Surfactant-free electrochemical synthesis of fluoridated hydroxyapatite nanorods for biomedical applications

Fluoridated hydroxyapatite (FHA) [Ca₁₀(PO₄)₆F_x(OH)_2−x, x = 0–2] is believed to be a promising calcium phosphate (CaP) to replace pure hydroxyapatite (HA) for next-generation implants, owing to its better biocompatibility, higher antibacterial activity, and lower solubility. Notably, the shape and size of the CaP crystals play key roles in their performance and can influence their applications. One-dimensional (1D) FHA nanorods are important CaP materials which have been widely used in regenerative medicine applications such as restorative dentistry. Unfortunately, the traditional synthesis methods for FHA nanorods either employ surfactants or take a relatively long time. In this study, we aimed to propose a facile synthesis route to fabricate FHA nanorods without any surfactants using an electrochemical deposition method for the first time. This study focused on preparing FHA nanorods without the assistance of any surfactant, unlike the traditional synthesis methods, to avoid chemical impurities. FHA nanorods with lengths of 124–2606 nm, diameters of 28–211 nm, and aspect ratios of 4.4–21.8 were synthesized using the electrochemical method, followed by a heat treatment. For the as-synthesized FHA nanorods, the Ca/P ratio was 1.60 and the atomic concentration of F was 2.06 at.%. An ultrastructure examination revealed that each FHA nanorod possessed long-range order, good crystallinity, and a defect-free lattice with a certain crystallographic plane orientation along the whole rod. In short, we propose a novel, surfactant-free, cost-saving, and more efficient route to synthesize FHA nanorods which can be widely applied in multiple biomedical applications, including drug delivery, bone repair, and restorative dentistry.     

Improvement in the properties of low carbon MgO-C refractories through the addition of graphite-SiC micro-composite

Graphite–SiC micro-composites have been prepared in–house by carbothermal reduction process. Controlling the process parameters including the weight ratio of SiO₂ to graphite as well as carbothermal reduction temperature during the micro-composite preparation favors the homogeneous formation of SiC with preferred morphologies like ribbons and whiskers/fibers. The micro-composite modified low carbon MgO-C refractories have exhibited significantly improved bulk properties over the standard composition. To understand the beneficial role of SiC reinforcement on hot strength performance under air oxidizing conditions, we propose a scaling parameter known as strength factor (fs) based on the ratio of hot strength (HMOR) to cold strength (CCS). Correlating the strength factor data (fs) with oxidative damage provides new insights into the reinforcing effects of distinct SiC morphologies in this new class of micro-composite fortified refractory systems over the standard compositions.     

Numerical modeling of effect of slot on bubble motion in aluminum electrolytic process

A transient three-dimensional (3D) model was established to understand the bubble motion in an industrial electrolytic process. An anode with a new design was tested. It incorporates two slots that allow an efficient removal of gas bubbles. The electromagnetic fields were described by solving Maxwell's equations. The bubble movement was studied with two-way coupling Euler–Lagrange approach. The interplay of current density and bubble nucleation rate was included. The collision and coalescence of bubbles were considered. Random walk module was invoked for involving the chaotic effect of the turbulence. The numerical results were validated by experimental measurements. The results indicate that the current distribution and the bubble nucleation periodically change. Due to the slot, the bubble elimination heavily increases. The contribution of the slot to the bubble removal exceeds 50% in the case of three currents, and the promotion of the slot decays with increasing the current.     

1250°C liquidus for the CaO–MgO–SiO2–Al2O3–TiO2 system in air

Ti-bearing blast furnace slags have been regarded as an important secondary material in modern society, and the efficient recycling of Ti oxides from it is of key interest. For this reason, more thermodynamic data is needed regarding the phase relations in different composition ranges and sections. Therefore, the equilibrium phase relations of CaO–MgO–SiO₂–Al₂O₃–TiO₂ system in a low w(CaO)/w(SiO₂) ratio of 0.6–0.8 at 1250 °C in air and fixed concentrations of MgO and Al₂O₃, were investigated experimentally using a high temperature equilibration and quenching method followed by SEM-EDS (Scanning Electron Microscope and Energy Dispersive X-ray Spectrometer) analyses. The equilibrium solid phases of perovskite (CaO·TiO₂), a pseudo-brookite solid solution (MgO·2TiO₂, Al₂O₃·TiO₂)_ss, and anorthite (CaO·Al₂O₃·2SiO₂) were found to coexist with the liquid phase at 1250 °C. The calculated results of Factsage and MTDATA were used for comparisons, and significant discrepancies were found between predictions and the experimental results. The 1250 °C isotherm has been constructed and projected on the CaO–SiO₂–TiO₂-8 wt.% MgO-14 wt% Al₂O₃ quasi-ternary plane of the phase diagram. The obtained results provide new fundamental data for Ti-bearing slag recycling processes, and they add new experimental features for thermodynamic modeling of the high-order titanium oxide-containing systems.     

光伏废料制备Si3N4-SiC材料的抗氧化性和抗侵蚀性

将光伏废料经酸洗除杂后,与硅粉按85∶15的质量比配料,以聚乙二醇做结合剂,成型为10 mm×10 mm×20 mm的生坯后,在1380℃保温2 h氮化制成Si3N4-SiC材料,然后研究了该Si3N4-SiC材料的抗氧化性和抗侵蚀性。结果表明:1)制备的Si3N4-SiC材料在空气气氛中抗氧化性较好,主要是由于其氧化产物Si2N2O和SiO2填充气孔,促进烧结,提高了试样的致密度。2)在静态熔盐(Na3AlF6)中的抗侵蚀性能较好,主要是由于Na3AlF6渗入气孔中,使其显气孔率降低。3)在动态熔盐中的抗侵蚀性相对变差,主要是由于CO2气体的搅拌和对Si3N4、SiC的氧化二者共同作用的结果。     

Structural,electrochemical and catalytic activity of Prussian blue analogues embedded with functionalized carbon for solid state battery applications

The nanoparticles of Mn_1.5[Cr(CN)₆]∙mH₂O@Ni_1.5[Cr(CN)₆]∙nH₂O core-shell prussian blue analogues (PBA) embedded with carbon additives (PBA-C) were synthesized and characterized as electrode material for solid state battery application. The impedance spectroscopy and cyclic voltametry were used to study the electrochemical properties by adding functionalized carbon in 1:1 proportion to improve the electrical performance. The value of room temperature electrical conductivity of core-shell PBA and core-shell nanoparticles mixed with vulcan carbon (PBA-C) are found to be 1.574 × 10⁻³ and 1.92 × 10⁻³ Scm⁻¹_, respectively. Using Li₇La₃Zr₂O₁₂ (LZZO) electrolyte, single cell was fabricated with PBA-C material, and studied its charging-discharging cycles, which exhibits higher current density with stable performance for 400 cycles for time slots of 400 min. The study reveals that the PBA core-shell nanoparticles mixed with carbon (PBA-C) may be a potential candidate as an electrode material in the form of a single cell using LZZO electrolyte.     

Surface properties and surface patterning of UV-curable coating using perfluorosilane-treated nanosilica

In this work, a one-step film formation method is demonstrated to obtain the patterned surface of an acrylate photocuring coating using nano-silica particles treated with a perfluoroalkoxysilane ((heptadecafluoro-1,1,2,2-tetra hydrodecyl) triethoxysilane) as a nanoadditive. Nanosilica particles were treated with perfluoroalkoxysilane and used in a UV-curable matrix. The typical patterns on the surface of the UV-cured films are revealed in AFM images. The surface properties of the cured films were investigated by measuring water contact angle and surface energy. The degree of conversion of the samples was obtained by FTIR analysis and pendulum hardness was measured using a Konig hardness meter. Scratch resistance of cured films was measured by standard scratch measuring pens. The characteristics obtained from AFM analysis showed that rough surface patterns in this system are controlled linearly by changes in the treated nano-particle concentration. The subtraction of surface energy of the cured film was clear and the water contact angle showed a 60% increase with the addition of a fluorinated nano-particle concentration. Surface hardness decreased and scratch resistance increased as the concentration of treated nanoparticles increased, while the final degree of conversion of the film remained unchanged.     

Microstructure evolution during near-net-shape fabrication of NixAly-TiC cermets through binder jet additive manufacturing and pressureless melt infiltration

Titanium carbide-nickel aluminide (TiC-Ni_xAl_y) intermetallic matrix composite materials were fabricated with additive manufacturing and pressureless melt infiltration for applications intended for high-wear and corrosive environments while maintaining low density. Here, two compositions of nickel aluminide are infiltrated into porous, printed TiC preforms. Net shaping of a nickel-rich infiltrant is less compared to the net shaping of the aluminum-rich infiltrant due to dissolution of TiC in the molten infiltrant. The microstructures and porosity of the two infiltrants with TiC are examined after processing. The explanation of shape retention from infiltration is explained, and the excellent shape retention in an Al-rich infiltrant system is thought to be from peritectic behavior and a metered infiltration of different phases during cooling and solidification without significant dissolution. The metered infiltration contributed to some porosity, microcracking, and segregated Ni_xAl_y phases. This work demonstrates that TiC can be shaped and infiltrated with intermetallics to provide a method of making composites with limited shrinkage and controlled geometry.     

Densification and grain boundary nitrides in spark plasma sintered SAF 2205 -TiN composite

Densification and nature of α-ferrite γ-austenite interface associated with the spark plasma sintering (SPS) of SAF 2205 reinforced with TiN nanoparticles was investigated. The sintering data obtained during SPS was used to evaluate the densification mechanism. EBSD and TKD technique were used to characterize the SAF 2205 composite. The grain and grain boundary properties were evaluated using nanoindentation technique. Three densification stages relating to particles rearrangement, bulk deformation and rapid densification of the SAF 2205 composite was observed during SPS. The EBSD revealed a reverse ferrite to austenite phase transformation and a refined microstructure after SPS. TKD analysis of the grain boundary showed nanosized sintered-in nitride coexisting with ferrite and austenite upon sintering at α/γ interface but also at α/α and γ/γ interfaces. TKD-EDS compositional mapping revealed Ti-rich grain boundary. Nanoindentation experiments reveal that the TiN dominated grain boundaries exhibit lower penetration depths, an indication of higher hardness and modulus.     

用SiO2微粉制备碳化硅粉体的研究

为回收利用SiO2微粉,探究了以SiO2微粉为原料通过碳热还原法制备碳化硅粉体的最佳工艺条件;研究了分别以石油焦、活性炭和石墨粉为还原剂对冶炼效果的影响。在最佳碳质还原剂的基础上,研究了不同配碳比(还原剂与SiO2微粉的质量比为1∶3.5、1∶3、1∶2.5、1∶2、1∶1.5)和不同冶炼时间(15、30、45、60 min)对冶炼效果的影响。结果表明:石油焦、活性炭、石墨粉3种碳质还原剂中,石油焦的冶炼效果最佳;将石油焦与原料SiO2微粉以质量比1∶2进行混合,在中频感应炉中以1650℃冶炼45 min为最佳冶炼工艺条件;以此能够得到晶粒生长较好、品质较高的碳化硅粉体,碳化硅含量高达93.50%(w)。