Inorganics, Volume 11, Issue 1 (January 2023) – 46 articles

We propose here a novel green synthesis route of core-shell magnetic nanomaterials based on the polyol method, which uses bio-based substances (BBS) derived from biowaste, as stabilizer and directing agent. First, we studied the effect of BBS concentration on the size, morphology, and composition of magnetic iron oxides nanoparticles obtained in the presence of BBS via the polyol synthesis method (MBBS). Then, as a proof of concept, we further coated MBBS with mesoporous silica (MBBS@mSiO₂) or titanium dioxide (MBBS@TiO₂) to obtain magnetic nanostructured core-shell materials. All the materials were deeply characterized with diverse physicochemical techniques. Results showed that both the size of the nanocrystals and their aggregation strongly depend on the BBS concentration used in the synthesis: the higher the concentration of BBS, the smaller the sizes of the iron oxide nanoparticles. On the other hand, the as-prepared magnetic core-shell nanomaterials were applied with good performance in different systems. In particular, MBBS@SiO₂ showed to be an excellent nanocarrier of ibuprofen and successful adsorbent of methylene blue (MB) from aqueous solution. MBBS@TiO₂ was capable of degrading MB with the same efficiency of pristine TiO₂. These excellent results encourage the use of bio-based substances in different types of synthesis methods since they could reduce the fabrication costs and the environmental impact. Full article

The present study, concerned with high-performance ORR catalysts, may be a valuable resource for a wide range of researchers within the fields of nanomaterials, electrocatalysis, and hydrogen energy. The objects of the research are electrocatalysts based on platinum–copper nanoparticles with onion-like and solid-solution structures. To evaluate the functional characteristics of the catalysts, the XRD, XRF, TEM, HAADF-STEM, and EDX methods, as well as the voltammetry method on a rotating disk electrode have been used. This work draws the attention of researchers to the significance of applying a protocol of electrochemically activating bimetallic catalysts in terms of the study of their functional characteristics on the rotating disk electrode. The choice of the potential range during the pre-cycling stage has been shown to play a crucial role in maintaining the durability of the catalysts. The activation of the PtCu/C catalyst during cycling of up to 1.0 V allows for an increase in the durability of the catalysts with onion-like and solid-solution structures of nanoparticles by 28% and 23%, respectively, as compared with activation of up to 1.2 V. Full article

Removing organic dyes from contaminated wastewater resulting from industrial effluents with a cost-effective approach addresses a major global challenge. The adsorption technique onto carbon-based materials and metal oxide is one of the most effective dye removal procedures. The current work aimed to evaluate the application of calcium oxide-doped carbon nitride nanostructures (CaO-g-C₃N₄) to eliminate basic fuchsine dyes (BF) from wastewater. CaO-g-C₃N₄ nanosorbent were obtained via ultrasonication and characterized by scanning electron microscopy, X-ray diffraction, TEM, and BET. The TEM analysis reveals 2D nanosheet-like nanoparticle architectures with a high specific surface area (37.31 m²/g) for the as-fabricated CaO-g-C₃N₄ nanosorbent. The adsorption results demonstrated that the variation of the dye concentration impacted the elimination of BF by CaO-C₃N₄ while no effect of pH on the removal of BF was observed. Freundlich isotherm and Pseudo-First-order adsorption kinetics models best fitted BF adsorption onto CaO-g-C₃N₄. The highest adsorption capacity of CaO-g-C₃N₄ for BF was determined to be 813 mg. g⁻¹. The adsorption mechanism of BF is related to the π-π stacking bridging and hydrogen bond, as demonstrated by the FTIR study. CaO-g-C₃N₄ nanostructures may be easily recovered from solution and were effectively employed for BF elimination in at least four continuous cycles. The fabricated CaO-g-C₃N₄ adsorbent display excellent BF adsorption capacity and can be used as a potential sorbent in wastewater purification. Full article

The development and implementation of technology that can capture and transform carbon dioxide (CO₂) is of ongoing interest. To that end, the integration of molecular electrocatalysts into devices is appealing because of the desirable features of molecules, such as the ability to modify active sites. Here, we explore how the identity of the aliphatic group in 1,4,8,11,15,18,22,25-octaalkoxyphthalocyanine cobalt(II) affects the catalytic behavior for heterogeneous CO₂ reduction electrocatalysis. The alkyl R-groups correspond to n-butoxy, sec-butoxy, and 2-ethylhexoxy. All of the catalysts are soluble in organic solvents and are readily solution-processed. However, the larger 2-ethylhexoxy group showed solution aggregation behavior at concentrations ≥1 mM, and it was, in general, an inferior catalyst. The other two catalysts show comparable maximum currents, but the octa sec-butoxy-bearing catalyst showed larger CO₂ reduction rate constants based on foot-of-the-wave analyses. This behavior is hypothesized to be due to the ability of the sec-butoxy groups to eliminate the ability of the alkoxy oxygen to block Co Sites via ligation. CO₂ reduction activity is rationalized based on solid-state structures. Cobalt(II) phthalocyanine and its derivatives are known to be good CO₂ reduction catalysts, but the results from this work suggest that straightforward incorporation of bulky groups can improve the processability and per site activity by discouraging aggregation. Full article

In the last few years, many efforts have been devoted to investigating the antibacterial activity of metal nanoparticles, especially against multidrug-resistant bacteria. Recently extensively drug-resistant (XDR) bacteria have emerged and caused a global threat. The purpose of this manuscript was to synthesize nanostructured γ-Al₂O₃ as an antibacterial agent against some XDRs. The results showed that Al₂O₃ was a mix of rod and spherical shapes in the nano range with diameters of less than 30 nm. The zeta potential was determined to estimate the surface charge for the synthesized γ-Al₂O₃, which was recorded as −34 ± 1.8 mV, indicating good stability. The synthesized nanostructured γ-Al₂O₃ showed a potent antibacterial activity against extensively drug-resistant Acinetobacter baumanii, with an inhibition zone diameter that reached 19 mm and a minimum inhibitory concentration (MIC) value that reached 2 µg/mL. The observed antibacterial activity of the prepared Al₂O₃ nanoparticles confirmed that the main mechanistic actions include bacterial cells apoptosis, ROS increment, cellular membrane disruption, and DNA damage. The cytotoxic effect (CC50) of the prepared γ-Al₂O₃-NPs was 1250 µg/mL in a normal human lung fibroblast cell line (WI-38 cells). It can be concluded that the synthesized γ-Al₂O₃ had an acceptable toxicity, which may pave the way for its use as a potent agent in the fight against XDR bacteria. Full article

Conductive electrochemically active metallopolymers are outstanding materials for energy storage and conversion, electrocatalysis, electroanalysis, and other applications. The hybrid inorganic–organic nature of these materials ensures their rich chemistry and offers wide opportunities for fine-tuning their functional properties. The electrochemical modulation of the nanomechanical properties of metallopolymers is rarely investigated, and the correlations between the structure, stiffness, and capacitive properties of these materials have not yet been reported. We use electrochemical atomic force microscopy (EC-AFM) to perform in-situ quantitative nanomechanical measurements of two Schiff base metallopolymers, poly[NiSalphen] and its derivative that contains two methoxy substituents in the bridging phenylene diimine unit poly[NiSalphen(CH₃O)₂], during their polarization in the electrolyte solution to the undoped and fully doped states. We also get insight into the electrochemical p-doping of these polymers using electrochemical quartz crystal microgravimetry (EQCM) coupled with cyclic voltammetry (CV). Combined findings for the structurally similar polymers with different interchain interactions led us to propose a correlation between Young’s modulus of the material, its maximum doping level, and ion and solvent fluxes in the polymer films upon electrochemical oxidation. Full article

The silver nanoparticle is a good antibacterial material being used as a broad-spectrum fungicide, including against some multidrug-resistant strains. Compared with the normal chemical and physical preparation methods, green synthesis has attracted wide attention, because of the pharmaceutical activities of the natural product, mild reaction conditions, and environmentally friendly, etc. In this study, the synthesis of silver nanoparticles (Ag NPs) was prepared from Bletilla striata polysaccharide (BSP) and characterized by UV-vis spectroscopy and Dynamic Light Scattering (DLS). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated the morphology of Ag NPs was subspherical with an average size of 20–35 nm. Bletilla striata polysaccharide not only can be used as a natural reducing agent, but also has good repairing ability. Moreover, the antibacterial experimental results showed its great antimicrobial activity against Gram-positive bacteria (Staphylococcus aureus), Gram-negative bacteria (Escherichia coli) and Candida albicans. Full article

The perovskites used for optoelectronic devices have been more attractive during recent years due to their wide variety of advantages, such as their low cost, high photoluminescence quantum yield (PLQY), high carrier mobility, flexible bandgap tunability, and high light absorption ability. However, optoelectronic applications for traditional inorganic and organic materials present dilemmas due to their hardly tunable bandgap and instability. On the other hand, there are some more important benefits for perovskite nanocrystals, such as a size-dependent bandgap and the availability of anion exchange at room temperature. Therefore, perovskite NC-based applications are currently favored, offering a research direction beyond perovskite, and much research has focused on the stability issue and device performance. Thus, the synthesis and applications of perovskite NCs need to be thoroughly discussed for the future development of solar cells, light-emitting diodes, photodetectors, and laser research. Full article

There is a growing interest in alternatives to lanthanide ion (Ln(III))-based luminescence sensitizing chromophores for in vivo applications, mainly in optical biological windows. Transition metals (M) are relevant candidates as chromophores as they have high absorption rates and emission bands covering a wide range of visible to near-infrared spectrum. However, despite the importance of theoretical models for the design of M–Ln(III) complexes, few contributions have devoted efforts to elucidating the energy transfer (ET) processes between M and Ln(III) ions. In this context, we adapted the intramolecular energy transfer (IET) to calculate, for the first time, the energy transfer rates for M–Ln(III) complexes. A new model was proposed that considers the assistance of phonons in the calculation of ET rates. As an example, the proposed model can estimate the ET rates between Eu(III) and Cr(III) ions in the [CrEuL₃]⁶⁺ complex (where L = 2-{6-[N,N-diethylcarboxamido]pyridin-2-yl}-1,1′-dimethyl-5,5′-methylene-2′-(5-methylpyridin-2-yl)bis [1H-benzimidazole]). The calculated rates (930–1200 s⁻¹) are in excellent agreement with the experimentally available data (750–1200 s⁻¹) when a phonon-assisted energy transfer process is considered. Thus, this proposed model can be useful to predict and explain photophysical properties driven by the energy transfer between Ln(III) ions and transition metals. Full article

The development and study of Na ion batteries are expanding. This study employs the hydrothermal technique to produce single-phase, well-crystallized, fluorine-added O₃-type NaFe_1-xMg_xO₂. Using XRD, FESEM, and HRTEM, the sample’s phase structure and morphological information were characterized. Initially, without adding fluorine the electrode suffers from poor stability at high voltage ranges and also during long-term cycling. So, fluorine was added to the structure and the electrochemical performance of the material was greatly increased. The electrochemical performance of O₃-type positive electrode materials for rechargeable Na ion batteries is evaluated. The capacity of fluorine-added O₃-type NaFe1-xMgxO₂ is approximately 163 mAh g⁻¹ (50 mA g⁻¹). Adding fluorine to the host structure increases the stability of the electrode, leading to improved electrochemical performance during long-term cycling. The electrochemical results indicate that fluorine-added O₃-type NaFe_1-xMg_xO₂ cathode material for cost-effective and environmentally friendly sodium-ion batteries is promising. Fluorine-based electrodes will be a future for Na ion energy storage devices Full article

The field of coordination chemistry has undergone rapid transformation from preparation of monometallic complexes to multimetallic complexes. So far numerous multimetallic coordination complexes have been synthesized. Multimetallic coordination complexes with well-defined architectures are often called as metal organic polygons and polyhedra (MOPs). In recent past, MOPs have received tremendous attention due to their potential applicability in various emerging fields. However, the field of coordination chemistry of MOPs often suffer set back due to the instability of coordination complexes particularly in aqueous environment-mostly by aqueous solvent and atmospheric moisture. Accordingly, the fate of the field does not rely only on the water solubilities of newly synthesized MOPs but very much dependent on their stabilities both in solution and solid state. The present review discusses several methodologies to prepare MOPs and investigates their stabilities under various circumstances. Considering the potential applicability of MOPs in sustainable way, several methodologies (remedies) to enhance the stabilities of MOPs are discussed here. Full article

Gypsum (GPS) has great potential for structural fire protection and is increasingly used in construction due to its high-water retention and purity. However, many researchers aim to improve its physical and mechanical properties by adding other organic or inorganic materials such as fibers, recycled GPS, and waste residues. This study used a novel method to add non-natural GPS from factory waste (phosphogypsum (PG)) as a secondary material for GPS. This paper proposes to mix these two materials to properly study the effect of PG on the physico-mechanical properties and fire performance of two Tunisian GPSs (GPS1 and GPS2). PG initially replaced GPS at 10, 20, 30, 40, and 50% weight percentage (mixing plan A). The PGs were then washed with distilled water several times. Two more mixing plans were run when the pH of the PG was equal to 2.4 (mixing plan B), and the pH was equal to 5 (mixing plan C). Finally, a comparative study was conducted on the compressive strength, flexural strength, density, water retention, and mass loss levels after 90 days of drying, before/after incineration of samples at 15, 30, 45, and 60 min. The results show that the mixture of GPS1 and 30% PG (mixing plan B) obtained the highest compressive strength (41.31%) and flexural strength (35.03%) compared to the reference sample. The addition of 10% PG to GPS1 (mixing plan A) improved fire resistance (33.33%) and the mass loss (17.10%) of the samples exposed to flame for 60 min compared to GPS2. Therefore, PG can be considered an excellent insulating material, which can increase physico-mechanical properties and fire resistance time of plaster under certain conditions. Full article

Benzo[c][1,2,5]oxadiazoles and benzo[c][1,2,5]thiadiazoles are recognized to possess potent pharmacological activities including anticancer potential. In continuation of our research endeavors in the development of boron-based heterocycles as potential therapeutic agents, herein we report the design and synthesis of new series of boron-based benzo[c][1,2,5]oxadiazoles and benzo[c][1,2,5]thiadiazoles as anticancer agents targeting tumor hypoxia. A series of seventeen compounds were synthesized in two steps in an efficient manner via substitution reactions followed by subsequent hydrolysis of aryltrifluoroboronate salts into corresponding boronic acid derivatives in the presence of silica. This is the first example to develop boron-based hypoxia agents. The synthesized hybrids were characterized by suitable spectroscopic techniques. The biological studies are currently underway. Full article

In this study, a low-temperature synthetic approach was developed for the fabrication of calcium hydroxyapatite (CHAp) coatings on a titanium substrate. The titanium substrates were first coated with CaCO₃ by a spin-coating technique using a sol–gel chemistry approach, and the obtained product was transformed into CHAp during a dissolution–precipitation reaction. The phase purity and structural and morphological features of the obtained CHAp coatings were evaluated by X-ray diffraction (XRD) analysis, FTIR spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM) and using a 3D optical profilometer. It was demonstrated that almost-single-phase CHAp formed on the titanium substrate with a negligible number of side phases, such as Na₂HPO₄ (starting material) and TiO₂. In the Raman spectrum of the CHAp coating, the peaks of phosphate group vibrations were clearly seen. Thus, the obtained results of Raman spectroscopy correlated well with the results of X-ray diffraction analysis. The corrosive behaviour of CHAp coatings on a titanium substrate was also evaluated using electrochemical methods. It was found that the corrosion resistance of titanium coated with CHAp increased significantly. These CHAp thin films may be potential candidates for use in not only in regenerative medicine but also in the development of different sensors. Full article

The mesomorphic behavior and the miscibility properties of binary mixtures of a new series of Schiff base metallomesogen (MOM) are evaluated by differential scanning calorimetry (DSC) and polarized optical microscopy (POM). Nuclear magnetic resonance (NMR), elemental analysis (CHNX), Fourier-transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA) were used to certify the molecular structure of the compounds. The results revealed that the studied mixtures are completely miscible throughout the composition field and exhibit a nematic phase which covered the whole composition range. In the mixtures, the stability of the nematic phase varies continuously, and it is possible to highlight the presence of a eutectic composition with a wide mesogenic stability range. Full article

Experimental magnetic studies performed on the [{CuLX}₂] system (HL = pyridine-2-carbaldehyde thiosemicarbazone, X = Cl⁻, Br⁻, I⁻) point to the larger electronegativity in X, the lower magnitude of the antiferromagnetic interactions. In order to confirm this and other trends observed and to dip into them, computational studies on the [{CuLX}₂] (X = Cl⁻ (1), I⁻ (2)) compounds are here reported. The chemical and structural comparisons have been extended to the compounds obtained in acid medium. In this regard, chlorido ligands yield the [Cu(HL)Cl₂]∙H₂O (3) complex, whose crystal structure shows that thiosemicarbazone links as a tridentate chelate ligand to square pyramidal Cu(II) ions. On the other hand, iodido ligands provoke the formation of the [{Cu(H₂L)I₂}₂] (4) derivative, which contains pyridine-protonated cationic H₂L⁺ as a S-donor monodentate ligand bonded to Cu(I) ions. Crystallographic, infrared and electron paramagnetic resonance spectroscopic results are discussed. Computational calculations predict a greater stability for the chlorido species, containing both the neutral (HL) and anionic (L⁻) ligand. The theoretical magnetic studies considering isolated dimeric entities reproduce the sign and magnitude of the antiferromagnetism in 1, but no good agreement is found for compound 2. The sensitivity to the basis set and the presence of interdimer magnetic interactions are debated. Full article

A series of latonduine derivatives, namely 11-nitro-indolo[2,3-d]benzazepine-7-(1-amino-hydantoin) (B), triazole-fused indolo[2,3-d]benzazepine-based Schiff bases HL¹ and HL² and metal complexes [M(p-cymene)(HL¹)Cl]Cl, where M = Ru (1), Os (2), and [Cu(HL²)Cl₂] (3) were synthesized and characterized by spectroscopic techniques (UV–vis, ¹H, ¹³C, ¹⁵N–¹H HSQC NMR) and ESI mass spectrometry. The molecular structures of B and HL¹ were confirmed by single-crystal X-ray diffraction, while that of 3 by electron diffraction of nanometer size crystalline sample. Molecular docking calculations of species B in the binding pocket of PIM-1 enzyme revealed that the 1-amino-hydantoin moiety is not involved in any hydrogen-bonding interactions, even though a good accommodation of the host molecule in the ATP binding pocket of the enzyme was found. The antiproliferative activity of organic compounds B, HL¹ and HL², as well as complexes 1–3 was investigated in lung adenocarcinoma A549, colon adenocarcinoma LS-174 and triple-negative breast adenocarcinoma MDA-MB-231 cells and normal human lung fibroblast cells MRC-5 by MTT assays; then, the results are discussed. Full article

Despite the large number of peptidomimetics with incorporated heteroannularly functionalized ferrocenes, few studies have investigated their bioactivity. Here, we report the biological evaluation and conformational analysis of enantiomeric dipeptides derived from 1′-aminoferrocene-1-carboxylic acid (Fca) and hydrophobic amino acids (AA = Val, Leu, Phe). The conformational properties of Y-AA-Fca-OMe (Y = Ac, Boc) were elucidated by experimental (IR, NMR, CD, and X-ray) and theoretical (DFT) methods. The prepared dipeptides were screened for their antimicrobial activity against selected Gram-positive and Gram-negative bacteria, lactic acid bacteria and yeasts, while their antioxidant activity was tested by DPPH and FRAP methods. Of all compounds tested, dipeptide d-2a showed the best antibacterial properties against S. aureus, B. subtilis, and P. aeruginosa at a concentration of 2 mM. The time–kill curves showed that antibacterial activity was concentration- and time-dependent. Chirality (d-) and a more polar-protecting group (Ac) were found to affect the biological activity, both antimicrobial and antioxidant. All investigated peptides are considered to be highly hydrophobic and chemically stable in both acidic and buffer media. Dipeptides d-1a–3a, which showed biological activity, were subjected to the determination of proteolytic activity, revealing very good resistance to proteolysis in the presence of chymotrypsin. Full article

The bimetallic PtRu nanoparticles deposited on the carbon support with the metals’ atomic ratio of 1:1 have been obtained by different liquid-phase synthesis methods. The metals’ mass fraction in the obtained PtRu/C catalysts is about 27%. The average size of the bimetallic nanoparticles ranges from 1.9 to 3.9 nm. The activity of the obtained PtRu/C catalysts in the methanol electrooxidation reaction as well as their tolerance to intermediate products of its oxidation have been studied. The sample synthesized by the polyol method has proved to be the most active material. The values of its electrochemical surface area and activity in the methanol electrooxidation reaction are 1.5–1.7 times higher than those of the commercial PtRu/C analogue. Nevertheless, the use of the polyol method leads to losses of the metals during the synthesis. Therefore, this method needs further optimization. Full article

Glass samples were synthesized according to 10Li₂O + 20CuO + xBi₂O₃ + (70 − x)B₂O₃, where x = 0, 10, 20, 30, 40 mol% by the melt-quenching method. The ability of the prepared glass to protect against gamma rays and neutrons was examined experimentally and theoretically. The mass attenuation coefficient (MAC) was calculated experimentally at energies of 0.662, 1.173, and 1.333 MeV using ¹³⁷Cs and ⁶⁰Co sources. The obtained results were compared with the theoretical ones using a Phy-x/PSD software program version 0.1.0.0. It was found that the experimental and theoretical results are very agreed upon. Moreover, other nuclear radiation shielding parameters were evaluated. The results showed that the addition of bismuth oxide leads to an improvement in the ability of the composite glass to attenuate gamma rays by increasing the values of MAC and Z_eff, while it led to a decrease in the HVL and MFP, as well as the EBF and EABF. The results also showed that the addition of copper oxide led to an improvement in the ability of the present glass to slow down fast neutrons. Sample BiS40 showed the best result for gamma ray attenuation and sample BiS10 gave the best result for fast neutron removal cross section. The results were compared with some materials used for gamma ray shielding and fast neutron removal cross section, and it was concluded that samples Bi40 and BiS10 outperformed all commercial materials. Full article

The alloy TiFe is widely used as hydrogen storage material. However, the first hydrogenation is difficult. It was found that the addition of zirconium greatly improves the kinetic of first hydrogenation, but the mechanism is not well understood. In this paper, we report the use of scanning photoemission microscopy to investigate the composition and chemical state of the various phases present in this alloy and how they change upon hydrogenation/dehydrogenation. We found the presence of different oxide phases that were not seen by conventional SEM investigation. The nature of these oxides phases seems to change upon hydrogenation/dehydrogenation cycle. This indicates that oxide phases may play a more significant role in the hydrogen absorption as what was previously believed. Full article

The experimental and theoretical study of the influence of metal complexing on geometry, aromaticity, chirality, and the ability to twist the nematic phase by complexes based on modified natural chlorin e6 was carried out. The geometry optimization of the chlorin e6 13(N)-methylamide-15,17-dimethyl ester (MADMECl) and its Zn, Cu, and Ni complexes by DFT (CAM-B3LYP/6–31 G(d,p) functional) method was performed. Based on these calculations, the acoplanarity degree of the macrocyclic ligand and the distortion energy of its dianion were estimated, which allowed the arrangement of the MADMECl complexes in the series Ni > Cu > Zn. Aromaticity was evaluated using the NICS criterion (nuclear independent chemical shift). An increase in the degree of aromaticity of the macrocycle upon complex formation was established. At the same time, the aromaticity of the inner conjugation contour corresponds to the same series as the acoplanarity, while the outer π-delocalization is characterized by the reverse sequence. An experimental evaluation of the electron circular dichroism of the Soret and the Q-bands, as well as the g-factor of dissymmetry, was carried out. The growth of these parameters with an increase in the degree of acoplanarity and aromaticity of the internal conjugation contour was determined. The induction of helical phases in mixtures of nematic liquid crystals (LCs) based on cyanobiphenyls and MADMECl macrocyclic metal complexes was studied by polarization microscopy, and the clearance temperatures and helix pitch of the mesophases were measured. A strong effect of the metal on the phase transition temperature and helical twisting power was established. Full article

Pollution of the aquatic environment by halogen derivatives widely used as antiseptic compounds, as well as chemicals for various industrial purposes, is significant. Existing systems of bioremediation poorly solve the problem of eliminating pollution. This paper discusses the preparation of novel macroporous chitosan-based cryogels with in situ-immobilized Pd or Pt nanoparticles as a catalyst for dichlorination reactions. The formation mechanism of metal coordinated chitosan gels using Medusa software modelling and rheology (G’ and G’’) is discussed. Metal coordinated chitosan gels were subsequently converted into covalently cross-linked macroporous cryogels with in situ-immobilized Pd or Pt nanoparticles using the redox potentials difference of the reaction mixture. Noble metal nanoparticles of average size, 2.4 nm, were evenly distributed in the cryogel structure. The effectiveness of these gels as a catalyst for the decomposition of chloro-compounds o-chlorophenol, p-chlorophenol and 2,4-dichlorophenol was tested. The catalytic hydrogenation reaction was carried out using the “green reducing agent” formic acid. Increasing the excess of formic acid with heating increases the degree of conversion up to 80–90%. The CHI-GA-PdNPs cryogel at pH 6 showed better efficiency in the hydrogenation process compared to the CHI-GA-PtNPs cryogel; however, no significant difference in the degree of conversion at pH 3 was observed. The termination of a catalytic reaction in a batch mode have been studied. Several control tests were carried out to elucidate the mechanism of catalyst poisoning. The presented catalytic system may be of interest for studying reactions in a flow through mode, including the reactions for obtaining valuable chemicals. Full article

Zeolite Y, as a solid acid catalyst with excellent performance, is a landmark in petroleum refining and chemical industry production–especially in catalytic cracking reactions. Improving the SAR of Y zeolite, enriching its pore structure, and modifying it with heteroatoms can realize the multifunctional catalysis of Y zeolite, improve the application value of it, and then meet the demands of petroleum refining. In this review, the synthesis of Y zeolites with high SAR, multistage pores, and heteroatom modification is summarized. Full article

A new metal–organic framework {[Mn₄(Cx)₃(etdipy)₅]·2ClO₄}_n (1) was prepared via the complexation of manganese ion from a Mn(ClO₄)₂ source with 1,3-bis(carboxypropyl)tetramethyldisiloxane (Cx) and 1,2-di(4-pyridyl)ethylene (etdipy) in the presence of 2,4-lutidine as a deprotonating agent. The single-crystal X-ray diffraction analysis revealed a dense 3D framework structure. The presence in the structure of flexible tetramethyldisiloxane moieties, which tend to orient themselves at the interface with the air, gives the compound a highly hydrophobic character, as indicated by the result of the water vapor sorption analysis in the dynamic regime, as well as the shape and stability of the water droplet on the crystalline mass of the compound. The compound is an electrical insulator, and due to its hydrophobicity, this characteristic is unaffected by environmental dampness. The thermal analysis indicated thermal stability up to about 300 °C and an unusual thermal transition for an MOF structure, more precisely a glass transition at 24 °C, the latter also being attributed to the flexible segments in the structure. The magnetic studies showed dominant antiferromagnetic interactions along the metal ion chain in compound 1. Full article

In this study, we report the successful growth of single crystals of a magnetic Weyl semimetal candidate NdAlGe with the space group I4₁md. The crystals were grown using a floating-zone technique, which used five laser diodes, with a total power of 2 kW, as the heat source. To ensure that the molten zone was stably formed during the growth, we employed a bell-shaped distribution profile of the vertical irradiation intensity. After the nominal powder, crushed from an arc-melted ingot, was shaped under hydrostatic pressure, we sintered the feed and seed rods in an Ar atmosphere under ultra-low oxygen partial pressure (<10⁻²⁶ atm) generated by an oxygen pump made of yttria-stabilized zirconia heated at 873 K. Single crystals of NdAlGe were successfully grown to a length of 50 mm. The grown crystals showed magnetic order in bulk at 13.5 K. The fundamental physical properties were characterized by magnetic susceptibility, magnetization, specific heat, thermal expansion, and electrical resistivity measurements. This study demonstrates that the magnetic order induces anisotropic magnetoelasticity, magneto-entropy, and charge transport in NdAlGe. Full article

The surface modification of textile fabrics and therefore, the development of advanced textile materials featuring specific implemented and new properties, such as improved durability and resistance, is increasingly in demand from modern society and end-users. In this regard, the sol–gel technique has shown to be an innovative and convenient synthetic route for developing functional sol–gel coatings useful for the protection of textile materials. Compared with the conventional textile finishing process, this technique is characterized by several advantages, such as the environmentally friendly approaches based on one-step applications and low concentration of non-hazardous chemicals. The sol–gel method, starting from inorganic metal alkoxides or metal salts, leads to inorganic sols containing particles that enable a chemical or physical modification of fiber surfaces, giving rise to final multifunctional properties of treated textile fabrics. This review considered the recent developments in the synthesis of inorganic nanoparticles and nanosols by sol–gel approach for improving wear and UV resistance, as well as antibacterial or antimicrobial effects for textile applications. Full article

A novel approach was carried to prepare trans-CuCl₂L₂ complex with the ligand L, (E)-(4-chlorophenyl)-N-(3-phenyl-4H-1,2,4-triazol-4-yl)methanimine which was formed in situ during the reaction of CuCl₂ with 4-(4-chlorobenzylideneamino)-5-phenyl-2H-1,2,4-triazole-3(4H)-thione. The synthesized compounds were characterized by applying various spectroscopic techniques. The crystal structure of the complex was unambiguously determined using X-ray analysis indicating square planar geometry. Intermolecular H-bonds govern the supramolecular structure of the copper complex. Aromatic rings are stacked in an offset packing due to occurrence of π–π interactions. The structure is further corroborated with a detailed computational investigation. A thione–thiol tautomerism for the triazole compound was also studied. The Schiff base 1,2,4-triazole copper chloride complex is expected to have high anticancer activity. Full article

The discovery of new inorganic magnesium electrolytes may act as a foundation for the rational design of novel types of solid-state batteries. Here we investigated a new type of organic-inorganic metal hydride, isopropylamine magnesium borohydride, Mg(BH₄)₂∙(CH₃)₂CHNH₂, with hydrophobic domains in the solid state, which appear to promote fast Mg²⁺ ionic conductivity. A new synthetic strategy was designed by combination of solvent-based methods and mechanochemistry. The orthorhombic structure of Mg(BH₄)₂∙(CH₃)₂CHNH₂ was solved ab initio by the Rietveld refinement of synchrotron X-ray powder diffraction data and density functional theory (DFT) structural optimization in space group I2₁2₁2₁ (unit cell, a = 9.8019(1) Å, b = 12.1799(2) Å and c = 17.3386(2) Å). The DFT calculations reveal that the three-dimensional structure may be stabilized by weak dispersive interactions between apolar moieties and that these may be disordered. Nanoparticles and heat treatment (at T > 56 °C) produce a highly conductive composite, σ(Mg²⁺) = 2.86 × 10⁻⁷, and 2.85 × 10⁻⁵ S cm⁻¹ at −10 and 40 °C, respectively, with a low activation energy, E_a = 0.65 eV. Nanoparticles stabilize the partially eutectic molten state and prevent recrystallization even at low temperatures and provide a high mechanical stability of the composite. Full article