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In this study, advanced oxidation-protective CrSi coatings were developed and deposited on N-type (Zr,Ti)Ni(Sn,Sb) and P-type (Zr,Ti)Co(Sn,Sb) thermoelectric (TE) materials using an environmentally friendly closed field unbalanced magnetron sputtering PVD system. The oxidation behaviour of the CrSi-coated and uncoated samples was evaluated through static oxidation tests at 500 °C and 600 °C for 10h and 50 h, respectively. In addition, the samples were exposed to cyclic oxidation tests between 25 °C and 500 °C for 10, 30 and 50 cycles, with each cycle consisting of 1h of oxidation at 500 °C, to examine the coating ability to withstand thermal shock, which is involved in the service of TE devices. The surface morphology, cross-section layer structure, elemental distribution and phase constitution were analysed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX) and X-ray diffraction (XRD). The mass gain after the oxidation tests was measured and calculated for each sample to study the oxidation kinetics. The uncoated samples exhibited a considerable amount of oxidation, leading to change in the surface morphologies, and the formation of alternated layers including oxide products (Zr(Ti)O2, SnO2) and Ni3Sn4 compound for the N-type and (Zr(Ti)O2, SnO2, Sb2O4) and CoSb compound for the P-type material, after static and cyclic oxidation tests. The experimental work in this study has, for the first time, demonstrated that the CrSi coatings developed with very high thermal stability and oxidation resistance can effectively protect both the N-type and P-type materials from oxidation and sublimation even during cyclic oxidation tests. The strong affinity of Cr and Si to oxygen can trap oxygen, retard its inward diffusion and thus protect the TE material substrate from oxidation. This finding could pave the way towards the further development of long-life high-performance TE generators and devices, thus contributing to the net zero target.

In this study, the fabricated Hf-free N-type (Zr,Ti)Ni(Sn,Sb) and P-type (Zr,Ti)Co(Sn,Sb) thermoelectric materials were subjected to cyclic oxidation testing at 500 °C for 10, 30, and 50 cycles. The oxidation behaviour of the materials was systematically investigated by evaluating mass gain to study the oxidation kinetics and by analysing surface morphology, phase constitution and elemental distribution to investigate the oxidation mechanism. The results indicated that both of the materials were severely oxidised during the cyclic oxidation testing, and the mass gain followed the parabolic kinetics and the parabolic rate constant (kp) being 0.006165 mg2cm−4s−1 and 0.000109 mg2cm−4s−1 for the N-type and the P-type TE materials, respectively. Alternated multilayers of Ni3Sn4+SnO2+(Zr,Ti)O2 and CoSb + SnO2+Sb2O4+(Zr,Ti)O2 were identified on the surface of the N-type and P-type materials, respectively, after the cyclic testing, which would deteriorate the thermoelectric performance of the materials. The outcome of this study strongly suggests that it is essential to improve the oxidation resistance and the thermal stability of the N-type (Zr,Ti)Ni(Sn,Sb) and P-type (Zr,Ti)Co(Sn,Sb) thermoelectric materials for high-temperature applications.

In recent years, the utilisation of oxygen-deficient zirconia (ZrO2-α), commonly referred to as black zirconia, has garnered considerable attention due to its potential applications for solid oxide fuel cells (SOFCs), gas sensors, biomedical implant materials, and photocatalysis. However, current methods employed to manufacture ZrO2-α exhibit noticeable limitations regarding their scalability, environmental sustainability, and cost-effectiveness. Our recent work has successfully demonstrated the feasibility for bulk conversion of conventional white zirconia into oxygen-deficient black zirconia through direct current (DC) plasma treatment (i.e. plasma blackening). This study elucidates the conditions for plasma blackening and provides a unique mechanism for the bulk transformation of zirconia. A systematic investigation of different plasma technologies (DC, active-screen plasma), treatment configurations (contact conditions, cathode material, and cathode potential), and treatment parameters (voltage, temperature, duration) uncover the crucial variables that influence the feasibility and rate of the reduction process. The reduction of zirconia is shown to initiate from localised contacting points at the cathode-facing surface and grow, with a hemispherical shape, towards the anode-facing surface. A series of development stages are proposed for the process, namely: bulk oxygen vacancy conductance, surface activation, oxygen vacancy generation and a moving cathode front. The findings of this study provide insights into the underlying mechanisms involved in the bulk-reduction of zirconia and help to pave the way towards future scalable and cost-effective generation of oxygen-deficient zirconia.

The possibility of directly growing carbon nanofibers (CNFs) and carbon nanotubes (CNTs) on half-Heusler alloys by Chemical Vapour Deposition (CVD) is investigated for the first time, without using additional catalysts, since the half-Heusler alloys per se may function as catalytic substrates, according to the findings of the current study. As a carbon source, acetylene is used in the temperature range of 700–750 °C. The n-type half-Heusler compound Zr0.4Ti0.60.33Ni0.33Sn0.98Sb0.020.33 is utilized as the catalytic substrate. At first, a computational model is developed for the CVD reactor, aiming to optimize the experimental process design and setup. The experimental process conditions are simulated to investigate the reactive species concentrations within the reactor chamber and the activation of certain reactions. SEM analysis confirms the growth of CNFs with diameters ranging from 450 nm to 1 μm. Raman spectroscopy implies that the formed carbon structures resemble CNFs rather than CNTs, and that amorphous carbon also co-exists in the deposited samples. From the characterization results, it may be concluded that a short reaction time and a low acetylene flow rate lead to the formation of a uniform CNF coating on the surface of half-Heusler alloys. The purpose of depositing carbon nanostructures onto half-Heusler alloys is to improve the current transfer, generated from these thermoelectric compounds, by forming a conductive coating on their surface.

Low friction and high wear resistance are critical properties for sliding bearings. In this research, advanced Cu/GO nanocomposite coatings have been developed by a brush plating method to improve the tribological performance of brass-based sliding bearings. A series of brush plating studies under voltages from 2 to 6 V with different GO concentrations (0.2–0.8 g/L) was conducted, and the coating microstructures were characterised by SEM, EDX, GDOES and XRD and the tribological behaviour of the Cu/GO composite coatings were evaluated using dry ball-on-plane tribological tests The experimental results have demonstrated that GO can be successfully introduced into the whole composite coating layer; the Cu/GO composite coatings can reduce the friction of brass and increase its wear resistance by two orders of magnitude, mainly due to the self-lubricating GO added into the coatings.

Ceramic conversion treatment (CCT) is an effective way to modify the surface of titanium alloys. However, this process normally needs more than a 100-h treatment at 600–700 °C to form a hard and wear-resistant titanium oxide layer. In this paper, we pre-deposited a thin gold layer on the surface of Ti-6Al-2Sn-4Zr-2Mo (Ti6242) samples before CCT to investigate if Au can speed up the treatment. Treatments at 640/670/700 °C were carried out for 10 or 120 h. After CCT, the surface roughness, surface morphology, microstructure, elemental composition, and phase constituents were characterized. Surface hardness and the nano-hardness depth distribution were measured. Finally, reciprocating sliding tribological tests were carried out to study the friction and wear of the surface layers. Thin gold layers accelerated the CCT significantly with a much thicker oxide layer. The friction of the untreated Ti6242 alloy against the WC ball was unsteady and high, but it was much lower and stable for the CCTed samples pre-deposited with Au because of the formation of titanium oxides and lubrication effect of the gold particles. The wear resistance of the CCTed Ti6242 alloy samples with gold was reinforced significantly. By pre-depositing a thin gold layer on the surface of Ti6242, the treatment time can be cut significantly, and CCT becomes more efficient.

Thermoplastic polymers exhibit relatively limited surface energies and this results in poor adhesion when bonded to other materials. Plasma surface modification offers the potential to overcome this challenge through the functionalisation of the polymer surfaces. In this study, three polymers of differing hydrophobicity (HDPE, PA12, and PA6) were subjected to a novel, atmospheric, μPlasma surface treatment technique, and its effectiveness at increasing the surface energies was evaluated via measurement of the contact angle. To characterise the physical and chemical changes following μPlasma surface modification, the surface morphology was observed using atomic force microscopy (AFM), and the functionalisation of the surface was evaluated using infrared spectroscopy. Immediately after treatment, the contact angle decreased by 47.3° (HDPE), 42.6° (PA12), and 50.1° (PA6), but the effect was not permanent in that there was a pronounced relaxation or ageing phenomenon in operation. The ageing process over five hours was modelled using a modified stretched exponential function Kohlrausch–Williams–Watts (KWW) model, and it was found that the ageing rate was dependent on the hydrophilicity of polymers, with polyamides ageing more rapidly than polyethylene.

This study focuses on the development of a pilot-scale sizing line, including its initial design and installation, operational phases, and optimization of key process parameters. The primary objective is the identification of critical parameters for achieving a uniform sizing onto the fibres and the determination of optimal conditions for maximum production efficiency. This investigation focused on adjusting the furnace desizing temperature for the removal of commercial sizing, adjusting the drying temperature, as well as optimizing the corresponding residence time of carbon fibres passing through the furnaces. The highest production rate, reaching 1 m sized carbon fibres per minute, was achieved by employing a desizing temperature of 550 °C, a drying temperature of 250 °C, and a residence time of 1 min. Furthermore, a range of sizing solutions was investigated and formulated, exploring carbon-based nanomaterial types with different surface functionalizations and concentrations, to evaluate their impact on the surface morphology and mechanical properties of carbon fibres. In-depth analyses, including scanning electron microscopy and contact angle goniometry, revealed the achievement of a uniform coating on the carbon fibre surface, leading to an enhanced affinity between fibres and the polymeric epoxy matrix. The incorporation of nanomaterials, specifically N2-plasma-functionalized carbon nanotubes and few-layer graphene, demonstrated notable improvements in the interfacial shear properties (90% increase), verified by mechanical and push-out tests.

Titanium is characterized by poor wear resistance which restricts its application. Ceramic conversion treatment (CCT) is used to modify the surface; however, it is a time-consuming process. In this work, a thin vanadium layer was pre-deposited on the commercial pure titanium (CPTi) samples’ surface, and it increased the oxygen absorption significantly and assisted in obtaining a much thicker oxide layer than those samples without a V layer at the treatment temperatures of 620 °C and 660 °C. The oxidation of the samples pre-deposited with the V layer had a much higher oxidation rate, and V was evenly distributed in the oxide layer. After CCT, all samples had a low wear volume and stable coefficient of friction in comparison to the untreated CPTi sample. A slightly higher wear area in the wear track was observed on the V pre-deposited samples than those samples without vanadium, especially those with a thicker oxide layer (>4 µm). This might be associated with defects in a thicker oxide layer and insufficient support from a shallower oxygen diffusion zone or hard debris created at the initial stage. Vanadium in the oxide layer reduced the contact angles of the surface and increased the wettability significantly.

In this study, self-sensing materials have been developed owing to their ability to indicate material damage through an evident optical signal. For this, fluorescent core–shell microcapsules were synthesized by in situ polymerization in an oil-water emulsion. These microcapsules, embedded in a black epoxy resin, release a revealing substance during damage processes that allow microcracks detection in the material. The morphology, chemical structure, size distribution, thermal stability and mechanical properties of the fabricated microcapsules were characterized. Furthermore, the mechanical and optical characterizations of the composite were performed. As result, it has been shown how the microcracks cannot be observed under visible light but it was possible to identify and detect them under a conventional 254 nm ultraviolet (UV) lamp, introducing an additional functionality in the material for damage detection/monitoring.

In this study, a closed-field unbalanced magnetron sputtering system, which is environmentally friendly and has high deposition efficiency, was used to deposit CrSi coatings on 316 austenitic stainless steel. This system utilised separate Cr and Si targets, and the appropriate content of Cr and Si of the coatings was adjusted by changing the currents applied to the targets. A series of CrSi coatings with different Si/Cr ratios were produced, and their oxidation behaviour at elevated temperatures was investigated. By analysing the weight gain, surface morphology and microstructure, composition and phase constituents, the oxidation behaviour at 600 °C, 700 °C and 800 °C was investigated and the optimized coating to protect the stainless steel has been identified. The outcome of the research indicated that a small amount of Si (between 4–7 at.%) in Cr coatings is effective in protecting the austenitic stainless steel against oxidation at high temperatures, while a high Si content (around 10 at.% or more) makes the coating more brittle and prone to cracking or delamination during oxidation at 800 °C.

Zr and its alloys are widely used in multiple areas, including the nuclear and medical fields. Previous studies indicate that a ceramic conversion treatment (C2T) of Zr-based alloys can address the issues of low hardness, high friction, and poor wear resistance of Zr based alloys. This paper introduced a novel catalytic ceramic conversion treatment (C3T) to Zr702 by pre-depositing a catalytic film (such as silver, gold, platinum, etc.) before the ceramic conversion treatment, which efficiently promoted the C2T process, in terms of reduced treatment times, with a thick, good quality, surface ceramic layer. The formed ceramic layer significantly improved the surface hardness and tribological properties of Zr702 alloy. Compared with conventional C2T, the C3T technique provided two orders of magnitude reduction of wear factor and reduced the coefficient of friction from 0.65 to

Thermoelectric (TE) technology attracts much attention due to the fact it can convert thermal energy into electricity and vice versa. Thin-film TE materials can be synthesized on different kinds of substrates, which offer the possibility of the control of microstructure and composition to higher TE power, as well as the development of novel TE devices meeting flexible and miniature requirements. In this work, we use magnetron sputtering to deposit N-type and P-type BiTe-based thin films on silicon, glass, and Kapton HN polyimide foil. Their morphology, microstructure, and phase constituents are studied by SEM/EDX, XRD, and TEM. The electrical conductivity, thermal conductivity, and Seebeck coefficient of the thin film are measured by a special in-plane advanced test system. The output of electrical power (open-circuit voltage and electric current) of the thin film is measured by an in-house apparatus at different temperature gradient. The impact of deposition parameters and the thickness, width, and length of the thin film on the power output are also investigated for optimizing the thin-film flexible TE device to harvest thermal energy.

Three multifunctional smart composites for next-generation applications have been studied differently through versatile nanoindentation investigation techniques. They are used in order to determine peculiarities and specific properties for the different composites and to study the charge/matrix, charge/surface, or smart functions interactions. At first, a mapping indentation test was used to check the distribution of hardness and modulus across a large region to examine any non-uniformity due to structural anomalies or changes in properties for a carbon nanotubes (CNTs)-reinforced polypropylene (PP V-2) nanocomposite. This smart composite is suitable to be used in axial impeller fans and the results can be used to improve the process of the composite produced by injection moulding. Secondly, the interfacial properties of the carbon fibre (CF) and the resin were evaluated by a push-out method utilizing the smaller indentation tip to target the individual CF and apply load to measure its displacement under loads. This is useful to evaluate the effectiveness of the surface modification on the CFs, such as sizing. Finally, nanoindentation at different temperatures was used for the probing of the in situ response of smart shape memory polymer composite (SMPC) usable in grabbing devices for aerospace applications. Furthermore, the triggering temperature of the shape memory polymer response can be determined by observing the change of indentations after the heating and cooling cycles.

This paper investigated the modification of the advanced active screen plasma (ASP) technology on PAN-derived carbon fibres (CFs) with gas mixtures of N2-H2 and N2-H2-Ar, separately. A more-than-30% improvement was found in the interfacial shear strength (IFSS) between the modified CFs and the epoxy substrate in the resulting composites, as disclosed by single fibre push-out tests. Based on the study of surface morphology, surface chemistry and water-sorption behaviour, the interfacial adhesion enhancement mechanisms were attributed to (1) the increased chemical bonding between the introduced functional groups on the fibre surface and the matrix; (2) the improved surface hydrophilicity of CFs; and (3) the enhanced van der Waals bonding due to the removal of surface contaminations.

A polyamide (PA) 12-based thermoplastic composite was modified with carbon nanotubes (CNTs), CNTs grafted onto chopped carbon fibers (CFs), and graphene nanoplatelets (GNPs) with CNTs to improve its thermal conductivity for application as a heat sink in electronic components. The carbon-based nanofillers were examined by SEM and Raman. The laser flash method was used to measure the thermal diffusivity in order to calculate the thermal conductivity. Electrical conductivity measurements were made using a Keithley 6517B electrometer in the 2-point mode. The composite structure was examined by SEM and micro-CT. PA12 with 15 wt% of GNPs and 1 wt% CNTs demonstrated the highest thermal conductivity, and its processability was investigated, utilizing sequential interdependence tests to evaluate the composite material behavior during fused filament fabrication (FFF) 3D printing processing. Through this assessment, selected printing parameters were investigated to determine the optimum parametric combination and processability window for the composite material, revealing that the selected composition meets the necessary criteria to be processable with FFF.

Glass fibre reinforced polyamide 6 (GFPA6) thermoplastic composites (TPCs) are promising materials with excellent properties, but due to their low surface free energy they are usually difficult to wet, and therefore, possesses poor adhesion properties. μPlasma modification offers potential solutions to this problem through functionalisation of the GFPA6 surface. In this study, the effect of μPlasma on the wetting behaviour of GFPA6 surfaces was investigated. Following single μPlasma treatment scans of GFPA6 samples, a substantial enhancement in wettability was observed. However, the effect of the μPlasma modification was subject to an ageing (hydrophobic recovery) phenomenon, although the enhancement was still partially maintained after 4 weeks. The ageing process was slower when the GFPA6 material was pre-dried and stored in low humidity conditions, thereby demonstrating the importance of the storage environment to the rate of ageing. Orientation of the fibres to the observed contact angle was found to be crucial for obtaining reproducible measurements with lower deviation. The influence of testing liquid, droplet volume and surface texture on the repeatability of the measured contact angle were also investigated.

Titanium oxide layers were produced via a novel catalytic ceramic conversion treatment (CCCT, C3T) on Ti-6Al-4V. This CCCT process is carried out by applying thin catalytic films of silver and palladium onto the substrate before an already established traditional ceramic conversion treatment (CCT, C2T) is carried out. The layers were characterised using scanning electron microscopy, X-ray diffraction, transmission electron microscopy; surface micro-hardness and reciprocating tribological performance was assessed; antibacterial performance was also assessed with S. aureus. This CCCT has been shown to increase the oxide thickness from ~5 to ~100 µm, with the production of an aluminium rich layer and agglomerates of silver and palladium oxide surrounded by vanadium oxide at the surface. The wear factor was significantly reduced from ~393 to ~5 m3/N·m, and a significant reduction in the number of colony-forming units per ml of Staphylococcus aureus on the CCCT surfaces was observed. The potential of the novel C3T treatment has been demonstrated by comparing the performance of C3T treated and untreated Ti6Al4V fixation pins through inserting into simulated bone materials.

In this work, different amounts of CNFs were added into a complex formulation to coat the CFs surfaces via sizing in order to enhance the bonding between the fibre and the resin in the CF-reinforced polymer composites. The sized CFs bundles were characterised by SEM and Raman. The nanomechanical properties of the composite materials produced were assessed by the nanoindentation test. The interfacial properties of the fibre and resin were evaluated by a push-out method developed on nanoindentation. The average interfacial shear strength of the fibre/matrix interface could be calculated by the critical load, sheet thickness and fibre diameter. The contact angle measurements and resin spreadability were performed prior to nanoindentation to investigate the wetting properties of the fibre. After the push-out tests, the characterisation via optical microscopy/SEM was carried out to ratify the results. It was found the CFs sizing with CNFs (1 to 10 wt%) could generally increase the interfacial shear strength but it was more cost-effective with a small amount of evenly distributed CNFs on CFs.

Carbon Fibres (CFs) are widely used in textile-reinforced composites for the construction of lightweight, durable structures. Since their inert surface does not allow effective bonding with the matrix material, the surface treatment of fibres is suggested to improve the adhesion between the two. In the present study, different surface modifications are compared in terms of the mechanical enhancement that they can offer to the fibres. Two main advanced technologies have been investigated; namely, plasma treatment and electrochemical treatment. Specifically, active screen plasma and low-pressure plasma were compared. Regarding the electrochemical modification, electrochemical oxidation and electropolymerisation of monomer solutions of acrylic and methacrylic acids, acrylonitrile and N-vinyl pyrrolidine were tested for HTA-40 CFs. In order to assess the effects of the surface treatments, the morphology, the physicochemical properties, as well as the mechanical integrity of the fibres were investigated. The CF surface and polymeric matrix interphase adhesion in composites were also analysed. The improvement of the carbon fibre’s physical–mechanical properties was evident for the case of the active screen plasma treatment and the electrochemical oxidation.

Following the past successful four events in Leicester (2010), Wuhan (2012), Oxford (2014) and Chongqing (2016), the 5th UK−China Steel Research Forum, in conjunction with the 16th Conference of Chinese Materials Association in the UK on Materials Science and Engineering, was held at the University of Birmingham, UK on 4−7 July 2018 [...]

Due to their relatively low cost, large surface area and good chemical and physical properties, carbon nanofibers (CNFs) are attractive for the fabrication of electrodes for supercapacitors (SCs). However, their relatively low electrical conductivity has impeded their practical application. To this end, a novel active-screen plasma activation and deposition technology has been developed to deposit silver, platinum and palladium nanoparticles on activated CNFs surfaces to increase their specific surface area and electrical conductivity, thus improving the specific capacitance. The functionalised CNFs were fully characterised using scanning electron microscope (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffraction (XRD) and their electrochemical properties were evaluated using cyclic voltammetry and electrochemical impedance spectroscopy. The results showed a significant improvement in specific capacitance, as well as electrochemical impedance over the untreated CNFs. The functionalisation of CNFs via environmental-friendly active-screen plasma technology provides a promising future for cost-effective supercapacitors with high power and energy density.

A lean duplex stainless steel, LDX2404, was DC plasma nitrided under a range of treatment conditions. The microstructure characterisation evaluation of the treated samples revealed that a dense, super-hard surface layer can be produced by low-temperature (450 °C) plasma nitrided samples was found to be significantly worse than that of the untreated material.

Inspired by some typical plants such as lotus leaves, superhydrophobic surfaces are commonly prepared by a combination of low surface energy materials and hierarchical micro/nano structures. In this work, superhydrophobic surfaces on copper substrates were prepared by a rapid, facile one-step pulse electrodepositing process, with different duty ratios in an electrolyte containing lanthanum chloride (LaCl3·6H2O), myristic acid (CH3(CH2)12COOH), and ethanol. The equivalent electrolytic time was only 10 min. The surface morphology, chemical composition and superhydrophobic property of the pulse electrodeposited surfaces were fully investigated with SEM, EDX, XRD, contact angle meter and time-lapse photographs of water droplets bouncing method. The results show that the as-prepared surfaces have micro/nano dual scale structures mainly consisting of La[CH3(CH2)12COO]3 crystals. The maximum water contact angle (WCA) is about 160.9°, and the corresponding sliding angle is about 5°. This method is time-saving and can be easily extended to other conductive materials, having a great potential for future applications.