Microgel,nanogel and hydrogel–hydrogel semi-IPN composites for biomedical applications: synthesis and characterization

Quaternary ammonium salt hydrogels from a cationic monomer, (3-acrylamidopropyl)-trimethylammonium chloride (APTMACl), in a variety sizes such as bulk, micro- and nano- has been prepared. The synthesis of micro- and nanogels were carried out in the microenvironment of water-in-oil microemulsions using two types of surfactants, namely, L-α- phosphatidylcholine (lecithin) and dioctyl sulfosuccinate sodium salt (AOT). Additionally, hydrogel–hydrogel composite semi-interpenetrating polymer networks (semi-IPN) was synthesized by dispersing previously prepared micro/nanogel into neutral monomers such as acrylamide (AAm) or 2-hydroxylethyl methcarylate (HEMA) before network formation. Hydrogel swelling and pH response behaviors have been investigated for bulk gels. Morphology, structure, and size of nano-, micro- and bulk materials were explored utilizing transmission electron microcopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM). It was confirmed with gel electrophoresis that completely charged nanogel form a strong complex with DNA.     

Structural characterization of protein–polymer conjugates for biomedical applications with small-angle scattering

Protein–polymer conjugates, typically consisting of one or more polymers covalently attached to a protein, are an increasingly common component in biotechnology. Polymers can increase circulation time, alter immune responses, and influence the self-assembly of proteins to which they are attached. To understand and take full advantage of the benefits that protein–polymer conjugates provide, there is a strong need for structural characterization of both the conjugates and their self-assembled structures. Although X-ray crystallography is suitable for determining protein structure, protein–polymer conjugates do not generally crystallize, requiring the use of alternative techniques. Small-angle scattering, with neutrons in particular, is one such technique. In this article, we review recent work in the area of protein–polymer conjugates and highlight the important role that structure plays. We then highlight shape-dependent and shape-independent approaches for structural characterization of protein–polymer conjugates and future directions in small-angle scattering interpretation. We conclude by introducing a new model that we suggest may be useful in the future to acquire more detailed structural properties.     

Sol–gel synthesis and characterisation of nanoporous zirconium titanate coated on 316L SS for biomedical applications

In this study, the nanoporous zirconium titanate was prepared using sol–gel process and coated over 316L SS implants via dip-coating technique. XRD patterns of zirconium titanate are crystalline and orthorhombic in structure. FT-IR spectra showed a broad band between 3,500 and 3,300 cm⁻¹, which was assigned to fundamental stretching vibrations of hydroxyl groups. The set of overlapping peaks in the range of 810–520 cm⁻¹ are related to Zr–O and Zr–O–Ti groups. SEM-EDAX and TEM showed the surface morphology of coated zirconium titanate to be porous and uniform. Excellent adhesion of the coating to the substrate has been achieved. The contact angle value was found to be 12°. The coating acts as a barrier layer to the metallic implants and induces the formation of hydroxyapatite layer on the metal surfaces. These results revealed that the nano zirconium titanate coated 316L SS exhibit higher bioactivity compared to that of uncoated 316L SS.     

Electrochemical preparation and characterization of magnetic core–shell nanowires for biomedical applications

Magnetic CoNi@Au core–shell nanorods have been electrochemically synthesized, characterized and functionalized to test their inherent cytotoxicity in order to assess their potential use for biomedical applications. The initially electrodeposited CoNi nanorods have been covered with a gold layer by means of galvanic displacement to minimize the nanowires toxicity and their aggregation, and favour the functionalization. The presence of a gold layer on the nanorod surface slightly modifies the magnetic behaviour of the as-deposited nanorods, maintaining their soft-magnetic behaviour and high magnetization of saturation. The complete covering of the nanorods with the gold shell favours a good functionalization with a layer of (11-Mercaptoundecyl)hexa(ethylene glycol) molecules, in order to create a hydrophilic coating to avoid the aggregation of nanorods, keeping them in suspension and give them stability in biological media. The presence of the organic layer incorporated was detected by means of electrochemical probe experiments. A cytotoxicity test of functionalized core–shell nanorods, carried out with adherent HeLa cells, showed that cell viability was higher than 80% for amounts of nanorods up to 10 μg mL^− 1. These results make functionalized nanorods promising vehicles for targeted drug delivery in medicine, which gives a complementary property to the magnetic nanoparticles.     

Anodizing parameters optimization of Ti–6Al–4V titanium alloy using response surface methodology

The present paper depicts application of response surface methodology (RSM) for optimizing the anodizing parameters of Ti–6Al–4V (TA6V) titanium alloy. Three operating parameters, i.e., voltage (V), temperature (T) and time (t), are designed as factors by using RSM design. Reliable regression models were established between the input parameters and the given responses, namely oxide thickness (e), Vickers hardness (Hv) and polarization resistance (R_p) with regression coefficients multiples of 0.940, 0.925, 0.865, respectively, indicating good agreement between the experimental values and those predicted using the quadratic model.The predicted values of V (42.67 V), t (45.9 min) and T (29.5 °C) are the optimal anodization combination leading to a TiO₂ layer with the best compromise between the oxide thickness (28.7 μm), Vickers hardness (321.90) and bias resistance (6.37 MΩ cm²). It was observed that the hardness characteristic is more affected by anodizing time and temperature, and less sensitive to voltage and parameter interactions. Polarization resistance is strongly influenced by voltage, modestly influenced by anodizing time and temperature, and less sensitive to parameter interactions. Moreover, higher anodizing parameters lead to higher thickness. Therefore, RMS could be a suitable method to optimize anodizing parameters of titanium alloys.     

One-pot synthesis of porous nickel–manganese sulfides with tuneable compositions for high-performance energy storage

Mixed-metal compounds, especially for the sulfides, have been investigated as a very attractive type of electroactive materials for supercapacitors. In this work, we demonstrate nickel?manganese (Ni?Mn) sulfides are very attractive for supercapacitors with promising electrochemical performance. The Ni?Mn sulfides with different Ni to Mn ratios have been synthesized via a facile one-pot hydrothermal method, which show a similar structure of interconnected particles and are very porous in microstructure. And then, the Ni?Mn sulfides are investigated by three-electrode measurements and demonstrate strong synergy between Ni and Mn. The Ni?Mn sulfide with a Ni to Mn ratio of 2:1 demonstrates superior performance of 1068?F?g^?1 at 1?A?g^?1. Lastly, The Ni?Mn sulfide with a Ni to Mn ratio of 2:1 are used as positive electrode for two-electrode test, and the asymmetric supercapacitor shows both high energy and power densities combined with excellent cycling stability. Our work demonstrates that the Ni?Mn sulfides are also very electrochemical active for supercapacitors and their performance can be tuned by changing the Ni to Mn ratio.

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Effect of morphology and precipitation of Si phase on thermal properties of Al–Si–Mg–Cu foundry alloy

Journal of Thermal Analysis and Calorimetry - In this study, CuAl13?xTax (% mass x?=?1; 1.5; 2; 2.5) shape-memory alloys were produced through arc-melting method. Phase...     

Corrosion behaviour of an Mg–Y–RE alloy used in biomedical applications studied by electrochemical techniques

Magnesium, due to its biocompatibility, a necessity in metabolic processes, and better mechanical properties than polymer, is an ideal candidate for biodegradable implants. The main actual limitation for the use of magnesium alloys is its too fast degradation rate in the physiological environment. The corrosion behaviour of an Mg–Y–RE magnesium alloy in two different physiological solutions (artificial plasma (AP) and simulated body fluid (SBF)) was investigated, using electrochemical impedance spectroscopy (EIS).The investigation showed that SBF is significantly more aggressive than AP with regard to the polished surface. A large difference in the corrosion rate and mechanisms (uniform or localized corrosion) is observed as a function of the buffer capacity of the media, but also of the carbonate and chloride content. For temporary surface protection, the formation of an approximately 350–400 nm dense hydroxide layer is obtained by electrochemical anodising. An increase of the corrosion resistance of the treated alloy for both physiological solutions is obtained, and this is especially noticeable for a long immersion time in AP.     

Electrodeposition and electrochemical properties of novel ternary tin–cobalt–phosphorus alloy electrodes for lithium-ion batteries

Porous Sn–Co–P alloy with reticular structure were prepared by electroplating using copper foam as current collector. The structure and electrochemical performance of the electroplated porous Sn–Co–P alloy electrodes were investigated in detail. Experimental results illustrated that the porous Sn–Co–P alloy consists of mainly SnP_0.94 phase with a minor quantity of Sn and Co₃Sn₂. Galvanostatic charge–discharge tests of porous Sn–Co–P alloy electrodes confirmed its excellent performances: at 50th charge–discharge cycle, the discharge specific capacity is 503 mAh g^?1 and the columbic efficiency is as high as 99%. It has revealed that the porous and multi-phase composite structure of the alloy can restrain the pulverization of electrode in charge/discharge cycles, and accommodate partly the volume expansion and phase transition, resulting in good cycleability of the electrode.     

Construction of hierarchical porous graphene–carbon nanotubes hybrid with high surface area for high performance supercapacitor applications

Journal of Solid State Electrochemistry - Unlike activated carbon, graphene sheets are lack of ion pathways on their basal planes and prone to agglomerate or restack unfortunately for their strong...     

Sol–gel synthesis of porous titania fibers by electro-spinning for water purification

In this study, porous ceramic fibers were prepared by the sol–gel-assisted electro-spinning process using colloidal dispersion of complex fluids for the application of phtotocatalysts. First, polystyrene nanospheres were synthesized by dispersion polymerization as sacrificial templates for porous fibers. Then, the mixture of polyvinylpyrrolidone and the ceramic precursor with the polymeric nanospheres was prepared as the spinning solution and self-organized by electro-spinning, followed by calcination of the electrospun composite fibers. The morphologies of the porous fibers could be controlled according to the size of the templates and the amount of the ceramic precursor. The nano-structure of the pores in the fibrous materials could also be adjusted as open or closed cavities with various potential applications. As a demonstrative application, the macroporous titania fibers could be utilized as photocatalysts for the removal of organic dyes dissolved in water. A better photocatalytic activity of the macroporous fibers with 700-nm pore diameter was observed compared to the result of nonporous titania fibers due to the increased porosity. Collectively, the macroporous ceramic fibers were found to be efficient functional materials to prepare the unique nano-structured materials other than simple nonporous fibers.     

Synthesis and properties of Co–Pt alloy silica core-shell particles

This paper describes a method for fabrication of silica-coated Co–Pt alloy nanoparticles in a liquid phase process. The Co–Pt nanoparticles were prepared from CoCl₂ (4.2 × 10⁻⁵ M), H₂PtCl₆ (1.8 × 10⁻⁵ M), citric acid (4 × 10⁻⁴ M) and NaBH₄ (1.2 × 10⁻² M) with a Co:Pt mole ratio of 7:3. The silica coating was performed in water/ethanol solution with a silane coupling agent, 3-aminopropyltrimethoxysilane (8 × 10⁻⁵ M), and a silica source, tetraethoxyorthosilicate (7.2 × 10⁻⁴ M) in the presence of the Co–Pt nanoparticles. Observations with a transmittance electron microscope and a scanning transmission electron microscope revealed that the Co-rich and Pt-rich nanoparticles were coated with silica. According to X-ray diffraction measurements, core particles were crystallized to metallic Co crystallites and fcc Co–Pt alloy crystallites with annealing in air at 300–500 °C. Magnetic properties of the silica-coated particles were strongly dependent on annealing temperature. Maximum values of 11.4 emu/g-sample for saturation magnetization and 365 Oe for coercive field were obtained for the particles annealed at 300 and 500 °C, respectively. Annealing at a temperature as high as 700 °C destroyed the coating structures because of crystallization of silica shell, resulting in reduction in saturation magnetization and coercive field.     

Crystallographic dependency of waste cow bone,hydroxyapatite, and β-tricalcium phosphate for biomedical application

In this research, waste cow bone was chosen as a sustainable source of biomaterials in pure hydroxyapatite form and synthesized hydroxyapatite (HAP) was prepared as a biphasic HAP (hydroxyapatite and β-tricalcium phosphate phase) and subsequently pure β-tricalcium phosphate (β-TCP). The samples were characterized by employing X-Ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) instrumentation, and in-depth crystallographic analysis was performed by calculating crystallite size, lattice parameters, HAp percentage, the volume fraction of β-TCP, β-TCP percentage, crystallinity index, degree of crystallinity, microstrain, and dislocation density. Excellent results was noticed for biocompatible properties such as cytotoxicity, hemolysis, and antimicrobial (E. coli, S. aureus, and A. niger). A relationship was established among the synthesized products and the crystallographic parameters.     

Evaluation of mechanical properties and characterization of silicon carbide–reinforced polyamide 6 polymer composites and their engineering applications

In this article, the tensile strength, impact, and hardness properties of silicon carbide (SiC) reinforced with polyamide 6 (PA6) are described for the first time. The composites were fabricated by an injection molding method using the SiC with varying weight percentages. The tensile and hardness of SiC/PA6 composites showed a regular trend of increasing tensile strength, impact, and hardness properties with varying weight percentages until 10 wt% and impact strength of SiC/PA6 composites increased up to 5 wt% afterwards decreasing the mechanical properties of the composite with greater weight percentages. Scanning electron microscope (SEM) studies were carried out to evaluate the SiC/PA6 interactions. The results related to SiC/PA6 composites were compared with those obtained for pure PA6.     

Electrochemical synthesis and properties of iron–titanium dioxide composite coatings

Deposition of Fe/TiO₂ composite coatings from a colloidal methanesulfonate electrolyte containing titanium dioxide hydrosol was studied. The TiO₂ content in the composite increases with increasing the dispersed phase content and decreasing the current density. Incorporation of TiO₂ particles into the iron matrix resilts in an increase in the microhardness of the deposit. The electroplated Fe/TiO₂ composite coating was used as a heterogeneous photocatalyst for the decomposition of an organic dye under the action of UV radiation.     

Fabrication and electrochemical properties of the Sn–Ni–P alloy rods array electrode for lithium-ion batteries

A new ternary Sn–Ni–P alloy rods array electrode for lithium-ion batteries is synthesized by electrodeposition with a Cu nanorods array structured foil as current collector. The Cu nanorods array foil is fabricated by heat treatment and electrochemical reduction of Cu(OH)₂ nanorods film, which is grown directly on Cu substrate through an oxidation method. The Sn–Ni–P alloy rods array electrode is mainly composed of pure Sn, Ni₃Sn₄ and Ni–P phases. The electrochemical experimental results illustrate that the Sn–Ni–P alloy rods array electrode has high reversible capacity and excellent coulombic efficiency, with an initial discharge capacity and charge capacity of 785.0 mAh g^?1 and 567.8 mAh g^?1, respectively. After the 100th discharge–charge cycling, capacity retention is 94.2% with a value of 534.8 mAh g^?1. The electrode also performs with an excellent rate capacity.     

Sol–gel synthesis of IPTES and D10H consisting fluorinated silane system for hydrophobic applications

In this study, new fluorinated silane system was prepared by adding hydroxyl terminated Fluorolink D10H oligomer to 3-isocyanatopropyltrietoxysilane. The obtained silane system was independently composed with 3-Glycidyloxypropyltrimethoxysilane and 3-Glycidyloxy-propyltriethoxysilane. Then the prepared two different coating solutions were applied to glass surface by spin-coating method. The chemical bonding between groups in system was investigated by FTIR analysis. The elemental composition of coatings was determined by using EDX analysis. Their structure and surface properties were analyzed by scanning electron microscopy, atomic force microscopy, contact angle measurement and UV–vis spectrophotometer. The amounts of fluorine on the coatings prepared with IPTES-D10H-GLYEO and IPTES-D10H-GLYMO were 33 and 34 %wt, respectively. Transparent coatings with smooth surface and uniform thickness were obtained. The coatings had nanoscale roughness. The contact angles of coatings for water were range from 103° to 110°, and for n-hexadecane were range from 59° to 62°.     

Study on cytotoxicity and photocatalytic properties of different titania/hydroxyapatite nanocomposites prepared with a combination of sol–gel and precipitation methods

Research on Chemical Intermediates - In the present study different titania/hydroxyapatite nanocomposites were successfully synthesized via a combination of sol–gel and precipitation methods....     

Development of ion chromatography and capillary electrophoresis methods for the determination of Li in Li–Al alloy

Two methods were developed for determination Li content in Li–Al alloy by employing ion chromatography (IC) and capillary electrophoresis (CE) without any prior separation of Al matrix. In absence of suitable certified reference material the two methods were used to validate each other. Using a high capacity column and a weaker eluent methane sulphonic acid, it was possible to separate Li in IC without eluting strongly retained Al. The method showed good precision and sensitivity and was extended for analysis of routine samples. In the case of CE using imidazole as co-ion, Li was detected in CE by indirect detection. In view of no interference from Al, samples were analyzed without any matrix separation. The CE method was used successfully for sample analysis and results were compared with IC results.