demonstrated the progressive break up of particles and results in decreased particle size with the optimised combination.     

Mechanical and structural characterisation of Nicalon SiC fibres up to 1300°C

The resurgence of interest in metal matrix composites has been fuelled by the development of new fibres with high temperature characteristics. The new family of continuous fine ceramic fibres based on SiC or Al₂O₃ offers the possibility of producing high temperature composites with metal or ceramic matrices. The toughening of ceramics by these fibres is a particularly interesting prospect.Two types of continuous silicon carbide Nicalon monofilaments (NLP 101 and NLM 102) have been tested in air and argon up to 1300°C. Tensile and creep tests have shown that the tensile strength falls and the fibres creep above 1000°C. Different behaviour was found for the two types of fibres. The NLM 102 fibre was stronger and crept less at high temperature under small strains. However its creep lifetime was less than that of the NLP 101 fibres.These differences have been interpreted with the aid of a microstructural study. The fibres were found to contain silicon, carbon and oxygen (electron microphobe and Auger spectrometer) and SiC was also detected (X-ray diffraction and transmission electron microscopy). The modification of the amorphous and microcrystalline structures during creep have been investigated. A fine segregation of free carbon particles was detected (X-ray diffraction and ESR) and was seen to disappear during heat treatment in both types of environment studied.     

Effect of moisture on the mechanical properties of CFRP–wood composite: An experimental and atomistic investigation

Adhesive bonding of fiber-reinforced polymers (FRP) to wood has been proven as a general way to achieve reinforcement and rehabilitation for wood structures. Although a significant mechanical enhancement can be acquired by using such approach, there exists a big concern about the long-term performance of the FRP–wood composite, especially under the effect of moisture. In this paper, both experimental and atomistic approaches are adopted for investigating the moisture effect on the entire FRP–wood composite system. Macroscopic mechanical tests show that its mechanical properties and its fracture behaviors notably change at different levels of ambient humidity. From an atomistic perspective, molecular dynamics (MD) simulations reveal that water molecules significantly reduce the adhesion energy between wood and epoxy. Results from experimental and numerical studies imply that the strength of the FRP–wood interface critically determines the mechanical performance of the entire system. The water molecules absorbed at the interface are crucial to the durability of multi-layer systems and a general mechanism governing the failure modes of such systems is found.     

Manufacture and mechanical characterisation of high voltage insulation for superconducting busbars – (Part 1) Materials selection and development

It is planned that the high voltage electrical insulation on the ITER feeder busbars will consist of interleaved layers of epoxy resin pre-impregnated glass tapes (‘pre-preg’) and polyimide. In addition to its electrical insulation function, the busbar insulation must have adequate mechanical properties to sustain the loads imposed on it during ITER magnet operation. This paper reports an investigation into suitable materials to manufacture the high voltage insulation for the ITER superconducting busbars and pipework. An R&D programme was undertaken in order to identify suitable pre-preg and polyimide materials from a range of suppliers. Pre-preg materials were obtained from 3 suppliers and used with Kapton HN, to make mouldings using the desired insulation architecture. Two main processing routes for pre-pregs have been investigated, namely vacuum bag processing (out of autoclave processing) and processing using a material with a high coefficient of thermal expansion (silicone rubber), to apply the compaction pressure on the insulation. Insulation should have adequate mechanical properties to cope with the stresses induced by the operating environment and a low void content necessary in a high voltage application. The quality of the mouldings was assessed by mechanical testing at 77 K and by the measurement of the void content.     

Influence of water ageing on mechanical properties and damage events of two reinforced composite materials: Flax–fibres and glass–fibres

Moisture absorption and durability in water environment are major concerns for natural fibres as reinforcement in composites. This paper presents a study on the influence of water ageing on mechanical properties and damage events of flax–fibre composites, compared with glass–fibre composites. The effects of the immersion treatment on the tensile characteristics, water absorption and acoustic emission (AE) recording were investigated. The water absorption results for the flax–fibre composites show that the evolution appears to be Fickian and the saturated weight gain is 12 times as high that the glass–fibre composites. Decreasing continuously with increasing water immersion time, the tensile modulus and the failure strain of flax–fibre composites are hardly affected by water ageing whereas only the tensile stress is reduced regarding the glass–fibre composites. AE indicate that matrix–fibres interface weakening is the main damage mechanism induced by water ageing for both composites.     

Microstructural and mechanical properties of Sn–Ag–Cu lead-free solders with minor addition of Ni and/or Co

The effects of minor additives, that is, Co and Ni, on the microstructural and mechanical properties of Sn–3.0 mass%Ag–0.5 mass%Cu (SAC305) bulk solder were investigated. The addition of Co and/or Ni resulted in microstructural changes of the SAC305 solder, such as the formation of new intermetallic compounds (IMCs) and the refinement of grain size, as well as the suppression of undercooling. The single addition of Co in SAC305 solder resulted in the formation of CoSn₂ IMCs and undercooling suppression, whereas the single addition of Ni accelerated the appearance of rod-shaped (Cu,Ni)₆Sn₅ IMCs inside the β-Sn dendrites during the solidification process. The dual addition of Co–Ni resulted in refined β-Sn grains and suppression of undercooling, as well as the formation of CoSn₂ IMCs. In tensile tests, Co and/or Ni additives had little effect on the tensile strength of SAC305 solder, but obviously suppressed the elongation ratio and reduction of area. During tensile deformation in samples with existing thin plate-like CoSn₂ IMCs, micro-cracks or cavities were easily initiated through the interface between CoSn₂ and the solder matrix, which was responsible for the decrease of ductility.     

Microstructural and mechanical characterization of Al–15%Mg2Si composite containing chromium

The microstructure and mechanical properties of Al–15%Mg₂Si composite containing different Cr contents (0.5 wt.%–5 wt.%) were studied. Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis were utilized to study the microstructures and fracture surfaces of the composite. The results revealed that the addition of Cr contents changes the size and morphology of both primary and eutectic Mg₂Si phases. A new intermetallic compound (Al₁₃Cr₄Si₄) was detected through the microstructural studies at higher Cr levels. Adding Cr also made significant raise in the hardness, ultimate tensile strength (UTS) and elongation values of the composite. A slight reduction in tensile properties was seen at high Cr concentrations (>2 wt.% Cr). The study of fracture surfaces of the Al–15%Mg₂Si–2%Cr composite revealed the presence of less broken particles and more fine dimples.     

An IR and XPS spectroscopy assessment of the physico-chemical surface properties of alumina–YAG nanopowders

Well-dispersed nano-crystalline transition alumina suspensions were mixed with yttrium chloride aqueous solutions, with the aim of producing by spray-drying Al₂O₃–Y₃Al₅O₁₂ (YAG) composite powders of increasing YAG vol.%. Two samples were prepared, with different Y content, corresponding to 5 and 20 YAG vol.%, respectively. Both samples were then treated at either 600 or 1150 °C. The obtained powders were characterized by X-Ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Fourier Transform Infra Red (FT-IR) spectroscopy and compared to three reference samples: commercial nano-crystalline transition alumina, YAG and Y₂O₃. YAG powders were obtained by co-precipitation route whereas Y₂O₃ powders were yielded by spray-drying of a yttrium chloride aqueous solution. Modification of physico-chemical properties of the surface of alumina nanoparticles were assessed by combining XPS and FT-IR spectroscopies. On the basis of the results obtained, a possible model is proposed for the structure of the obtained composites, in which Y basically reacts with more acidic hydroxyls of alumina, by forming Y-rich surface grains, the extension of which depends on the thermal treatment.     

In situ and operando characterisation of Li metal – Solid electrolyte interfaces

The use of lithium metal as the negative electrode holds great promise for high energy density solid-state batteries (SSBs) of the future, but at the same time presents major technical challenges in their development. Li metal, with its high reactivity, soft and ductile nature, and propensity towards mechanical deformation during electrochemical cycling, is susceptible to the formation of various defects such as voids, cracks and filamentary deposits at the Li metal - solid electrolyte interface, that eventually cause rapid degradation of electrochemical cell performance. In order to gain insights into these interfacial processes and identify mechanisms for failure, in situ and operando characterisation approaches are essential. In this perspective, we present our opinions on the current state of such techniques, while highlighting the existing limitations and scope of these methods. We also endeavour to present opportunities for future research into developing and building on existing approaches to better evaluate the Li metal-solid electrolyte interface so as to guide the appropriate choice of materials to further enable efficient SSB architectures.     

A review of bast fibres and their composites. Part 2 – Composites

Bast fibres are defined as those obtained from the outer cell layers of the stems of various plants. The fibres find use in textile applications and are increasingly being considered as reinforcements for polymer matrix composites as they are perceived to be “sustainable”. The fibres are composed primarily of cellulose which potentially has a Young’s modulus of ～140 GPa (being a value comparable with man-made aramid [Kevlar/Twaron] fibres). The plants which are currently attracting most interest are flax and hemp (in temperate climates) or jute and kenaf (in tropical climates). Part 2 of this review will consider the prediction of the properties of natural fibre reinforced composites, manufacturing techniques and composite materials characterisation using microscopy, mechanical, chemical and thermal techniques. The review will close with a brief overview of the potential applications and the environmental considerations which might expedite or constrain the adoption of these composites.     

Microstructural characterisation and thermal stability of in situ TiB2/60Si–Al composite synthesised by displacement reactions and spray forming

Abstract

A novel in situ reactive technique has been employed for preparing 2·0 wt-%TiB₂/60Si–Al composite. The kinetic equations and the Arrhenius type equation were applied to compute the coarsening rate constant and the activation energy for grain growth for the composite when it was heated at semisolid state for partial remelting. Experimental results have shown that the in situ TiB₂ particles can refine effectively the primary Si phase and restrain the Si phase growth. The cubic coarsening rate constant for the composite was computed to be in the range of 75–148 μm³ min^?1 at temperatures in the range of 600–700°C, which was much less than that for the 60Si–Al alloy (1323–4523 μm³ min^?1). The value of activation energy for grain growth for the composite was about twice of that for the 60Si–Al alloy. The composite exhibited a higher thermal stability than that of the 60Si–Al alloy, suggesting that the in situ TiB₂ particles can effectively pin the grain boundaries and arrest the migration of liquid film in the semisolid state of the composite.     

Effect of β heat treatment temperature on microstructure and mechanical properties of in situ titanium matrix composites

TiB and La₂O₃ reinforced titanium matrix composites were in situ prepared by casting and hot working. An effort was made to investigate relationship between β heat treatment temperature, microstructure and mechanical properties. Tensile tests were performed at room temperature, 600, 650 and 700 °C, respectively. Results indicated that composites treated at 10 °C above β transus points obtained fine grain microstructures and superior mechanical properties. When composites were treated at 20 °C above β transus points, the larger α colonies sizes led extremely decreased strength and the effect of reinforcements’ volume fraction on matrix of composites was reduced; dominant failure modes at high temperatures also differed from the fine microstructure.     

Microstructural and mechanical behavior of SnCu–Ge solder alloy subjected to high temperature storage

This paper addresses the effect of high temperature storage on the microstructural and mechanical behavior of novel SnCu–Ge solder alloys. Eutectic Sn99.3Cu0.7 solder was micro-alloyed with the addition of minor Ge as an anti-oxidant and to improve the wetting performance of the alloy. The addition of Ge significantly reduced the aging degradation of the alloy. The ultimate tensile strength and yield stress dropped within first few days of aging and the fracture strain increased with aging. The corresponding microstructure changed after annealing at 125 °C for 3 months; the average grain size of the β-tin portions of the microstructure increased with aging and the imbedded IMC particles segregated along and/or within the grains. Based on growth kinetics and activation energy arguments, we suggest that the addition of Ge restricts the Cu diffusion into the alloy and inhibits the IMC growth.     

Microstructural characterisation and corrosion behaviour of laser cladded Al–12Si alloy onto magnesium AS41/carbon fibre composite

Abstract

The quality and properties of laser clad layers are dependent on the microstructure and properties of the interfaces with the substrate. The present paper reports, in details, on the characterisation of microstructure of the coating and interfacial layers evolved as a result of the CO₂ laser remelting of previously plasma sprayed Al–12Si alloy onto C short fibres reinforced AS41–Mg composite. Scanning electron microscopy (SEM), wavelength dispersive X-ray (WDX) analysis and X-ray diffraction (XRD) were employed to identify the phases arising in the interfacial layers. The latter are composed mainly of Mg₁₇Al₁₂ and Mg₂Si phases. XRD was conducted on the clad layers at different distances from the interface. At the same layers, the potentiodynamic polarisation in sodium chloride solution was measured and it was found that as the Mg content increases in the clad coating, the corrosion resistance decreases. However, the corrosion current of the clad coating is around two orders of magnitude lower than that of the C/Mg composite.