Effects of Bonding Treatment and Ball Milling on W-20 wt.% Cu Composite Powder for Injection Molding

W-20 wt.% Cu pseudo-alloys were produced via powder injection molding (PIM) with powders prepared thermochemically. Bonding treatment and ball milling (BTBM) were used, and the effects of BTBM on the characteristics of the powders, rheological properties of the feedstock, shrinkage and properties of the sintered samples were studied. The morphology of the powder changed from extremely agglomerated small particles to pebble-shaped smooth large particles which were composed of several small particles combined tightly. The tap density increased from 3.25 g/cm³ to 7.22 g/cm³, and the specific surface area decreased from 0.86 m²/g to 0.45 m²/g. The critical powder loading of the feedstock increased from 45 vol.% to 56 vol.% due to the change in powder characteristics, thereby improving densification and dimension precision. For the PIM samples sintered at 1290 °C for 120 min in a hydrogen gas, the oversizing factor decreased from 1.297 to 1.216, and the dimension fluctuation ratio decreased from ±0.61% to ±0.33%. At the same time, the relative density increased from 97.8% to 98.6%, the thermal conductivity increased from 218 W/(m·K) to 233 W/(m·K), and the average coefficients of thermal expansion were roughly similar, within the range of 8.43–8.52 × 10⁻⁶/K.     

Microwave-Assisted Hydrothermal Synthesis of Zinc-Aluminum Spinel ZnAl2O4

The drawback of the hydrothermal technique is driven by the fact that it is a time-consuming operation, which greatly impedes its commercial application. To overcome this issue, conventional hydrothermal synthesis can be improved by the implementation of microwaves, which should result in enhanced process kinetics and, at the same time, pure-phase and homogeneous products. In this study, nanometric zinc aluminate (ZnAl₂O₄) with a spinel structure was obtained by a hydrothermal method using microwave reactor. The average ZnAl₂O₄ crystallite grain size was calculated from the broadening of XRD lines. In addition, BET analysis was performed to further characterize the as-synthesized particles. The synthesized materials were also subjected to microscopic SEM and TEM observations. Based on the obtained results, we concluded that the grain sizes were in the range of 6–8 nm. The surface areas measured for the samples from the microwave reactor were 215 and 278 m² g⁻¹.     

Synthesis of Mg-Al Hydrotalcite Clay with High Adsorption Capacity

A novel Mg-Al metal oxide has been successfully synthesized by the calcination of hierarchical porous Mg-Al hydrotalcite clay obtained by using filter paper as a template under hydrothermal conditions. Various characterizations of the obtained nanoscale oxide particles verified the uniform dispersion of Mg-Al metal oxides on the filter paper fiber, which had a size of 2–20 nm and a highest specific surface area (SSA) of 178.84 m²/g. Structural characterization revealed that the as-prepared Mg-Al metal oxides preserved the tubular morphology of the filter paper fibers. Further experiments showed that the as-synthesized Mg-Al metal oxides, present at concentrations of 0.3 g/L, could efficiently remove sulfonated lignite from oilfield wastewater (initial concentration of 200 mg/L) in a neutral environment (pH = 7) at a temperature of 298 K. An investigation of the reaction kinetics found that the adsorption process of sulfonated lignite (SL) on biomorphic Mg-Al metal oxides fits a Langmuir adsorption model and pseudo-second-order rate equation. Thermodynamic calculations propose that the adsorption of sulfonated lignite was spontaneous, endothermic, and a thermodynamically feasible process.     

Characteristics of the Mg-Zn-Ca-Gd Alloy after Mechanical Alloying

Magnesium-based materials are interesting alternatives for medical implants, as they have promising mechanical and biological properties. Thanks to them, it is possible to create biodegradable materials for medical application, which would reduce both costs and time of treatment. Magnesium as the sole material, however, it is not enough to support this function. It is important to determine proper alloying elements and methods. A viable method for creating such alloys is mechanical alloying, which can be used to design the structure and properties for proper roles. Mechanical alloying is highly influenced by the milling time of the alloy, as the time of the process affects many properties of the milled powders. X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS) were carried out to study the powder morphology and chemical composition of Mg₆₅Zn₃₀Ca₄Gd₁ powders. Moreover, the powder size was assessed by granulometric method and the Vickers hardness test was used for microhardness testing. The samples were milled for 6 min, 13, 20, 30, 40, and 70 h. The hardness correlated with the particle size of the samples. After 30 h of milling time, the average value of hardness was equal to 168 HV and it was lower after 13 (333 HV), 20 (273 HV), 40 (329 HV), and 70 (314 HV) h. The powder particles average size increased after 13 (31 μm) h of milling time, up to 30 (45–49 μm) hours, and then sharply decreased after 40 (28 μm) and 70 (12 μm) h.     

Surface Characteristics and Catalytic Activity of Copper Deposited Porous Silicon Powder

Porous structured silicon or porous silicon (PS) powder was prepared by chemical etching of silicon powder in an etchant solution of HF: HNO₃: H₂O (1:3:5 v/v). An immersion time of 4 min was sufficient for depositing Cu metal from an aqueous solution of CuSO₄ in the presence of HF. Scanning electron microscopy (SEM) analysis revealed that the Cu particles aggregated upon an increase in metal content from 3.3 wt% to 9.8 wt%. H₂-temperature programmed reduction (H₂-TPR) profiles reveal that re-oxidation of the Cu particles occurs after deposition. Furthermore, the profiles denote the existence of various sizes of Cu metal on the PS. The Cu-PS powders show excellent catalytic reduction on the p-nitrophenol regardless of the Cu loadings.     

Upconversion Luminescence of Silica–Calcia Nanoparticles Co-doped with Tm3+ and Yb3+ Ions

Looking for upconverting biocompatible nanoparticles, we have prepared by the sol–gel method, silica–calcia glass nanopowders doped with different concentration of Tm³⁺ and Yb³⁺ ions (Tm³⁺ from 0.15 mol% up to 0.5 mol% and Yb³⁺ from 1 mol% up to 4 mol%) and characterized their structure, morphology, and optical properties. X-ray diffraction patterns indicated an amorphous phase of the silica-based glass with partial crystallization of samples with a higher content of lanthanides ions. Transmission electron microscopy images showed that the average size of particles decreased with increasing lanthanides content. The upconversion (UC) emission spectra and fluorescence lifetimes were registered under near infrared excitation (980 nm) at room temperature to study the energy transfer between Yb³⁺ and Tm³⁺ at various active ions concentrations. Characteristic emission bands of Tm³⁺ ions in the range of 350 nm to 850 nm were observed. To understand the mechanism of Yb³⁺–Tm³⁺ UC energy transfer in the SiO₂–CaO powders, the kinetics of luminescence decays were studied.     

Microstructures and Properties of Cu-rGO Composites Prepared by Microwave Sintering

This study investigated the effects of microwave sintering on the microstructures and properties of copper-rGO composites. Graphene oxide was coated onto copper particles by wet ball milling, and copper-rGO composites were formed upon microwave sintering in an argon atmosphere. Scanning electron microscopy was then used to observe the mixing in the ball-milled composite powder, and the morphology of the bulk composite after microwave sintering. Raman spectra revealed how graphene oxide changed with ball milling and with microwave sintering. The microhardness, electrical conductivity, and thermal conductivity of the composite were also measured. The results showed that graphene oxide and copper particles were well combined and uniformly distributed after wet ball milling. The overall microhardness of microwave-sintered samples was 81.1 HV, which was 14.2% greater than that of pure copper (71 HV). After microwave sintering, the microhardness of the samples in areas showing copper oxide precipitates with eutectic structures was 89.5 HV, whereas the microhardness of the precipitate-free areas was 70.6 HV. The electrical conductivity of the samples was 87.10 IACS%, and their thermal conductivity was 391.62 W·m⁻¹·K⁻¹.     

Magnetic Nanoparticles Embedded in a Silicon Matrix

This paper represents a short overview of nanocomposites consisting of magnetic nanoparticles incorporated into the pores of a porous silicon matrix by two different methods. On the one hand, nickel is electrochemically deposited whereas the nanoparticles are precipitated on the pore walls. The size of these particles is between 2 and 6 nm. These particles cover the pore walls and form a tube-like arrangement. On the other hand, rather well monodispersed iron oxide nanoparticles, of 5 and 8 nm respectively, are infiltrated into the pores. From their size the particles would be superparamagnetic if isolated but due to magnetic interactions between them, ordering of magnetic moments occurs below a blocking temperature and thus the composite system displays a ferromagnetic behavior. This transition temperature of the nanocomposite can be varied by changing the filling factor of the particles within the pores. Thus samples with magnetic properties which are variable in a broad range can be achieved, which renders this composite system interesting not only for basic research but also for applications, especially because of the silicon base material which makes it possible for today’s process technology.     

Effect of Fine Size-Fractionated Sunflower Husk Biochar on Water Retention Properties of Arable Sandy Soil

Biochar application has been reported to improve the physical, chemical, and hydrological properties of soil. However, the information about the size fraction composition of the applied biochar as a factor that may have an impact on the properties of soil-biochar mixtures is often underappreciated. Our research shows how sunflower husk biochar (pyrolyzed at 650 °C) can modify the water retention characteristics of arable sandy soil depending on the biochar dose (up to 9.52 wt.%) and particle size (<50 µm, 50–100 µm, 100–250 µm). For comparison, we used soil samples mixed with biochar passed through 2 mm sieve and an unamended reference. The addition of sieved biochar to the soil caused a 30% increase in the available water content (AWC) in comparing to the soil without biochar. However, the most notable improvement (doubling the reference AWC value from 0.078 m³ m⁻³ to 0.157 m³ m⁻³) was observed at the lowest doses of biochar (0.95 and 2.24 wt.%) and for the finest size fractions (below 100 µm). The water retention effects on sandy soil are explained as the interplay between the dose, the size of biochar particles, and the porous properties of biochar fractions.     

Mechanochemical Activation and Spark Plasma Sintering of the Lead-Free Ba(Fe1/2Nb1/2)O3 Ceramics

This paper investigates the impact of the technological process (Mechanochemical Activation (MA) of the powder in combination with the Spark Plasma Sintering (SPS) method) on the final properties of lead-free Ba(Fe_1/2Nb_1/2)O₃ (BFN) ceramic materials. The BFN powders were obtained for different MA duration times (x from 10 to 100 h). The mechanically activated BFN powders were used in the technological process of the BFN ceramics by the SPS method. The measurements of the BFN_xMA ceramic samples included the following analysis: Scanning Electron Microscopy (SEM), Energy Dispersive Spectrometry (EDS), DC electrical conductivity, and dielectric properties. X-ray diffractions (XRD) tests showed the appearance of the perovskite phase of BFN powders after 10 h of milling time. The longer milling time (up 20 h) causes the amount of the perovskite phase to gradually increase, and the diffraction peaks are more clearly visible. Short high energy milling times favor a large heterogeneity of the grain shape and size. Increasing the MA milling time to 40 h significantly improves the microstructure of BFN ceramics sintered in the SPS technology. The microstructure becomes fine-grained with clearly visible grain boundaries and higher grain size uniformity. Temperature measurements of the BFN ceramics show a number of interesting dielectric properties, i.e., high values of electric permittivity, relaxation properties with a diffusion phase transition, as well as negative values of dielectric properties occurring at high temperatures. The high electric permittivity values predestines the BFN_xMA materials for energy storage applications e.g., high energy density batteries, while the negative values of dielectric properties can be used for shield elements against the electromagnetic radiation.     

Purification of Oncornaviruses by Agglutination with Concanavalin A

Concanavalin A (Con A) has been used to rapidly and selectively agglutinate murine and avian oncornavirions from culture medium or plasma. The agglutinated virus was concentrated rapidly and gently by low-speed centrifugation and solubilization with α-methyl mannoside. Infectious virus was purified 2.3 times with respect to nucleic-acid content, and more than 60% of its infectivity was recovered. Infectious particles of densities 1.18 and 1.16 g/cm³ were found in mouse cells infected with Friend virus. Con A reacted only with particles of density 1.16 g/cm³, indicating heterogeneity with respect to carbohydrate content or structure as well as buoyant density. Electron microscopy of virus agglutinated with Con A showed a zone of Con A-glycoprotein complexes averaging 12-15 nm in thickness.     

Tuning the Pore Geometry of Ordered Mesoporous Carbons for Enhanced Adsorption of Bisphenol-A

Mesoporous carbons were synthesized via both soft and hard template methods and compared to a commercial powder activated carbon (PAC) for the adsorption ability of bisphenol-A (BPA) from an aqueous solution. The commercial PAC had a BET-surface of 1027 m²/g with fine pores of 3 nm and less. The hard templated carbon (CMK-3) material had an even higher BET-surface of 1420 m²/g with an average pore size of 4 nm. The soft templated carbon (SMC) reached a BET-surface of 476 m²/g and a pore size of 7 nm. The maximum observed adsorption capacity (q_max) of CMK-3 was the highest with 474 mg/g, compared to 290 mg/g for PAC and 154 mg/g for SMC. The difference in adsorption capacities was attributed to the specific surface area and hydrophobicity of the adsorbent. The microporous PAC showed the slowest adsorption, while the ordered mesopores of SMC and CMK-3 enhanced the BPA diffusion into the adsorbent. This difference in adsorption kinetics is caused by the increase in pore diameter. However, CMK-3 with an open geometry consisting of interlinked nanorods allows for even faster intraparticle diffusion.     

Effect of Polyphenylsulfone and Polysulfone Incompatibility on the Structure and Performance of Blend Membranes for Ultrafiltration

This study deals with the modification of polyphenylsulfone ultrafiltration membranes by introduction of an incompatible polymer polysulfone to the polyphenylsulfone casting solution to improve the permeability. The correlation between properties of the blend polyphenylsulfone/polysulfone solutions and porous anisotropic membranes for ultrafiltration prepared from these solutions was revealed. The blend polyphenylsulfone/polysulfone solutions were investigated using a turbidity spectrum method, optical microscopy and measurements of dynamic viscosity and turbidity. The structure of the prepared blend flat sheet membranes was studied using scanning electron microscopy. Membrane separation performance was investigated in the process of ultrafiltration of human serum albumin buffered solutions. It was found that with the introduction of polysulfone to the polyphenylsulfone casting solution in N-methyl-2-pyrrolidone the size of supramolecular particles significantly increases with the maximum at (40–60):(60:40) polyphenylsulfone:polysulfone blend ratio from 76 nm to 196–354 nm. It was shown that polyphenylsulfone/polysulfone blend solutions, unlike the solutions of pristine polymers, are two-phase systems (emulsions) with the maximum droplet size and highest degree of polydispersity at polyphenylsulfone/polysulfone blend ratios (30–60):(70–40). Pure water flux of the blend membranes passes through a maximum in the region of the most heterogeneous structure of the casting solution, which is associated with the imposition of a polymer-polymer phase separation on the non-solvent induced phase separation upon membrane preparation. The application of polyphenylsulfone/polysulfone blends as membrane-forming polymers and polyethylene glycol (M_n = 400 g·mol⁻¹) as a pore-forming agent to the casting solutions yields the formation of ultrafiltration membranes with high membrane pure water flux (270 L·m⁻²·h⁻¹ at 0.1MPa) and human serum albumin rejection of 85%.     

Matrix Structure Evolution and Nanoreinforcement Distribution in Mechanically Milled and Spark Plasma Sintered Al-SiC Nanocomposites

Development of homogenous metal matrix nanocomposites with uniform distribution of nanoreinforcement, preserved matrix nanostructure features, and improved properties, was possible by means of innovative processing techniques. In this work, Al-SiC nanocomposites were synthesized by mechanical milling and consolidated through spark plasma sintering. Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray Spectroscopy (EDS) facility was used for the characterization of the extent of SiC particles’ distribution in the mechanically milled powders and spark plasma sintered samples. The change of the matrix crystallite size and lattice strain during milling and sintering was followed through X-ray diffraction (XRD). The density and hardness of the developed materials were evaluated as function of SiC content at fixed sintering conditions using a densimeter and a digital microhardness tester, respectively. It was found that milling for 24 h led to uniform distribution of SiC nanoreinforcement, reduced particle size and crystallite size of the aluminum matrix, and increased lattice strain. The presence and amount of SiC reinforcement enhanced the milling effect. The uniform distribution of SiC achieved by mechanical milling was maintained in sintered samples. Sintering led to the increase in the crystallite size of the aluminum matrix; however, it remained less than 100 nm in the composite containing 10 wt.% SiC. Density and hardness of sintered nanocomposites were reported and compared with those published in the literature.     

Structure and Properties of Barium Titanate Lead-Free Piezoceramic Manufactured by Binder Jetting Process

This article presents the results of manufacturing samples from barium titanate (BaTiO₃) lead-free piezoceramics by using the binder jetting additive manufacturing process. An investigation of the manufacturing process steps for two initial powders with different particle size distributions was carried. The influence of the sintering and the particle size distribution of the starting materials on grain size and functional properties was evaluated. Samples from fine unimodal powder compared to coarse multimodal one have 3–4% higher relative density values, as well as a piezoelectric coefficient of 1.55 times higher values (d₃₃ = 183 pC/N and 118 pC/N correspondingly). The influence of binder saturation on sintering modes was demonstrated. Binder jetting with 100% saturation for both powders enables printing samples without delamination and cracking. Sintering at 1400 °C with a dwell time of 6 h forms the highest density samples. The microstructure of sintered samples was characterized with scanning electron microscopy. The possibility of manufacturing parts from functional ceramics using additive manufacturing was demonstrated.     

Simple Preparation of Novel Metal-Containing Mesoporous Starches

Metal-containing mesoporous starches have been synthesized using a simple and efficient microwave-assisted methodology followed by metal impregnation in the porous gel network. Final materials exhibited surface areas >60 m² g⁻¹, being essentially mesoporous with pore sizes in the 10–15 nm range with some developed inter-particular mesoporosity. These materials characterized by several techniques including XRD, SEM, TG/DTA and DRIFTs may find promising catalytic applications due to the presence of (hydr)oxides in their composition.     

Phenomena Occurring upon the Sintering of a Mixture of Yttria–Zirconia Nanometric Powder and Sub-Micrometric Pure Zirconia Powder

Mixtures of powders essentially differing in their particle morphology and size were applied to prepare polycrystals in a Y₂O₃-ZrO₂ system. An yttria–zirconia solid solution nanometric powder with a Y₂O₃ concentration of 3.5% was prepared by subjecting co-precipitated gels to hydrothermal treatment at 240 °C. The crystallization occurred in distilled water. The pure zirconia powders composed of elongated and sub-micrometer size particles were also manufactured through the hydrothermal treatment of pure zirconia gel, although in this case, the process took place in the NaOH solution. Mixtures of the two kinds of powder were prepared so as to produce a mean composition corresponding to an yttria concentration of 3 mol%. Compacts of this powder mixture were sintered, and changes in phase composition vs. temperature were studied using X-ray diffraction. The dilatometry measurements revealed the behavior of the powder compact during sintering. The polished surfaces revealed the microstructure of the resulting polycrystal. Additionally, the electron back scattering diffraction technique (EBSD) allowed us to identify symmetry between the observed grains. Hardness, fracture toughness, and mechanical strength measurements were also performed.     

Synthesis and Enhanced Phosphate Recovery Property of Porous Calcium Silicate Hydrate Using Polyethyleneglycol as Pore-Generation Agent

The primary objective of this paper was to synthesize a porous calcium silicate hydrate (CSH) with enhanced phosphate recovery property using polyethyleneglycol (PEG) as pore-generation agent. The formation mechanism of porous CSH was proposed. PEG molecules were inserted into the void region of oxygen–silicon tetrahedron chains and the layers of CSH. A steric hindrance layer was generated to prevent the aggregation of solid particles. A porous structure was formed due to the residual space caused by the removal of PEG through incineration. This porous CSH exhibited highly enhanced solubility of Ca²⁺ and OH⁻ due to the decreased particle size, declined crystalline, and increased specific surface area (S_BET) and pore volume. Supersaturation was increased in the wastewater with the enhanced solubility, which was beneficial to the formation of hydroxyapatite (HAP) crystallization. Thus, phosphate can be recovered from wastewater by producing HAP using porous CSH as crystal seed. In addition, the regenerated phosphate-containing products (HAP) can be reused to achieve sustainable utilization of phosphate. The present research could provide an effective approach for the synthesis of porous CSH and the enhancement of phosphate recovery properties for environmental applications.     

Enhanced Hydrogen Generation Performance of Al-Rich Alloys by a Melting-Mechanical Crushing-Ball Milling Method

The main problem for the application of hydrogen generated via hydrolysis of metal alloys is the low hydrogen generation rate (HGR). In this paper, active Al alloys were prepared using a new coupled method-melting-mechanical crushing-mechanical ball milling method to enhance the HGR at room temperature. This method contains three steps, including the melting of Al, Ga, In, and Sn ingots with low melting alloy blocks and casting into plates, then crushing alloy plate into powders and ball milling with chloride salts such as NiCl₂ and CoCl₂ were added during the ball milling process. The microstructure and phase compositions of Al alloys and reaction products were investigated via X-ray diffraction and scanning electron microscopy with energy dispersed X-ray spectroscopy. The low-melting-point Ga-In -Sn (GIS) phases contain a large amount of Al can act as a transmission medium for Al, which improves the diffusion of Al to Al/H₂O reaction sites. Finer GIS phases after ball milling can further enhance the diffusion of Al and thus enhance the activity of Al alloy. The hydrogen generation performance through hydrolysis of water with Al at room temperature was investigated. The results show that the H₂ generation performance of the Al-low-melting point alloy composite powder is significantly higher than the results reported to date. The highest H₂ generation rate and H₂ conversion efficiency can reach 5337 mL·min⁻¹·g⁻¹ for the hydrolysis of water with 1 g active alloy.     

Sodium Solid Electrolytes: NaxAlOy Bilayer-System Based on Macroporous Bulk Material and Dense Thin-Film

A new preparation concept of a partially porous solid-state bilayer electrolyte (BE) for high-temperature sodium-ion batteries has been developed. The porous layer provides mechanical strength and is infiltrated with liquid and highly conductive NaAlCl₄ salt, while the dense layer prevents short circuits. Both layers consist, at least partially, of Na-β-alumina. The BEs are synthesized by a three-step procedure, including a sol-gel synthesis, the preparation of porous, calcined bulk material, and spin coating to deposit a dense layer. A detailed study is carried out to investigate the effect of polyethylene oxide (PEO) concentration on pore size and crystallization of the bulk material. The microstructure and crystallographic composition are verified for all steps via mercury intrusion, X-ray diffraction, and scanning electron microscopy. The porous bulk material exhibits an unprecedented open porosity for a Na_xAlO_y bilayer-system of ≤57% with a pore size of ≈200–300 nm and pore volume of ≤0.3 cm³∙g⁻¹. It contains high shares of crystalline α-Al₂O₃ and Na-β-alumina. The BEs are characterized by impedance spectroscopy, which proved an increase of ionic conductivity with increasing porosity and increasing Na-β-alumina phase content in the bulk material. Ion conductivity of up to 0.10 S∙cm⁻¹ at 300 °C is achieved.