Electrosprayed Chitosan–Copper Complex Microspheres with Uniform Size

Chitosan-based nano- and microspheres have shown great potential in a broad range of applications, including drug delivery, bone tissue engineering, wastewater treatments, etc. The preparation of uniformly sized spheres with controlled morphology and microstructure is still a challenge. This work investigates the influence of cupric ions (Cu²⁺) on the size, shape, morphology and stability of electrosprayed chitosan–copper (CHT–Cu²⁺) complex microspheres, using chitosans with different degrees of deacetylation. The dynamic viscosity of CHT–Cu²⁺ solutions was measured by Höppler viscometer, while attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) was used for the identification of dried microspheres. The size, shape and morphology of microspheres were analyzed by light microscope and scanning electron microscopy (SEM), while stability of dried microspheres was evaluated in different buffer solutions. The volume ratio of wet and dry microspheres was assessed based on the estimated diameter of microspheres. The higher concentration of Cu²⁺ ions resulted in a decrease in viscosity of CHT–Cu²⁺ solutions and volume ratio of prepared microspheres. Changes in the intensities and wave numbers of absorption bands of amino and hydroxyl groups, amide I and amide II suggested that the nitrogen and oxygen atoms in chitosan are coordinating the cupric ions. Micrographs obtained by light microscope and SEM showed that all prepared samples are spherical. The increase of cupric ions concentration changed the topography of microspheres and decreased their size. These results indicated the successful electrospraying of CHT–Cu²⁺ microspheres with uniform size and good stability in aqueous medium.     

Understanding Electrodeposition of Chitosan–Hydroxyapatite Structures for Regeneration of Tubular-Shaped Tissues and Organs

Tubular-shaped hydrogel structures were obtained in the process of cathodic electrodeposition from a chitosan–hydroxyapatite solution carried out in a cylindrical geometry. The impact of the initial concentration of solution components (i.e., chitosan, hydroxyapatite, and lactic acid) and process parameters (i.e., time and voltage) on the mass and structural properties of deposit was examined. Commercially available chitosan differs in average molecular weight and deacetylation degree; therefore, these parameters were also studied. The application of Fourier-transform infrared spectroscopy, scanning electron microscopy, and time-of-flight secondary ion mass spectrometry allowed obtaining fundamental information about the type of bonds and interactions created in electrodeposited structures. Biocompatible tubular implants are highly desired in the field of regeneration or replacement of tubular-shaped tissues and organs; therefore, the possibility of obtaining deposits with the desired structural properties is highly anticipated.     

Copper Surface Treatment Method with Antibacterial Performance Using “Super-Spread Wetting” Properties

In this work, a copper coating is developed on a carbon steel substrate by exploiting the superwetting properties of liquid copper. We characterize the surface morphology, chemical composition, roughness, wettability, ability to release a copper ion from surfaces, and antibacterial efficacy (against Escherichia coli and Staphylococcus aureus). The coating shows a dense microstructure and good adhesion, with thicknesses of approximately 20–40 µm. X-ray diffraction (XRD) analysis reveals that the coated surface structure is composed of Cu, Cu₂O, and CuO. The surface roughness and contact angle measurements suggest that the copper coating is rougher and more hydrophobic than the substrate. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) measurements reveal a dissolution of copper ions in chloride-containing environments. The antibacterial test shows that the copper coating achieves a 99.99% reduction of E. coli and S. aureus. This study suggests that the characteristics of the copper-coated surface, including the chemical composition, high surface roughness, good wettability, and ability for copper ion release, may result in surfaces with antibacterial properties.     

Assessment of AlN/Mg–8Al Composites Reinforced with In Situ and/or Ex Situ AlN Particles

In this paper, 8.2AlN/Mg–8Al composites reinforced with in situ and/or ex situ AlN particles have been synthesized. The in situ-formed AlN particles are nano-sized, performing as particle chains. It has been clarified that the in situ AlN particles are more efficient than ex situ particles for the enhancement of mechanical properties. The in situ-prepared composite exhibits improved density, hardness and compressive strength compared to the ex situ ones. This work may be referred to for designing particle-reinforced Mg composites by various methods.     

In Situ Tungsten Carbide Formation in Nanostructured Copper Matrix Composite Using Mechanical Alloying and Sintering

In this study, an in situ nanostructured copper tungsten carbide composite was synthesized by mechanical alloying (MA) and the powder metallurgy route. The microstructure and phase changes of the composite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. Tungsten carbide phases (WC and W₂C) were only present after MA and combination of sintering. Higher energy associated with a longer milling time was beneficial for the formation of WC. Formation of W₂C and WC resulted from internal refinement due to heavy plastic deformation in the composite. The solubility of the phases in the as-milled and sintered composite was described by the changes of the lattice parameter of Cu. Chemical analysis of the surface of a composite of W 4f and C 1s revealed that the increased defects introduced by MA affect the atomic binding of the W-C interaction.     

The In Situ Hydrothermal and Microwave Syntheses of Zinc Oxides for Functional Cement Composites

This study presents the results of research on cement mortars amended with two zinc oxides obtained by two different methods: hydrothermal ZnO-H and microwave ZnO-M. Our work indicates that, in contrast to spherical ZnO-H, ZnO-M was characterized by a columnar particle habit with a BET surface area of 8 m²/g, which was four times higher than that obtained for hydrothermally obtained zinc oxide. In addition, ZnO-M induced much better antimicrobial resistance, which was also reported in cement mortar with this oxide. Both zinc oxides showed very good photocatalytic properties, as demonstrated by the 4-chlorophenol degradation test. The reaction efficiency was high, reaching the level of 90%. However, zinc oxides significantly delayed the cement binder setting: ZnO-H by 430 min and ZnO-M by 380 min. This in turn affected the increments in compressive strength of the produced mortars. No significant change in compressive strength was observed on the first day of setting, while significant changes in the strengths of mortars with both zinc oxides were observed later after 7 and 28 days of hardening. As of these times, the compressive strengths were about 13–15.5% and 12–13% higher than the corresponding values for the reference mortar, respectively, for ZnO-H and ZnO-M. There were no significant changes in plasticity and flexural strength of mortars amended with both zinc oxides.     

In Situ Synthesis of a Double-Layer Chitosan Coating on Cotton Fabric to Improve the Color Fastness of Sodium Copper Chlorophyllin

Natural dye’s poor affinity for cotton and poor fastness properties still hinder its applications in the textile industry. In this study, a doubled-layered chitosan coating was cured on cotton fabric to serve as bio-mordant and form a protective layer on it. Under the optimal treatment conditions, the maximum q_e (adsorption amount) of the natural dye sodium copper chlorophyllin (SCC) calculated from the Langmuir isothermal model was raised from 4.5 g/kg to 19.8 g/kg. The dye uptake of the treated fabric was improved from 22.7% to 96.4% at 1% o.w.f. dye concentration. By a second chitosan layer cured on the dyed fabric via the cross-linking method, the wash fastness of the cotton fabric dyed with SCC can be improved from 3 to 5 (ISO 105 C-06). The natural source of the biopolymer material, chitosan, and its ability to biodegrade at end of life met with the initial objective of green manufacturing in applying natural dyes and natural materials to the textile industry.     

Copper Chalcogenide–Copper Tetrahedrite Composites—A New Concept for Stable Thermoelectric Materials Based on the Chalcogenide System

For the first time, an alternative way of improving the stability of Cu-based thermoelectric materials is proposed, with the investigation of two different copper chalcogenide–copper tetrahedrite composites, rich in sulfur and selenium anions, respectively. Based on the preliminary DFT results, which indicate the instability of Sb-doped copper chalcogenide, the Cu_1.97S–Cu₁₂Sb₄S₁₃ and Cu_2−xSe–Cu₃SbSe₃ composites are obtained using melt-solidification techniques, with the tetrahedrite phase concentration varying from 1 to 10 wt.%. Room temperature structural analysis (XRD, SEM) indicates the two-phase structure of the materials, with ternary phase precipitates embed within the copper chalcogenide matrix. The proposed solution allows for successful blocking of excessive Cu migration, with stable electrical conductivity and Seebeck coefficient values over subsequent thermal cycles. The materials exhibit a p-type, semimetallic character with high stability, represented by a near-constant power factor (PF)—temperature dependences between individual cycles. Finally, the thermoelectric figure-of-merit ZT parameter reaches about 0.26 (623 K) for the Cu_1.97S–Cu₁₂Sb₄S₁₃ system, in which case increasing content of tetrahedrite is a beneficial effect, and about 0.44 (623 K) for the Cu_2−xSe–Cu₃SbSe₃ system, where increasing the content of Cu₃SbSe₃ negatively influences the thermoelectric performance.     

Electrodeposition and Corrosion Properties of Nickel–Graphene Oxide Composite Coatings

Nickel-based composite electrochemical coatings (CEC) modified with multilayer graphene oxide (GO) were obtained from a sulfate-chloride electrolyte in the reverse electrolysis mode. The microstructure of these CECs was investigated by X-ray phase analysis and scanning electron microscopy. The corrosion-electrochemical behavior of nickel–GO composite coatings in a 0.5 M solution of H₂SO₄was studied. Tests in a 3.5% NaCl solution showed that the inclusion of GO particles into the composition of electrolytic nickel deposits makes their corrosion rate 1.40–1.50 times less.     

Fabrication of Copper Matrix Composites Reinforced with Carbon Nanotubes Using an Innovational Self-Reduction Molecular-Level-Mixing Method

An innovational self-reduction molecular-level-mixing method was proposed as a simplified manufacturing technique for the production of carbon nanotube copper matrix composites (CNT/Cu). Copper matrix composites reinforced with varying amounts of (0.1, 0.3, 0.5 and 0.7 wt%) carbon nanotubes were fabricated by using this method combined with hot-pressing sintering technology. The surface structure and elemental distribution during the preparation of CNT/Cu mixing powder were investigated. The microstructure and comprehensive properties of the CNT/Cu composites were examined by metallography, mechanical and electrical conductivity tests. The results revealed that the CNT/Cu could be produced by a high temperature reaction at 900 degrees under vacuum, during which the carbon atoms in the carbon nanotubes reduced the divalent copper on the surface to zero-valent copper monomers. The decrease in the ratio of D and G peaks on the Raman spectra indicated that the defective spots on the carbon nanotubes were wrapped and covered by the copper atoms after a self-reduction reaction. The prepared CNT/Cu powders were uniformly embedded in the grain boundaries of the copper matrix materials and effectively hindered the tensile fracture. The overall characteristics of the CNT/Cu composites steadily increased with increasing CNT until the maximum at 0.7 wt%. The performance was achieved with a hardness of 86.1 HV, an electrical conductivity of 81.8% IACS, and tensile strength of 227.5 MPa.     

Smart Graphite–Cement Composites with Low Percolation Threshold

The objective of this work was to obtain cement composites with low percolation thresholds, which would reduce the cost of graphite and maintain good mechanical properties. For this purpose, exfoliated graphite was used as a conductive additive, which was obtained by exfoliating the expanded graphite via ultrasonic irradiation in a water bath with surfactant. To obtain evenly distributed graphite particles, the exfoliated graphite was incorporated with the remaining surfactant into the matrix. This study is limited to investigating the influence of exfoliated graphite on the electrical and mechanical properties of cement mortars. The electrical conductivity of the composites was investigated to determine the percolation threshold. The flexural and compressive strength was tested to assess the mechanical properties. In terms of the practical applications of these composites, the piezoresistive, temperature–resistivity, and thermoelectric properties were studied. The results showed that the incorporation of exfoliated graphite with surfactant is an effective way to obtain a composite with a percolation threshold as low as 0.96% (total volume of the composite). In addition, the mechanical properties of the composites are satisfactory for practical application. These composites also have good properties in terms of practical applications. As a result, the exfoliated graphite used can significantly facilitate the practical use of smart composites.     

Electrical Properties of In Situ Synthesized Ag-Graphene/Ni Composites

Ag/Ni composite contact materials are widely used in low-voltage switches, appliances, instruments, and high-precision contacts due to their good electrical conductivity and processing properties. The addition of small amounts of additives can effectively improve the overall performance of Ag/Ni contact materials. Graphene has good applications in semiconductors, thermal materials, and metal matrix materials due to its good electrical and thermal conductivity and mechanical properties. In this paper, Ag-graphene composites with different added graphene contents were prepared by in situ synthesis of graphene oxide (GO) and AgNO₃ by reduction at room temperature using ascorbic acid as a reducing agent. The Ag-graphene composites and nickel powder were ball-milled and mixed in a mass ratio of 85:15. The Ag-graphene/Ni was tested as an electrical contact material after the pressing, initial firing, repressing, and refiring processes. Its fusion welding force and arc energy were measured. The results show a 12% improvement in electrical conductivity with a graphene doping content of approximately 0.3 wt% compared to undoped contacts, resulting in 33.8 IACS%. The average contact fusion welding force was 49.49 cN, with an average reduction in the fusion welding force of approximately 8.04%. The average arc ignition energy was approximately 176.77 mJ, with an average decrease of 13.06%. The trace addition of graphene can improve the overall performance of Ag/Ni contacts and can promote the application of graphene in electrical contact materials.     

Electrodeposition of Copper and Brass Coatings with Olive-Like Structure

One method of creating a brass coating is through electrodeposition, which is most often completed in cyanide galvanic baths. Due to their toxicity, many investigations focused on the development of more environmentally friendly alternatives. The purpose of the study was to explore a new generation of non-aqueous cyanide-free baths based on 1-ethyl-3-methylimidazolium acetate ionic liquids. The study involved the formation of copper, zinc, and brass coatings. The influence of the bath composition, cathodic current density, and temperature was determined. The obtained coatings were characterized in terms of their morphology, chemical composition, phase composition, roughness, and corrosion resistance. It was found that the structure of the obtained coatings is strongly dependent on the process parameters. The three main structure types observed were as follows: fine-grained, porous, and olive-like. To the best knowledge of the authors, it is the first time the olive-like structure was observed in the case of an electrodeposited coating. The Cu-Zn coatings consisted of 19–96 at. % copper and exhibited relatively good corrosion resistance. A significant improvement of corrosion properties was found in the case of copper and brass coatings with the olive-like structure.     

Process–Structure–Property Relationships of Copper Parts Manufactured by Laser Powder Bed Fusion

The process–structure–property relationships of copper laser powder bed fusion (L-PBF)-produced parts made of high purity copper powder (99.9 wt %) are examined in this work. A nominal laser beam diameter of 100 μm with a continuous wavelength of 1080 nm was employed. A wide range of process parameters was considered in this study, including five levels of laser power in the range of 200 to 370 W, nine levels of scanning speed from 200 to 700 mm/s, six levels of hatch spacing from 50 to 150 μm, and two layer thickness values of 30 μm and 40 μm. The influence of preheating was also investigated. A maximum relative density of 96% was obtained at a laser power of 370 W, scanning speed of 500 mm/s, and hatch spacing of 100 μm. The results illustrated the significant influence of some parameters such as laser power and hatch spacing on the part quality. In addition, surface integrity was evaluated by surface roughness measurements, where the optimum Ra was measured at 8 μm ± 0.5 μm. X-ray photoelectron spectroscopy (XPS) and energy-dispersive X-ray spectroscopy (EDX) were performed on the as-built samples to assess the impact of impurities on the L-PBF part characteristics. The highest electrical conductivity recorded for the optimum density-low contaminated coils was 81% IACS.     

Effect of Nanoparticle Size on the Mechanical Strength of Ni–Graphene Composites

The effect of the size of nickel nanoparticles on the fabrication of a Ni–graphene composite by hydrostatic pressure at 0 K followed by annealing at 1000 and 2000 K is studied by molecular dynamics simulation. Crumpled graphene, consisting of crumpled graphene flakes interconnected by van der Waals forces is chosen as the matrix for the composite and filled with nickel nanoparticles composed of 21 and 47 atoms. It is found that the main factors that affect composite fabrication are nanoparticle size, the orientation of the structural units, and temperature of the fabrication process. The best stress–strain behavior is achieved for the Ni/graphene composite with Ni47 nanoparticle after annealing at 2000 K. However, all of the composites obtained had strength property anisotropy due to the inhomogeneous distribution of pores in the material volume.     

Fabrication and Characterization of Degradable Crop-Straw-Fiber Composite Film Using In Situ Polymerization with Melamine–Urea–Formaldehyde Prepolymer for Agricultural Film Mulching

Soil mulch composite films composed of biodegradable materials are being increasingly used in agriculture. In this study, mulch films based on wheat straw fiber and an environmentally friendly modifier were prepared via in situ polymerization and tested as the ridge mulch for crops. The mechanical properties of the straw fiber film were significantly enhanced by the modification. In particular, the films exhibited a noticeable increase in dry and wet tensile strength from 2.35 to 4.15 and 0.41 to 1.51 kN/m, respectively, with increasing filler content from 0% to 25%. The contact angle of the straw also showed an improvement based on its hydrophilicity. The crystallinity of the modified film was higher than that of the unmodified film and increased with modifier content. The changes in chemical interaction of the straw fiber film were determined by Fourier transform infrared spectroscopy, and the thermal stability of the unmodified film was improved by in situ polymerization. Scanning electron microscopy images indicated that the modifier was uniformly dispersed in the fiber film, resulting in an improvement in its mechanical properties. The modified straw fiber films could be degraded after mulching for approximately 50 days. Overall, the superior properties of the modified straw fiber film lend it great potential for agricultural application.     

In Situ Electrodeposition of Pb and Ag Applied on Fluorine Doped Tin Oxide Substrates: Comparative Experimental and Theoretical Study

A comparison between lead and silver electrodeposition onto fluorine-doped tin oxide (FTO) electrodes from nitrate solution was investigated in this work. Chronoamperometry has been used as an in situ technique to track the dynamics of the electrodeposition during advanced nucleation phases. The experimental results are correlated with a theoretical evaluation. It has shown that they have a strong correlation with each other. After that, the obtained deposits are characterized and compared as well by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), scanning electron microscopy (SEM), and impedance spectroscopy. The data reflects the effect of the material under investigation on current density, deposition density, and dielectric properties. Additionally, the electrodeposition approach (a two-in-one technique) can be followed in order to make well-controlled thin films that can be used for various purposes in addition to recovering heavy metals from wastewater.     

One-Step In Situ Patternable Reduction of a Ag–rGO Hybrid Using Temporally Shaped Femtosecond Pulses

In recent years, metallic nanoparticle (NP)–two-dimensional material hybrids have been widely used for photocatalysis and photoreduction. Here, we introduce a femtosecond laser reduction approach that relies on the repetitive ablation of recast layers by usi–ng temporally shaped pulses to achieve the fast fabrication of metallic NP–two-dimensional material hybrids. We selectively deposited silver-reduced graphene oxide (Ag–rGO) hybrids on different substrates under various fabrication conditions. The deposition of the hybrids was attributed to the redistribution of the cooling ejected plume after multiple radiation pulses and the exchange of carriers with ejected plume ions containing activated species such as small carbon clusters and H₂O. The proposed one-step in situ fabrication method is a competitive fabrication process that eliminates the additive separation process and exhibits morphological controllability. The Ag–rGO hybrids demonstrate considerable potential for chemomolecular and biomolecular detection because the surface-enhanced Raman scattering signal of the enhancement factor reached 4.04 × 10⁸.     

Microstructure and Mechanical Properties of TiN–TiB2–hBN Composites Fabricated by Reactive Hot Pressing Using TiN–B Mixture

In this study, TiN–TiB₂–hBN composite ceramics were prepared via reactive hot pressing using TiN and amorphous B powders as raw materials. Different sintering temperatures and composition ratios were studied. The results show that the 70 vol% TiN–17.6 vol% TiB₂–12.4 vol% hBN ceramic composites obtained ideal comprehensive properties at 1600 °C. The relative density, Vickers hardness, bending strength, and fracture toughness were 99%, 11 GPa, 521 MPa, and 4.22 MPa·m^1/2, respectively. Densification was promoted by the highly active reaction product TiB₂, and the structural defects formed in the grains. Meanwhile, the good interfacial bonding between TiN and TiB₂ grains and the uniform dispersion of ultrafine hBN in the matrix contributed to the excellent bending strength. Moreover, the toughening mechanism of crack deflection and grain pull-out improved the fracture toughness.     

Mechanical Characterization of Dental Prostheses Manufactured with PMMA–Graphene Composites

The use of a PMMA composite with graphene is being commercialized for application as dental prostheses. The different proportions of fibers provide a wide range of colors that favors dental esthetics in prostheses. However, there are no studies that have explained the influence that graphene has on the mechanical properties. In this contribution, we studied the PMMA and PMMA material with graphene fibers (PMMA-G) in the form of discs as supplied for machining. The presence of graphene fibers has been studied by Raman spectroscopy and the Shore hardness and Vickers micro hardness were determined. Mechanical compression tests were carried out to obtain the values of maximum strength and Young’s modulus (E) and by means of pin-on-disc wear tests, the specific wear rate and the friction coefficients were determined following the established international standards. Finally, the samples were characterized by field emission scanning electron microscopy (FESEM) to characterize the graphene’s morphology inside the PMMA. The results showed the presence of graphene in PMMA and was estimated in an amount of 0.1027% by weight in G-PMMA. The Shore hardness and Vickers microhardness values did not show statistically significant differences. Differences were observed in the compression maximum strength (129.43 MPa for PMMA and 140.23 for PMMA-G) and E values (2.01 for PMMA and 2.89 GPa for PMMA-G) as well as in the lower wear rate for the G-PMMA samples (1.93 × 10⁻⁷ for PMMA and 1.33 × 10⁻⁷ mm³/N·m) with a p < 0.005. The coefficients of friction for PMMA-G decreased from 0.4032 for PMMA to 0.4001 for PMMA-G. From the results obtained, a slight content in graphene produced a significant improvement in the mechanical properties that could be observed in the prosthesis material. Therefore, we can state that the main attraction of this material for dental prosthesis is its esthetics.