The Structure-Properties-Cytotoxicity Interplay: A Crucial Pathway to Determining Graphene Oxide Biocompatibility.

Interest in graphene oxide nature and potential applications (especially nanocarriers) has resulted in numerous studies, but the results do not lead to clear conclusions. In this paper, graphene oxide is obtained by multiple synthesis methods and generally characterized. The mechanism of GO interaction with the organism is hard to summarize due to its high chemical activity and variability during the synthesis process and in biological buffers' environments. When assessing the biocompatibility of GO, it is necessary to take into account many factors derived from nanoparticles (structure, morphology, chemical composition) and the organism (species, defense mechanisms, adaptation). This research aims to determine and compare the in vivo toxicity potential of GO samples from various manufacturers. Each GO sample is analyzed in two concentrations and applied with food. The physiological reactions of an easy model Acheta domesticus (cell viability, apoptosis, oxidative defense, DNA damage) during ten-day lasting exposure were observed. This study emphasizes the variability of the GO nature and complements the biocompatibility aspect, especially in the context of various GO-based experimental models. Changes in the cell biomarkers are discussed in light of detailed physicochemical analysis.

Control of Arms of Au Stars Size and its Dependent Cytotoxicity and Photosensitizer Effects in Photothermal Anticancer Therapy.

Gold nanostars (AuS NPs) are a very attractive nanomaterial, which is characterized by high effective transduction of the electromagnetic radiation into heat energy. Therefore, AuS NPs can be used as photosensitizers in photothermal therapy (PTT). However, understanding the photothermal conversion efficiency in nanostars is very important to select the most appropriate shape and size of AuS NPs. Therefore, in this article, the synthesis of AuS NPs with different lengths of star arms for potential application in PTT was investigated. Moreover, the formation mechanism of these AuS NPs depending on the reducer concentration is proposed. Transmission electron microscopy (TEM) with selected area diffraction (SEAD) and X-ray diffraction (X-Ray) showed that all the obtained AuS NPs are crystalline and have cores with similar values of the diagonal (parameter d), from 140 nm to 146 nm. However, the widths of the star arm edges (parameter c) and the lengths of the arms (parameter a) vary between 3.75 nm and 193 nm for AuS1 NPs to 6.25 nm and 356 nm for AuS4 NPs. Ultraviolet-visible (UV-Vis) spectra revealed that, with increasing edge widths and lengths of the star arms, the surface plasmon resonance (SPR) peak is shifted to the higher wavelengths, from 640 nm for AuS1 NPs to 770 nm for AuS4 NPs. Moreover, the increase of temperature in the AuS NPs solutions as well as the values of calculated photothermal efficiency grew with the elongation of the star arms. The potential application of AuS NPs in the PTT showed that the highest decrease of viability, around 75%, of cells cultured with AuS NPs and irradiated by lasers was noticed for AuS4 NPs with the longest arms, while the smallest changes were visible for gold nanostars with the shortest arms. The present study shows that photothermal properties of AuS NPs depend on edge widths and lengths of the star arms and the values of photothermal efficiency are higher with the increase of the arm lengths, which is correlated with the reducer concentration.

Single-step synthesis of Er3+ and Yb3+ ions doped molybdate/Gd2O3 core-shell nanoparticles for biomedical imaging.

Nanostructures as color-tunable luminescent markers have become major, promising tools for bioimaging and biosensing. In this paper separated molybdate/Gd2O3 doped rare earth ions (erbium, Er3+ and ytterbium, Yb3+) core-shell nanoparticles (NPs), were fabricated by a one-step homogeneous precipitation process. Emission properties were studied by cathodo- and photoluminescence. Scanning electron and transmission electron microscopes were used to visualize and determine the size and shape of the NPs. Spherical NPs were obtained. Their core-shell structures were confirmed by x-ray diffraction and energy-dispersive x-ray spectroscopy measurements. We postulated that the molybdate rich core is formed due to high segregation coefficient of the Mo ion during the precipitation. The calcination process resulted in crystallization of δ/ξ (core/shell) NP doped Er and Yb ions, where δ-gadolinium molybdates and ξ-molybdates or gadolinium oxide. We confirmed two different upconversion mechanisms. In the presence of molybdenum ions, in the core of the NPs, Yb3+-[Formula: see text] (∣2F7/2, 3T2〉) dimers were formed. As a result of a two 980 nm photon absorption by the dimer, we observed enhanced green luminescence in the upconversion process. However, for the shell formed by the Gd2O3:Er, Yb NPs (without the Mo ions), the typical energy transfer upconversion takes place, which results in red luminescence. We demonstrated that the NPs were transported into cytosol of the HeLa and astrocytes cells by endocytosis. The core-shell NPs are sensitive sensors for the environment prevailing inside (shorter luminescence decay) and outside (longer luminescence decay) of the tested cells. The toxicity of the NPs was examined using MTT assay.

Oxidative stress and genotoxic effects of diamond nanoparticles.

Due to the unique and useful properties of nanodiamonds (ND), their production and use is rapidly increasing. Thus, more of these particles will be released into the environment and organisms will inevitably be exposed to them. The current knowledge about the toxicity of ND, especially in vivo toxicity, is fragmentary. In this study, the toxicity of nanodiamonds was assessed in Acheta domesticus following chronic exposure to different nominal concentrations of ND (20 and 200µgg(-1) food) administrated in food for the entire lifespan. The activity of oxidative stress enzymes (catalase, glutathione peroxidase), total antioxidant capacity, as well as the level of heat shock protein were determined. A significant increase in all of the measured parameters was observed after seven weeks of exposure in individuals exposed to higher concentrations of ND (200µgg(-1) food). In animals exposed to lower concentrations of ND (20µgg(-1) food), there were few significant changes to these parameters. Analysis of DNA damage performed after fourteen weeks using the comet assay revealed DNA instabilities in the insects, especially the ones that had been exposed to the higher doses of ND. These findings may suggest that the toxicity of ND is concentration dependent. While high doses interact in a toxic manner, trace amounts, which are more likely in the environment, might be safe for organisms. Extreme caution should be taken when handling nanodiamonds.

Linear polymer separation using carbon-nanotube-modified centrifugal filter units.

The separation of linear polymers such as polysaccharides and polyethylene glycol was performed with modified commercial centrifugal filter units. The deposition of a 0.16-0.35 µm layer of modified carbon nanotubes prevented permeation of linear polymers of molecular weight higher than 20 000 Da through the membrane. It allowed facile purification of solution of 0.1 g of polymer samples from small molecules within 25 min by using a bench-top centrifuge. The structure of modified carbon nanotubes was optimized in order to achieve good adhesion to the low binding regenerated cellulose surface and low solubility in aqueous solutions after deposition. The best modification of carbon nanotubes was oxidation and subsequent amide formation of diethanolamine. Introduction of acetic acid groups using sodium chloroacetate worked equally well. The modified filter could be used multiple times without the decrease of the efficiency. The carbon nanotubes layer was stable in aqueous solutions in a pH range of 1-7. The proposed method provides a convenient way of purification of modified polymers in research areas such as drug delivery or macromolecular probes synthesis.

Using the IL-TEM Technique to Understand the Mechanism and Improve the Durability of Platinum Cathode Catalysts for Proton-Exchange Membrane Fuel Cells.

Proton-exchange membrane fuel cells are one of the most promising energy conversion technologies for both automotive and stationary applications. Scientists are testing a number of solutions to increase the durability of cells, especially catalysts, which are the most expensive component. These solutions include, among others, the modification of the composition and morphology of supported nanoparticles, the platinum-support interface, and the support itself. A detailed understanding of the mechanism of platinum degradation and the subsequent improvement of the durability of the entire cell requires the development of methods for effectively monitoring the behavior of catalytic nanoparticles under various cell operating conditions. The Identical-Location Transmission Electron Microscopy (IL-TEM) method makes it possible to visually track structural and morphological changes in the catalyst directly. Because the tests are performed with a liquid electrolyte imitating a membrane, they provide better control of the degradation conditions and, consequently, facilitate the understanding of nanoparticle degradation processes in various operating conditions. This review is primarily intended to disseminate knowledge about this technique to scientists using electron microscopy in the study of energy materials and to draw attention to issues related to the characterization of the structure of carbon supports.

Artificial Manganese Metalloenzymes with Laccase-like Activity: Design, Synthesis, and Characterization.

Laccase is an oxidase of great industrial interest due to its ability to catalyze oxidation processes of phenols and persistent organic pollutants. However, it is susceptible to denaturation at high temperatures, sensitive to pH, and unstable in the presence of high concentrations of solvents, which is a issue for industrial use. To solve this problem, this work develops the synthesis in an aqueous medium of a new Mn metalloenzyme with laccase oxidase mimetic catalytic activity. Geobacillus thermocatenulatus lipase (GTL) was used as a scaffold enzyme, mixed with a manganese salt at 50 °C in an aqueous medium. This leads to the in situ formation of manganese(IV) oxide nanowires that interact with the enzyme, yielding a GTL-Mn bionanohybrid. On the other hand, its oxidative activity was evaluated using the ABTS assay, obtaining a catalytic efficiency 300 times higher than that of Trametes versicolor laccase. This new Mn metalloenzyme was 2 times more stable at 40 °C, 3 times more stable in the presence of 10% acetonitrile, and 10 times more stable in 20% acetonitrile than Novozym 51003 laccase. Furthermore, the site-selective immobilized GTL-Mn showed a much higher stability than the soluble form. The oxidase-like activity of this Mn metalloenzyme was successfully demonstrated against other substrates, such as l-DOPA or phloridzin, in oligomerization reactions.

Bio-based protic salts as precursors for sustainable free-standing film electrodes.

Transforming amines with low boiling points and high volatilities into protic salts is a versatile strategy to utilize low molecular weight compounds as precursors for N-doped carbon structures in a straightforward carbonization procedure. Herein, conventional mineral acids commonly used for the synthesis of protic salts were replaced by bio-derived phytic acid, which, combined with various amines and amino acids, yielded partially or fully bio-derived protic salts. The biomass-based salts showed higher char-forming ability than their mineral acid-based analogs (up to 55.9% at 800°), simultaneously providing carbon materials with significant porosity (up to 1177 m2g-1) and a considerable level of N,P,O-doping. Here, we present the first comprehensive study on the correlation between the structure of the bio-derived protic precursors and the properties of derived carbon materials to guide future designs of biomass-derived precursors for the one-step synthesis of sustainable carbon materials. Additionally, we demonstrate how to improve the textural properties of the protic-salt-derived carbons (which suffer from high brittleness) by simply upgrading them into highly flexible nanocomposites using high-quality single-walled carbon nanotubes. Consequently, self-standing electrodes for the oxygen reduction reaction were created.

Exploring CVD Method for Synthesizing Carbon-Carbon Composites as Materials to Contact with Nerve Tissue.

The main purpose of these studies was to obtain carbon-carbon composites with a core built of carbon fibers and a matrix in the form of pyrolytic carbon (PyC), obtained by using the chemical vapor deposition (CVD) method with direct electrical heating of a bundle of carbon fibers as a potential electrode material for nerve tissue stimulation. The methods used for the synthesis of PyC proposed in this paper allow us, with the appropriate selection of parameters, to obtain reproducible composites in the form of rods with diameters of about 300 µm in 120 s (CF_PyC_120). To evaluate the materials, various methods such as scanning electron microscopy (SEM), scanning transmission electron microscope (STEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and tensiometer techniques were used to study their microstructural, structural, chemical composition, surface morphology, and surface wettability. Assessing their applicability for contact with nervous tissue cells, the evaluation of cytotoxicity and biocompatibility using the SH-SY5Y human neuroblastoma cell line was performed. Viability and cytotoxicity tests (WST-1 and LDH release) along with cell morphology examination demonstrated that the CF_PyC_120 composites showed high biocompatibility compared to the reference sample (Pt wire), and the best adhesion of cells to the surface among all tested materials.

Influence of Preheating Temperature on Structural and Mechanical Properties of a Laser-Welded MMC Cobalt Based Coating Reinforced by TiC and PCD Particles.

This article presents research on the structural and mechanical properties of an innovative metal matrix composite (MMC) coating designed for use in conditions of intense metal-mineral abrasive wear. The layer, which is intended to protect the working surface of drilling tools used in the oil and natural gas extraction sector, was padded using the multi-run technique on a sheet made of AISI 4715 low-alloy structural steel by Laser Direct Metal Deposition (LDMD) using a high-power fiber laser (FL). An innovative cobalt alloy matrix powder with a ceramic reinforcement of crushed titanium carbide (TiC) and tungsten-coated synthetic polycrystalline diamond (PCD) was used as the surfacing material. The influence of the preheating temperature of the base material on the susceptibility to cracking and abrasive wear of the composite coating was assessed. The structural properties of the coating were characterized by using methods such as optical microscopy, scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS), transmission electron microscopy (TEM) and X-ray diffraction analysis (XRD). The mechanical properties of the hardfaced coating were assessed on the basis of the results of a metal-mineral abrasive wear resistance test, hardness measurement, and the observation of the abrasion area with a scanning laser microscope. The results of laboratory tests showed a slight dissolution of the tungsten coating protecting the synthetic PCD particles and the transfer of its components into the metallic matrix of the composite. Moreover, it was proved that an increase in the preheating temperature of the base material prior to welding has a positive effect on reducing the susceptibility of the coating to cracking, reducing the porosity of the metal deposit and increasing the resistance to abrasive wear.

Ultrafine multi-metal (Zn, Cd, Pb) sulfide aggregates formation in periodically water-logged organic soil.

This study investigates authigenic metal (Zn, Cd, and Pb) sulfides formed in the upper (4-20 cm) layer of severely degraded soil close to ZnPb smelter in CE Europe (southern Poland). The soil layer is circumneutral (pH 6.0-6.8), organic, occasionally water-logged, and contains on average 26,400 mg kg-1 Zn, 18,800 mg kg-1 Pb, 1300 mg kg-1 Cd, and 2500 mg kg-1 of sulfur. The distribution of the authigenic sulfide mineralization is uneven, showing close association with the remains of vascular plants (Equisetaceae, Carex, and herbs). A combination of focused ion beam (FIB) technology with scanning (SEM) and transmission electron microscopy (TEM) is used to reveal the structure and organization of the metal sulfides at micro- and nanoscale resolution. The sulfides form spheroidal and botryoidal porous aggregates composed of nanocrystalline (<5 nm) ZnCd sulfide solid solution and minor discrete PbS (galena) crystals up to 15 nm. The solid solution exists in a cubic (sphalerite) polytype over a whole Zn/Cd range. An intricate core-shell structure is found to be a characteristic feature of the aggregates in which high-Zn outer layers encapsulate Cd-rich sulfide core. PbS resides between the Cd-rich and Cd poor sulfide within nano sites of increased porosity. The study highlights the importance of nanoscale analyses for the prediction of metal behavior in soils. The sulfide self-organization into complex structures and Cd encapsulation inside high-Zn sulfide indicate the occurrence of a self-sustainable mechanism specific to polluted periodically water-logged soil that limits Cd mobility. However, as the reduced Cd mobility is obtained at the Zn expense, the soil gets Cd enriched relative to Zn over extended periods. Although the study proves PbS crystallization in the soil, the process seems environmentally irrelevant even at high Pb contents, being suppressed by other soil processes (e.g., Pb sorption on organic matter). Our findings are valuable in remediation strategies and the management of contaminated soils rich in organic matter that address the mobility of toxic metals and their transfer into living organisms.

Electrodeposition of Ni-Mo alloy coatings from choline chloride and propylene glycol deep eutectic solvent plating bath.

Ni-Mo alloy coatings were deposited on a copper base material from a non-aqueous plating bath based on a deep eutectic solvent (DES) of choline chloride and propylene glycol in a 1:2 molar ratio containing 0.2 mol dm-3 NiCl2 · 6H2O and 0.01 mol dm-3 (NH4)6Mo7O24·4H2O. Uniform and adherent Ni-Mo deposits with a nodular morphology were obtained at all the deposition potentials investigated (from - 0.5 to - 0.9 V vs. Ag). By shifting the potential from - 0.5 to - 0.9 V, the deposition current density increased from - 0.4 to - 1.5 mA cm-2 and the overall surface roughness increased. It was also accompanied by an increase in the Mo content from ~ 7 to ~ 13 wt% in the potential range from - 0.5 to - 0.7 V. A further change in the potential from - 0.8 to - 0.9 V caused a decrease in the Mo content to ~ 10 wt% and a deterioration in the quality of the coating. For the most uniform coating, deposited at - 0.6 V and having a thickness of ca. 660 nm, the crystallite size did not exceed 10 nm. With the content of Ni (89 at.%) and Mo (11 at.%), the selected area electron diffraction (SAED) analysis allowed us to identify the cubic phase Ni3.64Mo0.36. The corrosion resistance of Ni-Mo coatings in 0.05 mol dm-3 NaCl solution generally increased during exposure of 18 h, as evidenced by ever higher polarization resistance. Finally, regardless of the applied deposition potential, low corrosion currents (in the range of 0.1-0.3 µA cm-2) have been measured for the coatings. EIS revealed that charge transfer resistances were the highest (57-67 kΩ cm2) for coatings deposited at - 0.5 V, - 0.6 V and - 0.7 V. Further increase in the deposition potential in the negative direction was unfavorable.

Investigation of the Implementation of Laser Surface Alloying of Cu with Cr-WC.

This paper presents research on the microstructure and mechanical properties of an alloyed composite copper (Cu) surface layer, reinforced with a mixture of chromium-tungsten carbide (Cr-WC) powders. Copper alloying was performed using a high-power diode laser (HPDL). In the tests, three mixtures of powders with different percentage contents (75%Cr 25%WC, 50%Cr 50%WC, 25%Cr 75%WC) were injected into the melting pool during the laser surface alloying process. Microstructural evolution and the properties of the surface layer of copper after laser alloying were investigated. Structural investigations were performed using light microscopy, scanning and transmission electron microscopy (SEM, TEM) and X-ray diffraction (XRD). Microhardness and wear resistance of the modified surface layer were examined as well. After laser treatment the applied powders appear as uniformly distributed particles in the alloyed zone as well as nanoscale precipitates in the Cu matrix. Several types of precipitate characteristics, in terms of morphology, structure and chemical composition, were observed. Laser alloying of the surface layer modified the microstructure, which resulted in an increase in the hardness of the surface layers compared to the base material.

TEM Study of the Microstructure of an Alumina/Al Composite Prepared by Gas-Pressure Infiltration.

Ceramic injection moulding and gas-pressure infiltration were employed for the manufacturing of alumina/AlSi10Mg composites. Porous ceramic preforms were prepared by mixing alumina powder with a multi-binder system and injection moulding the powder polymer slurry. Then, the organic part was removed through a combination of solvent and thermal debinding, and, finally, the materials were sintered at different temperatures. Degrading the binder enabled open canals to form. The sintering process created a porous ceramic material consisting of alumina without any residual carbon content. During infiltration, the liquid metal filled the empty spaces (pores) effectively and formed a three-dimensional network of metal in the ceramic. The microstructure and properties of the manufactured materials were examined using high-resolution transmission electron microscopy, porosimetry, and bending strength testing. Microscopy observations showed that the fabricated composite materials are characterised by a percolation type of microstructure and a lack of unfilled pores. The research confirmed the diversified nature of the connection at the particle-matrix interface. It was observed that the interphase boundary was characterised by the lack of a transition zone between the components or a continuous transition zone, with the thickness not exceeding 30 nm. Thanks to their increased mechanical properties and low density, the obtained composites could be used in the automotive industry as a material for small piston rings and rods, connecting rods, or even gears.

Morphology, Phase and Chemical Analysis of Leachate after Bioleaching Metals from Printed Circuit Boards.

The article presents the assessment of solutions and dried residues precipitated from solutions after the bioleaching process of Printed Circuit Boards (PCB) utilizing the Acidithiobacillus ferrooxidans. The obtained dried residues precipitated from bioleaching solution (leachate) and control solution were tested using morphology, phase, and chemical composition analysis, with particular emphasis on the assessment of crystalline and amorphous components. The analysis of the dried residues from leachate after bioleaching as well as those from the sterile control solution demonstrated a difference in the component oxidation-the leachate consisted of mainly amorphous spherical particles in diameter up to 200 nm, forming lacy aggregates. In the specimenform control solution larger particles (up to 500 nm) were observed with a hollow in the middle and crystalline outer part (probably Fe2O3, CuFeS2, and Cu2O). The X-ray diffraction phase analysis revealed that specimen obtained from leachate after bioleaching consisted mainly of an amorphous component and some content of Fe2O3 crystalline phase, while the dried residue from control solution showed more crystalline components. The share of the crystalline and amorphous components can be related to efficiency in dissolving metals during bioleaching. Obtained results of the investigation confirm the activity and participation of the A. ferrooxidans bacteria in the solubilization process of electro-waste components, with their visible degradation-acceleration of the reaction owing to a continuous regeneration of the leaching medium. The performed investigations allowed to characterize the specimen from leachate and showed that the application of complementary cross-check of the micro (SEM and S/TEM) and macro (ICP-OES and XRD) methods are of immense use for complete guidance assessment and obtained valuable data for the next stages of PCBs recycling.

A Comprehensive Study of Pristine and Calcined f-MWCNTs Functionalized by Nitrogen-Containing Functional Groups.

We present the study of pristine and calcined f-MWCNTs functionalized by nitrogen-containing functional groups. We focus on the structural and microstructural modification tuned by the previous annealing. However, our primary goal was to analyze the electronic structure and magnetic properties in relation to the structural properties using a multi-technique approach. The studies carried out by X-ray diffraction, XPS, and 57Fe Mössbauer spectrometry revealed the presence of γ-Fe nanoparticles, Fe3C, and α-FeOOH as catalyst residues. XPS analysis based on the deconvolution of core level lines confirmed the presence of various nitrogen-based functional groups due to the purification and functionalization process of the nanotubes. The annealing procedure leads to a structural modification mainly associated with removing surface impurities as purification residues. Magnetic studies confirmed a significant contribution of Fe3C as evidenced by a Curie temperature estimated at TC = 452 ± 15 K. A slight change in magnetic properties upon annealing was revealed. The detailed studies performed on nanotubes are extremely important for the further synthesis of composite materials based on f-MWCNTs.

Metal-Support Interaction and Charge Distribution in Ceria-Supported Au Particles Exposed to CO.

Understanding how reaction conditions affect metal-support interactions in catalytic materials is one of the most challenging tasks in heterogeneous catalysis research. Metal nanoparticles and their supports often undergo changes in structure and oxidation state when exposed to reactants, hindering a straightforward understanding of the structure-activity relations using only ex situ or ultrahigh vacuum techniques. Overcoming these limitations, we explored the metal-support interaction between gold nanoparticles and ceria supports in ultrahigh vacuum and after exposure to CO. A combination of in situ methods (on powder and model Au/CeO2 samples) and theoretical calculations was applied to investigate the gold/ceria interface and its reactivity toward CO exposure. X-ray photoelectron spectroscopy measurements rationalized by first-principles calculations reveal a distinctly inhomogeneous charge distribution, with Au+ atoms in contact with the ceria substrate and neutral Au0 atoms at the surface of the Au nanoparticles. Exposure to CO partially reduces the ceria substrate, leading to electron transfer to the supported Au nanoparticles. Transferred electrons can delocalize among the neutral Au atoms of the particle or contribute to forming inert Auδ- atoms near oxygen vacancies at the ceria surface. This charge redistribution is consistent with the evolution of the vibrational frequencies of CO adsorbed on Au particles obtained using diffuse reflectance infrared Fourier transform spectroscopy.

Influence of the Halloysite Nanotube (HNT) Addition on Selected Mechanical and Biological Properties of Thermoplastic Polyurethane.

Halloysite nanotube (HNT) additions to the thermoplastic polyurethane (TPU) system were thoroughly evaluated in this study. The resultant composites have been designed for future personalized intervertebral disc implant applications, which requires additional technology to obtain the appropriate geometry unique to each patient. These requirements can be fulfilled using 3D printing. In this work, a technology was developed to produce filaments for fused deposition modeling (FDM). Nanocomposites were prepared using variable HNT content (1, 2, and 3 wt.%). The nanostructure of the resultant composites was confirmed using scanning transmission electron microscopy (STEM). Mechanical tests were used to measure the tensile modulus, stress, and elongation the composites and TPU matrix. Nanocomposites with 2% HNT content were able to withstand 26% increased stress and 50% increased elongation compared to pure TPU before fracturing in addition to a 13% reduction in the friction coefficient. A MTT cytotoxicity assay confirmed the cytotoxicity of all tested materials against human epidermal keratinocyte cells (HaCaT).

Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li7La3Zr2O12 Compound.

Li-ion batteries are widely used as energy storage devices due to their excellent electrochemical performance. The cubic Li7La3Zr2O12 (c-LLZO) compound is regarded as a promising candidate as a solid-state electrolyte for lithium-ion batteries due to its high bulk Li-ion conductivity, excellent thermal performance, and chemical stability. The standard manufacturing procedure involves the high-temperature and lengthy annealing of powders. However, the formation of the tetragonal modification of LLZO and other undesired side phases results in the deterioration of electrochemical properties. The mechanical milling of precursor powders can enhance the powders' reactivity and can result in an easier formation of c-LLZO. The aim of this work was to study the influence of selected milling and annealing parameters on c-LLZO compound formation. The starting powders of La(OH)3, Li2CO3, and ZrO2 were subjected to milling in various ball mills, under different milling conditions. The powders were then annealed at various temperatures for different lengths of times. These studies showed that the phase transformation processes of the powders were not very sensitive to the milling parameters. On the other hand, the final phase composition and microstructure strongly depended on heat treatment conditions. Low temperature annealing (750 °C) for 3 h produced 90% of c-LLZO in the powder structure.

Structure and Properties of Co-Cr-Mo Alloy Manufactured by Powder Injection Molding Method.

Cobalt-chromium-molybdenum alloys samples were obtained by the powder injection molding method (PIM). PIM is dedicated to the mass production of components and can manufacture several grades of dental screws, bolts, stabilizers, or implants. As a skeleton component, ethylene-vinyl acetate (EVA copolymer) with a low temperature of processing and softening point was used. The choice of a low-temperature binder made it necessary to use a coarse ceramic powder as a mechanical support of the green sample during sintering. The injection-molded materials were thermally degraded in N2 or Ar-5%H2 and further sintered in N2-5%H2 or Ar-5%H2 at 1300 or 1350 °C for 30 min. The structure of the obtained samples was characterized by X-ray diffraction and electron microscopy. Mechanical properties, including hardness and three-point bending tests, confirmed that a nitrogen-rich atmosphere significantly increases the bending strength compared to the material manufactured in Ar-5%H2. This is due to the precipitation of numerous fine nitrides and intermetallic phases that strengthen the ductile γ-phase matrix.