Search

This research investigates the potential of mechanosynthesis to transform inert waste mixtures into sustainable construction materials. Three waste streams were employed: recycled glass, recycled concrete, and excavated soils. Two alternative material formulations, F1 (50% recycled concrete, 30% recycled glass, 20% excavated soil) and F2 (60% excavated soil, 20% recycled concrete, 20% recycled glass), were developed. Cement pastes were produced by partially substituting cement (CEM I) with 50% of either F1 or F2. Characterization techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (ATR-FTIR), and mechanical testing, were performed. Cement pastes incorporating milled waste materials exhibited significantly enhanced compressive strength compared to their unmilled counterparts. At 28 curing days, compressive strengths reached 44, 47, 45, and 49.7 MPa, and at 90 curing days, they increased to 47.5, 50, 55, and 61 MPa for milling conditions of 200 rpm for 5 min, 200 rpm for 15 min, 400 rpm for 5 min, and 400 rpm for 15 min, respectively. In addition, F1 formulations showed higher compressive strengths than the reference CEM II and CEM III pastes. These results highlight the efficacy of mechanosynthesis in valorizing construction waste, mitigating CO2 emissions, and creating environmentally friendly construction materials. [ABSTRACT FROM AUTHOR]

This study compares the structural, microstructural, thermal, and mechanical properties of geopolymer pastes (GPs) created through traditional methods and those derived from ready-to-use powders for geopolymer (RUPG) materials. The metakaolin (MK) precursor was activated using a sodium silicate solution or CaO and MOH (where M is Na or K). Various ratios of precursor/activator and Na2SiO3 or CaO/MOH were tested to determine the optimal combination. For RUPG, the MK precursor was activated by replacing the sodium silicate solution with quicklime. Metakaolin, alkaline hydroxide, and quicklime powders were mixed at different CaO ratios (wt%) and subjected to extensive ball milling to produce RUPG. The RUPG was then hydrated, molded, and cured at 20 °C and 50% relative humidity until testing. Analytical methods were used to characterize the raw and synthesized materials. Classic geopolymers (CGPs) activated with quicklime burst after one hour of molding. The results indicated slight amorphization of GP compared to raw MK, as confirmed by X-ray diffraction analysis, showing N(K)-A-S-H in CGP and N(K)-A-S-H with calcium silicate hydrate (C-S-H/C-A-S-H) in RUPG. The compressive strength of MK-based geopolymers reached 31.45 MPa and 34.92 MPa for GP and CGP, respectively, after 28 days of curing. [ABSTRACT FROM AUTHOR]

Lead‐free metal halide perovskites can potentially be air‐ and water‐stable photocatalysts for organic synthesis, but there are limited studies on them for this application. Separately, machine learning (ML), a critical subfield of artificial intelligence, has played a pivotal role in identifying correlations and formulating predictions based on extensive datasets. Herein, an iterative workflow by incorporating high‐throughput experimental data with ML to discover new lead‐free metal halide perovskite photocatalysts for the aerobic oxidation of styrene is described. Through six rounds of ML optimization guided by SHapley Additive exPlanations (SHAP) analysis, BA2CsAg0.95Na0.05BiBr7 as a photocatalyst that afforded an 80% yield of benzoic acid under the standard conditions is identified, which is a 13‐fold improvement compared to the 6% with when using Cs2AgBiBr6 as the initial photocatalyst benchmark that is started. BA2CsAg0.95Na0.05BiBr7 can tolerate various functional groups with 22 styrene derivatives, highlighting the generality of the photocatalytic properties demonstrated. Radical scavenging studies and density functional theory calculations revealed that the formation of the reactive oxygen species superoxide and singlet oxygen in the presence of BA2CsAg0.95Na0.05BiBr7 are critical for photocatalysis. [ABSTRACT FROM AUTHOR]

Nowadays high entropy carbides (HECs) are an important group of advanced ceramics. They are composed by at least by five transition metals (TMs) in nearly equiatomic proportion and disordered distributed in the cationic sublattice of face centered cubic structures, with carbon atoms in the octahedral interstitial voids, with general formula (TM1,TM2,TM3,TM4,TM5)C. These HECs belong to the recent novel group of ultra-high temperature ceramics (UHTCs), with superior properties in comparison with the constituent binary carbides. However, the synthesis of those HECs can be modified to develop high entropy carbonitrides, HECNs, where the C are partially substituted by N, to form a solid solution in the anionic sublattice, with expected improved properties as UHTCs, but they are in an incipient state of development. Here, we report the synthesis and deep characterization of a non-previously obtained Hf 0.2 Nb 0.2 Ta 0.2 V 0.2 Zr 0.2 C 0.5 N 0.5 HECN, via a facile, single step and reproducible solid-gas reaction mechanosynthesis route. The synthesis was successfully completed in a planetary ball mill device, after 2h of milling time, at 400 rpm and using a ball-to- powder ratio of 60:1 in a pure N 2 atmosphere at room temperature. The as-synthesized HECNs powdered showed nanostructured morphology and outstanding high-temperature oxidation resistance up to 1500 °C. [ABSTRACT FROM AUTHOR]

Abstract Lead‐free metal halide perovskites can potentially be air‐ and water‐stable photocatalysts for organic synthesis, but there are limited studies on them for this application. Separately, machine learning (ML), a critical subfield of artificial intelligence, has played a pivotal role in identifying correlations and formulating predictions based on extensive datasets. Herein, an iterative workflow by incorporating high‐throughput experimental data with ML to discover new lead‐free metal halide perovskite photocatalysts for the aerobic oxidation of styrene is described. Through six rounds of ML optimization guided by SHapley Additive exPlanations (SHAP) analysis, BA2CsAg0.95Na0.05BiBr7 as a photocatalyst that afforded an 80% yield of benzoic acid under the standard conditions is identified, which is a 13‐fold improvement compared to the 6% with when using Cs2AgBiBr6 as the initial photocatalyst benchmark that is started. BA2CsAg0.95Na0.05BiBr7 can tolerate various functional groups with 22 styrene derivatives, highlighting the generality of the photocatalytic properties demonstrated. Radical scavenging studies and density functional theory calculations revealed that the formation of the reactive oxygen species superoxide and singlet oxygen in the presence of BA2CsAg0.95Na0.05BiBr7 are critical for photocatalysis.

Binary mixtures of active pharmaceutical ingredients (API) are researched to improve the oral bioavailability of pharmaceutical dosage forms. The purpose of this study was to obtain mixtures of meloxicam and L-tartaric acid because tartaric acid improves intestinal absorption and meloxicam is more soluble in a weakly basic environment. The mixtures in the 0–1 molar fraction range, obtained from solvent-assisted mechanosynthesis, were investigated by differential scanning calorimetry (DSC), Fourier Transform Infrared (FTIR) spectroscopy, Fourier Transform Raman spectroscopy (FT-Raman), X-ray powder diffraction (XRD) and solubility tests. The physicochemical characteristics of the compounds obtained from DSC data reveal, for the first time, the formation of a co-crystal at meloxicam molar fraction of 0.5. FTIR spectroscopy data show the existence of hydrogen bonds between the co-crystal components meloxicam and L-tartaric acid. FT-Raman spectroscopy was used complementary with FT-IR spectroscopy to analyze the pure APIs and their mixtures, to emphasize the appearance/disappearance and the shifts of the position/intensity of vibrational bands, following the formation of hydrogen-bonded structures or van der Waals interactions, and to especially monitor the crystal lattice vibrations below 400 cm−1. The experimental results obtained by X-ray powder diffraction confirmed the formation of the co-crystal by the loss and, respectively, the apparition of peaks from the single components in the co-crystal diffractogram. The solubility tests showed that the co-crystal product has a lower aqueous solubility due to the acidic character of the other component, tartaric acid. However, when the solubility tests were performed in buffer solution of pH 7.4, the solubility of meloxicam from the co-crystal mixture was increased by 57% compared to that of pure meloxicam. In conclusion, the studied API mixtures may be considered potential biomaterials for improved drug release molecular solids. [ABSTRACT FROM AUTHOR]

Polyvinyl chloride (PVC) plays an important role in industry; however, due to its uncontrolled accumulation in the environment, the methods for its utilization are of high demand. Herein we wish to report an approach for the utilization of PVC via its use as a carrier for some azole-based drugs, such as 2-mercaptobenzothiazole (multi-activity drug), 4-oxo-1,4-dihydropyrazolo[5,1-c]-1,2,4-triazine-3,8-dicarboxylic acid diethyl ester (antidiabetic drug) and 5-methyl-6-nitro-7-oxo-1,2,4-triazolo[1,5-a]pyrimidinide (antiviral drug). The abovementioned approach involves the reaction between PVC and potassium or sodium salts of these azole-based drugs either in solution or under ball-milling conditions. The as-obtained PVCs modified with azole-based drugs were isolated for the first time and characterized by means of 1H NMR-spectroscopy as well as gel-permeation chromatography (GPC).

This research investigates the potential of mechanosynthesis to transform inert waste mixtures into sustainable construction materials. Three waste streams were employed: recycled glass, recycled concrete, and excavated soils. Two alternative material formulations, F1 (50% recycled concrete, 30% recycled glass, 20% excavated soil) and F2 (60% excavated soil, 20% recycled concrete, 20% recycled glass), were developed. Cement pastes were produced by partially substituting cement (CEM I) with 50% of either F1 or F2. Characterization techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (ATR-FTIR), and mechanical testing, were performed. Cement pastes incorporating milled waste materials exhibited significantly enhanced compressive strength compared to their unmilled counterparts. At 28 curing days, compressive strengths reached 44, 47, 45, and 49.7 MPa, and at 90 curing days, they increased to 47.5, 50, 55, and 61 MPa for milling conditions of 200 rpm for 5 min, 200 rpm for 15 min, 400 rpm for 5 min, and 400 rpm for 15 min, respectively. In addition, F1 formulations showed higher compressive strengths than the reference CEM II and CEM III pastes. These results highlight the efficacy of mechanosynthesis in valorizing construction waste, mitigating CO2 emissions, and creating environmentally friendly construction materials.

This study compares the structural, microstructural, thermal, and mechanical properties of geopolymer pastes (GPs) created through traditional methods and those derived from ready-to-use powders for geopolymer (RUPG) materials. The metakaolin (MK) precursor was activated using a sodium silicate solution or CaO and MOH (where M is Na or K). Various ratios of precursor/activator and Na2SiO3 or CaO/MOH were tested to determine the optimal combination. For RUPG, the MK precursor was activated by replacing the sodium silicate solution with quicklime. Metakaolin, alkaline hydroxide, and quicklime powders were mixed at different CaO ratios (wt%) and subjected to extensive ball milling to produce RUPG. The RUPG was then hydrated, molded, and cured at 20 °C and 50% relative humidity until testing. Analytical methods were used to characterize the raw and synthesized materials. Classic geopolymers (CGPs) activated with quicklime burst after one hour of molding. The results indicated slight amorphization of GP compared to raw MK, as confirmed by X-ray diffraction analysis, showing N(K)-A-S-H in CGP and N(K)-A-S-H with calcium silicate hydrate (C-S-H/C-A-S-H) in RUPG. The compressive strength of MK-based geopolymers reached 31.45 MPa and 34.92 MPa for GP and CGP, respectively, after 28 days of curing.

This article details work performed on the synthesis and characterization of an inorganic mixed‐cation double halide perovskite, Cs2Ag.6Na.4In.85Bi.15Cl6 (CANIBIC). Single crystals have been created via a hydrothermal reaction, milled into a powder, and pressed into pellets, while nanocrystals have been directly synthesized via mechanosynthesis. A computational model is constructed to predict the X‐ray diffraction pattern of CANIBIC; this model aligns very well with the X‐ray diffraction pattern measured for CANIBIC crystal powder. This model can therefore be developed in the future as a tool to predict lattice parameters and crystal structures of other novel double‐halide perovskites. Photoluminescence spectra obtained from each format show broad emission centered at 630 nm, as is typical for self‐trapped exciton emission; self‐trapped exciton emission is also confirmed by investigating photoluminescence intensity as a function of laser power. Nanocomposites are produced via the loading of nanocrystals of CANIBIC into PMMA. Although nanocomposite disks consisting of a small proportion of CANIBIC nanocrystals in PMMA have a smaller mass attenuation coefficient than a pressed pellet of CANIBIC, these disks have comparatively bright radioluminescence due to their optical transparency. These nanocomposite disks are therefore a particularly useful format for the practical use of the CANIBIC scintillator. [ABSTRACT FROM AUTHOR]

Herein, thermodynamic assessment is proposed to screen suitable precursors for the solid-state synthesis of manganese ferrite, by mechanosynthesis at room temperature or by subsequent calcination at relatively low temperatures, and the main findings are validated by experimental results for the representative precursor mixtures MnO + FeO3, MnO2 + Fe2O3, and MnO2 +2FeCO3. Thermodynamic guidelines are provided for the synthesis of manganese ferrite from (i) oxide and/or metallic precursors; (ii) carbonate + carbonate or carbonate + oxide powder mixtures; (iii) other precursors. It is also shown that synthesis from metallic precursors (Mn + 2Fe) requires a controlled oxygen supply in limited redox conditions, which is hardly achieved by reducing gases H2/H2O or CO/CO2. Oxide mixtures with an overall oxygen balance, such as MnO + Fe2O3, act as self-redox buffers and offer prospects for mechanosynthesis for a sufficient time (>9 h) at room temperature. On the contrary, the fully oxidised oxide mixture MnO2 + Fe2O3 requires partial reduction, which prevents synthesis at room temperature and requires subsequent calcination at temperatures above 1100 °C in air or in nominally inert atmospheres above 750 °C. Oxide + carbonate mixtures, such as MnO2 +2FeCO3, also yield suitable oxygen balance by the decomposition of the carbonate precursor and offer prospects for mechanosynthesis at room temperature, and residual fractions of reactants could be converted by firing at relatively low temperatures (≥650 °C). [ABSTRACT FROM AUTHOR]

Functional nano-fillers are commonly used to reduce bacterial colonization in dentistry. This study aimed to synthesize, characterize, and evaluate the biological effects of magnesium oxide (MgO) nanoparticles (NP) obtained by mechanosynthesis. XRD, TEM, FT-IR, and UV-Vis were used to characterize MgO-NP which were subsequently tested for their activity against Staphylococcus aureus, Enterococcus faecalis and Escherichia coli (E. coli). The effects of MgO-NP on osteoblast cells were also analyzed. Three variables were studied: microbial inhibition by optical density (OD; 570-nm), viability estimated by colony-forming-units, and cell proliferation. The characterization of NP is consistent with nanostructures, minimum inhibitory concentration between 1.5-5 mg/mL, and microbial inhibition at 9.75 ug/mL concentration for E. coli were determined. There were different concentration-dependent effects on cell proliferation. Results were observed with 0.156 mg/mL MgO-NP, which increased cell proliferation at 24 and 48 h. The results suggest the antibacterial suitability of MgO-NP, with tolerable viability of mammalian cells for dental applications. [ABSTRACT FROM AUTHOR]

The electrocatalytic activity of a number of mechanically activated/mechanically alloyed carbide phases of iron and tungsten and Fe3W3C and Fe6W6C bimetallic carbides in the evolution of hydrogen has been studied. Electrocatalysts have been prepared by compacting carbide particles with polyaniline as a conducting polymer. The highest activity is exhibited by Fe3C and WC nanocrystalline particles. Metallic phases in the composition of the particles slow down the rate of hydrogen evolution. Subsequent annealing of these particles transforms metallic phases to bimetallic carbides and accelerates the hydrogen evolution. The activity of the phases of Fe3W3C and Fe6W6C bimetallic carbides in the hydrogen evolution is fairly high, but they are inferior to the Fe3C and WC nanocrystalline particles. [ABSTRACT FROM AUTHOR]

Transformations in the S–AgNO3–NH4X–NH4NO3 (X = Cl, Br, I) system show that nanoparticles and nanocomposites with a controlled size of particles and content of components can be synthesized via mechanical treatment and adding small amounts of a liquid in which the precursors are soluble. Nanoparticles form in a dimethyl sulfoxide (DMSO) medium through conventional (continuous dissolution–crystallization) or reactive means (continuous dissolution of precursors and their reacting with subsequent crystallization of the target product), rather than by direct mechanical activation. The first version is used for synthesizing sulfur nanoparticles (nanosulfur); the second, for synthesizing silver halides. Sulfur-containing S/AgX nanocomposites with a controlled content of sulfur are synthesized mechanochemically. A predetermined content of nanosulfur in the nanocomposites is obtained via the dissolution–crystallization (recrystallization) of sulfur in DMSO inside a mechanochemical reactor. The proposed technical solution allows the synthesis of S/AgX nanocomposites through processing AgNO3, NH4X, and NH4NO3 (diluent) precursors, commercial sulfur, and small amounts of DMSO in planetary ball mills with different fittings. The water-soluble components of the product of mechanosynthesis are readily washed off. [ABSTRACT FROM AUTHOR]

Cyanide ions are known to be lethal for insects and mammals and harmful for the environment, and new methods for their selective detection are in high demand. Herein, the mechanosynthesis of simple Schiff’s bases-based probes S1–S3 for visual detection of CN− anion is reported. These probes were obtained by means of a reaction between isomeric 4,4-, 3,3- and 2,2-diaminobiphenyls and 4-nitrobenzaldehyde under ball milling conditions. The probes showed high selectivity and sensitivity toward CN− anion via a dramatic “yellow-to-dark purple” color change with a detection limit of 26 × 103, 8.7 × 103 and 14 × 103 ppm for S1–S3, respectively. The proposed mechanism of the detection suggests the deprotonation of a proton from an imine moiety, followed by the formation of charge transfer complexes (CTC).

Binary mixtures of active pharmaceutical ingredients (API) are researched to improve the oral bioavailability of pharmaceutical dosage forms. The purpose of this study was to obtain mixtures of meloxicam and L-tartaric acid because tartaric acid improves intestinal absorption and meloxicam is more soluble in a weakly basic environment. The mixtures in the 0–1 molar fraction range, obtained from solvent-assisted mechanosynthesis, were investigated by differential scanning calorimetry (DSC), Fourier Transform Infrared (FTIR) spectroscopy, Fourier Transform Raman spectroscopy (FT-Raman), X-ray powder diffraction (XRD) and solubility tests. The physicochemical characteristics of the compounds obtained from DSC data reveal, for the first time, the formation of a co-crystal at meloxicam molar fraction of 0.5. FTIR spectroscopy data show the existence of hydrogen bonds between the co-crystal components meloxicam and L-tartaric acid. FT-Raman spectroscopy was used complementary with FT-IR spectroscopy to analyze the pure APIs and their mixtures, to emphasize the appearance/disappearance and the shifts of the position/intensity of vibrational bands, following the formation of hydrogen-bonded structures or van der Waals interactions, and to especially monitor the crystal lattice vibrations below 400 cm−1. The experimental results obtained by X-ray powder diffraction confirmed the formation of the co-crystal by the loss and, respectively, the apparition of peaks from the single components in the co-crystal diffractogram. The solubility tests showed that the co-crystal product has a lower aqueous solubility due to the acidic character of the other component, tartaric acid. However, when the solubility tests were performed in buffer solution of pH 7.4, the solubility of meloxicam from the co-crystal mixture was increased by 57% compared to that of pure meloxicam. In conclusion, the studied API mixtures may be considered potential biomaterials for improved drug release molecular solids.

Cyanide ions are known to be lethal for insects and mammals and harmful for the environment, and new methods for their selective detection are in high demand. Herein, the mechanosynthesis of simple Schiff's bases-based probes S1–S3 for visual detection of CN− anion is reported. These probes were obtained by means of a reaction between isomeric 4,4-, 3,3- and 2,2-diaminobiphenyls and 4-nitrobenzaldehyde under ball milling conditions. The probes showed high selectivity and sensitivity toward CN− anion via a dramatic "yellow-to-dark purple" color change with a detection limit of 26 × 103, 8.7 × 103 and 14 × 103 ppm for S1–S3, respectively. The proposed mechanism of the detection suggests the deprotonation of a proton from an imine moiety, followed by the formation of charge transfer complexes (CTC). [ABSTRACT FROM AUTHOR]

The manganese ferrite has been processed by mechanosynthesis, using reactive siderite and MnO 2 powder mixtures, with and without subsequent heat treatment. Taguchi planning was used to assess the impact of milling conditions (rotational speed and time) and subsequent calcination temperature on conversion of precursors, based on integrated intensities of the main XRD peaks of precursor phases FeCO 3 (104) and MnO 2 (110), and spinel phase (311), using Ni as internal pattern. Thermogravimetry provided additional information on the residual contents of reactants in the as-milled samples. The best conditions for complete conversion to spinel phase of as-milled samples were obtained by milling at 650 rpm, for 6 h ( I 311 , s p / I 111 , N i = 2.41) , and for calcined samples were obtained after milling at 650 rpm, for 3 h, and calcination at 650 °C (I 311 , s p / I 111 , N i = 2.35). The impact of processing conditions on structural features of the spinel phase was accounted by the contributions to variance of intensity of its (311) reflection, which were 90% ascribed to rotational speed and only 4% ascribed to milling time, for as-milled samples, or 58%, 15% and 16% ascribed to rotational speed, milling time and calcination temperature, for calcined samples. Readier conversion of FeCO 3 relative to MnO 2 occurred during the milling stage, at low or intermediate rotational speed, with impact on M n : F e ratio in the spinel phase, as revealed by changes in lattice parameter of as-milled samples, in the range of 0.8424–0.8464 nm. Subsequent calcination minimized or eliminated traces of secondary phases. The incorporation of magnesium oxide and possibly other secondary components of the siderite precursor also induced structural changes in the resulting spinel phase, mainly in calcined samples (a o = 0.8370–0.8434 nm). Partial oxidation also contributed to structural changes in calcined samples, as revealed by differences between samples calcined in inert and oxidising atmospheres. [ABSTRACT FROM AUTHOR]

The synthesis of cobalt hydroxysilicate Co3(Si2O5)2(OH)2 in a matrix of high dispersity amorphous silica has been proposed. It is shown the formation of a hydroxosilicate, which combines coordinated silica and cobalt-oxygen polyhedrons in the overall structure, as well as the availability of surface hydroxyl groups, contribute to the preservation of a high specific surface area as is in amorphous SiO2. The hydroxosilicate also contributes to the effective manifestation of photocatalytic properties due to the presence of cobalt (2+), which has a high reactivity. As methods of synthesis of SiO2/Сo composites hydrochemical methods are used by impregnation and autoclave treatment with solution of cobalt formate of silica. The influence of the amount of introduced cobalt on the composition, structure, and properties of a composite material containing Co3(Si2O5)2(OH)2 in a SiO2 matrix has been traced. SiO2/Co composites have been tested in the hydroquinone photooxidation reaction when exposed to ultraviolet radiation. The highest degree of hydroquinone decomposition amounting to 84% in 18 hours was achieved for SiO2/Co at a molar ratio of components Co:Si = 0.01:1.

Rhodamine‐based chromic materials have attracted significant interest owing to their cation recognition ability with high sensitivity. However, rhodamine chromophores with controllable sensing selectivity towards transition metal species are only at the advent. Herein, three triazole‐conjugated rhodamine dyads with different peripheral substituents were synthesized. The key triazole precursors required for the desired chemistry were prepared by adopting our recently developed CTAB catalyzed mechano‐click chemistry. Molecular properties derived from photophysics, electrochemistry and surface morphology of the synthesized dyads were analyzed. Furthermore, frontier molecular orbitals, electronic structure and secondary quantum chemical parameters of dyads were also compared. Screening of dyads for their sensing ability towards an array of alkali, alkaline and transition metal ions exhibited a noticeable naked‐eye detection of Cu2+ ions and was confirmed by spectrophotometric titration. The specific binding mode of dyads as probable with Cu2+ over other metal ions attributes to the chemoselectivity. [ABSTRACT FROM AUTHOR]

The present work describes the removal of Rhodamine B (Rh B), a model of organic dye, from aqueous solution by Sono-assisted catalytic process on magnesium oxide- iron (MgO–Fe) nanostructures as catalyst. This material was prepared by high-energy ball milling method and characterized by X-ray diffractometer (XRD), scanning electron microscope (SEM) coupled with EDS analyzer, specific surface analysis determined from by BET analysis and FTIR spectroscopy. The XRD patterns show the formation of the MgFe2O4 phase, which presents a face-centred cubic lattice after 1 h of milling. The BET surface area and total pore volume of the spinel were found to be 60 m2/g and 61cm3. The SEM micrographs show that the particles size is between 50 and 100 μm. The best sonocatalytic degradation of Rh B was obtained with MgO–Fe at 12 h of grinding with an almost complete Rh B degradation in 240 min. irradiation time. The results clearly demonstrated the applicability of this MgO–Fe catalyst for the sono-catalytic oxidation of Rh B (10 mg /L). The Rh B mineralization was confirmed by Chemical Oxygen Demand (COD) and High-Performance Liquid Chromatography (HPLC) analysis. [ABSTRACT FROM AUTHOR]

The effect of the action of temperature on the structure and phase composition of an Fe3C/Fe7C3/P-phase/Cam composite obtained by mechanosynthesis of Fe–75 at % C has been studied by the methods of X‑ray diffraction, Mössbauer spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. It is shown that the structural and phase changes at heating have a multistage character. In the temperature range 315–400°C crystallization of the paramagnetic P-phase with generation of Fe3C and/or Fe7C3 occur. In the course of heating to higher temperatures, complete decomposition of carbide Fe7C3 (in the range 450–550°C) and partial decomposition of Fe3C (at 600°C and above) are observed. After cooling from 800–1000°C the mechanocomposite consists of α-Fe, cementite Fe3C, and graphite. The phase transformations are accompanied by the processes of composite oxidation with the formation of Fe3O4 oxide and its subsequent reduction. The P-phase is a disorded amorphous carbide Fe1 – xCx, which is characterized by magnetic ordering at the temperature of liquid nitrogen. [ABSTRACT FROM AUTHOR]

X-ray, Mössbauer, and magnetic methods have been used to determine the structural-phase state of nanocomposites—carbide steels doped with chromium and nickel (Fe0.90 –xMn0.10Nix)83C17, where x = 0.05 and 0.10, obtained by mechanosynthesis followed by annealings. The magnetic (para- or ferro-) states of the phases and their influence on the formation of magnetic hysteresis properties of carbide steels have been studied. [ABSTRACT FROM AUTHOR]

In this study, tantalum carbide (TaC) was synthesized using an innovative approach that synergistically integrates mechanosynthesis and electric arc furnace processes. By employing high-energy ball-milling (HEBM) for 50 min under environmental conditions, TaC-WC powders were successfully synthesized, using a powder mixture of tantalum and carbon in a 1:1 stoichiometric ratio. This method yielded a composition of 72.5 wt% TaC and 27.5 wt% WC, with an average particle size of 0.7 ± 0.3 μ m. The use of an electric arc furnace led to the fabrication of a highly dense material with a relative density above 98%. Notably, WC derived from the mechanical milling material served as an effective sintering aid. x-ray photoelectron Spectroscopy (XPS) results indicated the formation of metal oxides on the surface of the sample, and despite the presence of these oxides, the density of the material remained uncompromised. Furthermore, x-ray diffraction (XRD) analysis after the electric arc furnace treatment demonstrated the preservation of the TaC and WC phases. Mechanical properties, including Vickers hardness, Young’s modulus and fracture toughness were 22.8 ± 0.5 GPa under an applied load of 9.8 N, 539 GPa and 6.6 MPa m ^1/2 , respectively. The results underscore a novel and efficient synthesis route for TaC-WC with enhanced mechanical properties and high density, which are crucial aspects for applications in ultra-high temperature ceramics.

Herein, thermodynamic assessment is proposed to screen suitable precursors for the solid-state synthesis of manganese ferrite, by mechanosynthesis at room temperature or by subsequent calcination at relatively low temperatures, and the main findings are validated by experimental results for the representative precursor mixtures MnO + FeO3, MnO2 + Fe2O3, and MnO2 +2FeCO3. Thermodynamic guidelines are provided for the synthesis of manganese ferrite from (i) oxide and/or metallic precursors; (ii) carbonate + carbonate or carbonate + oxide powder mixtures; (iii) other precursors. It is also shown that synthesis from metallic precursors (Mn + 2Fe) requires a controlled oxygen supply in limited redox conditions, which is hardly achieved by reducing gases H2/H2O or CO/CO2. Oxide mixtures with an overall oxygen balance, such as MnO + Fe2O3, act as self-redox buffers and offer prospects for mechanosynthesis for a sufficient time (>9 h) at room temperature. On the contrary, the fully oxidised oxide mixture MnO2 + Fe2O3 requires partial reduction, which prevents synthesis at room temperature and requires subsequent calcination at temperatures above 1100 °C in air or in nominally inert atmospheres above 750 °C. Oxide + carbonate mixtures, such as MnO2 +2FeCO3, also yield suitable oxygen balance by the decomposition of the carbonate precursor and offer prospects for mechanosynthesis at room temperature, and residual fractions of reactants could be converted by firing at relatively low temperatures (≥650 °C).

Sugar amides, such as aldonamides, are interesting, sugar-based molecules used in various fields, from detergency to medicine. Nevertheless, their valorization, especially as alternatives to petroleum-based substances, can be slowed down by their synthetic pathway, which is generally not in accordance with green chemistry principles, and is also not economically competitive. We propose herein a fast procedure for the synthesis of aldonamide-derived glycoconjugates with mechanochemistry. The conditions were first optimized with galactonolactone, used as a model lactone, and dodecylamine. After only 5 min of grinding of stoechiometric amounts of amine and lactone, in the presence of water used as a Liquid Assisted Grinding (LAG) agent, the corresponding galactonamide was isolated with a high yield (90%) after a simple aqueous work-up. The optimized conditions were then applied to a wide variety of amines and sugar lactones, showing the versatility of the methodology. Gluco- and ribono-lactone exhibited similarly excellent reactivity, showing that the procedure is not sugar-dependent. Furthermore, the procedure was shown to be compatible with various functional groups such as alkene, alkyne, thiol, ester and hydroxyl.

Three efficient synthetic approaches towards new azomethine- and terpyridine-containing 2,5-dihydropyrrolo[3,4-c]pyrrole-1,4-dione (diketopyrrolopyrrole, DPP) based polymers, such as P1 and P2, are reported. The first approach involves the Pd-catalyzed synthesis via two- or three-component Suzuki or Stille cross-coupling reaction in solution. The second approach involves Pd-catalyzed Suzuki cross-coupling reaction under ball-milling conditions. And, finally, the third approach involves Pd-free condensation reaction under ball-milling conditions. The newly obtained polymers exhibited absorbance around 700 nm and emission around 900 nm, and, thus, these polymers are considered to be NIR-fluorophores.

Low temperature magnetic properties of BiFeO3 powders sintered by flash and spark plasma sintering were studied. An anomaly observed in the magnetic measurements at 250 K proves the clear existence of a phase transition. This transformation, which becomes less well-defined as the grain sizes are reduced to nanometer scale, was described with regard to a magneto-elastic coupling. Furthermore, the samples exhibited enhanced ferromagnetic properties as compared with those of a pellet prepared by the conventional solid-state technique, with both a higher coercivity field and remnant magnetization, reaching a maximum value of 1.17 kOe and 8.5 10−3 emu/g, respectively, for the specimen sintered by flash sintering, which possesses the smallest grains. The specimens also show more significant exchange bias, from 22 to 177 Oe for the specimen prepared by the solid-state method and flash sintering technique, respectively. The observed increase in this parameter is explained in terms of a stronger exchange interaction between ferromagnetic and antiferromagnetic grains in the case of the pellet sintered by flash sintering. [ABSTRACT FROM AUTHOR]

A green chemistry method was applied in the synthesis of N2,N6-bis(6-iodo-2-methyl-4-oxoquinazolin-3(4H)-yl)pyridine-2,6-dicarboxamide. The desired compound was synthesized mechanochemically, using a choline chloride-based deep eutectic solvent as a catalyst. The synthesis took 20 min and the new compound was characterized using different spectral methods. [ABSTRACT FROM AUTHOR]

In this work, we reported obtaining mesoporous Bi-doped TiO2 by mechanosynthesis and bismuth loading of 0%, 1%, 3%, 5%, and 10% (milled TiO2, TiO2 Bi 1%, TiO2 Bi 3% TiO2 Bi 5%, and TiO2 Bi 10%, respectively). The effect of bismuth doping and ball milling on the crystal structure, optical properties, and photocatalytic performance of Bi-doped TiO2 mesoporous samples under UV, visible, and sun irradiation was investigated. According to the results of the Rietveld refinement, the estimated chemical formulas for the TiO2 Bi 1%, TiO2 Bi 3%, TiO2 Bi 5%, and TiO2 Bi10% samples were Ti0.99Bi0.01O2, Ti0.97Bi0.03O2, Ti0.96Bi0.04O2, and Ti0.91Bi0.09O2 respectively. The incorporation of Bi into the TiO2 lattice causes the crystallite size to decrease and, consequently, the absorption spectrum of TiO2 to extend into the visible region of the electromagnetic spectrum, resulting in a lower band gap (Eg) value. Bi-doped TiO2 mesoporous samples had Eg values of 2.90 eV, 2.83 eV, 2.77 eV, and 2.70 eV for the TiO2 Bi 1%, TiO2 Bi 3%, TiO2 Bi 5%, and TiO2 Bi 10% samples, respectively. Photocatalytic removal of methylene blue (MB) data fit well for second-order kinetics. Photocatalytic activity increase followed the order of TiO2 Bi 5% > TiO2 Bi 10% > TiO2 Bi 3% > TiO2 Bi 1% > pristine TiO2. The TiO2 Bi 5% sample exhibited excellent photocatalytic performance for MB photodegradation under natural sunlight (89.2%). [ABSTRACT FROM AUTHOR]

Nanostructured materials containing nickel improve the effectiveness of several applications. This study examines the preparation and characterization of nanostructured Ni 80 Co 17 Mo 3 alloy powders using high-energy mechanical alloying and subsequent annealing. A 72 h milling process used pure elemental powders to synthesise nanocrystalline FCC-NiCo(Mo) solid solution. The milled powders were then subjected to annealing at different temperatures:300°C, 500°C, and 750°C. X-ray diffraction, scanning electron microscopy coupled with energy-dispersive spectroscopy, and vibrating sample magnetometry indicated significant changes in the powdered alloy properties. The particles growth occurred as the annealing temperature increased, while the microstrain decreased significantly; 14.30±0.07 nm up to 56.30±0.28 nm and 0.680±0.003 % up to 0.180±0.001 %, at 25°C and 750°C respectively. SEM analysis revealed differences in particle size and shape as milling progressed. Surprisingly, the milled powdered alloy displayed improved magnetic properties, manifesting significant magnetic susceptibility and enhanced saturation magnetisation, remanent magnetisation, and coercivity within the temperature range of 300°C to 750°C. These findings indicate the development of a consistent and structured state, accompanied by significant crystal growth due to the annealing temperature. This study highlights the great importance of high-energy mechanical milling and subsequent annealing to tune / tailor the characteristics and subsequently investigate the potential utilization of nanostructured Ni-based alloys. [Display omitted] • The Ni80Co17Mo3 solid phase with a face-centred cubic (FCC) structure was generated after 12 h of milling. • Temperature-Induced Microstructural Evolution • The magnetization of Ni80Co17Mo3 decreases gradually with increasing at Elevated Temperatures. • The presence of nanocrystalline defects, namely stacking faults, causes a decrease in Hc. • The nanostructured Ni80Co17Mo3 material has a very pliable magnetic behaviour after it reaches saturation. [ABSTRACT FROM AUTHOR]

A green chemistry method was applied in the synthesis of N2,N6-bis(6-iodo-2-methyl-4-oxoquinazolin-3(4H)-yl)pyridine-2,6-dicarboxamide. The desired compound was synthesized mechanochemically, using a choline chloride-based deep eutectic solvent as a catalyst. The synthesis took 20 min and the new compound was characterized using different spectral methods.

Lead-free ferroelectric Ba 0.85 Ca 0.15 Zr 0.1 Ti 0.9 O 3 stands out among environmentally friendly alternatives to commercial Pb(Zr,Ti)O 3 piezoceramics for its large piezoelectric coefficients, and it is especially suitable for applications in which thermal depoling is not an issue like bio-implanted devices. However, ceramic processing by conventional means consistently results in exaggerated grain growth, which compromises reliability and has prevented its transfer to industry. We report here the application of high-energy milling for the mechanosynthesis of nanocrystalline Ba 0.85 Ca 0.15 Zr 0.1 Ti 0.9 O 3 powders with enhanced reactivity, and to the control of grain growth during ceramic processing to obtain materials with tailored microstructures and decreasing grain sizes down to the sub-10 µm range. Characterization of the electrical and electromechanical properties was accomplished and uncovered triggering of a new mechanism for very large strain under electric field in fine-grained ceramics. Process optimization by precursor selection and preliminary up-scaling studies are also presented. [ABSTRACT FROM AUTHOR]

Sugar amides, such as aldonamides, are interesting, sugar-based molecules used in various fields, from detergency to medicine. Nevertheless, their valorization, especially as alternatives to petroleum-based substances, can be slowed down by their synthetic pathway, which is generally not in accordance with green chemistry principles, and is also not economically competitive. We propose herein a fast procedure for the synthesis of aldonamide-derived glycoconjugates with mechanochemistry. The conditions were first optimized with galactonolactone, used as a model lactone, and dodecylamine. After only 5 min of grinding of stoechiometric amounts of amine and lactone, in the presence of water used as a Liquid Assisted Grinding (LAG) agent, the corresponding galactonamide was isolated with a high yield (90%) after a simple aqueous work-up. The optimized conditions were then applied to a wide variety of amines and sugar lactones, showing the versatility of the methodology. Gluco- and ribono-lactone exhibited similarly excellent reactivity, showing that the procedure is not sugar-dependent. Furthermore, the procedure was shown to be compatible with various functional groups such as alkene, alkyne, thiol, ester and hydroxyl. [ABSTRACT FROM AUTHOR]

Mechanochemical synthesis of 2,5-disubstituted 1,3,4-oxadiazoles was developed as an environmentally benign alternative to conventional solvent-based methods. In the presence of triphenylphosphine and trichloroisocyanuric acid, N -acylbenzotriazoles condense with acylhydrazides leading to oxadiazoles derivatives in good to excellent yields within minutes. The approach circumvents the need for strictly anhydrous conditions, external heating, long reaction times, as well as tedious multistep procedures. A range of substrates with reactive functionalities was also well tolerated. [ABSTRACT FROM AUTHOR]

An Si/Cu composite anode was prepared using a facile solid mechanosynthesis method and wet chemical etching. Phase transition and morphologies were investigated on pristine and as-synthesized composites. Effects of presence of Al80Si20 and super p carbon on ball-milling were investigated. Moreover, the etching effect was compared with that of pristine Cu–Zn and composites by addition of NH4Cl. The results of X-ray diffraction patterns, scanning-electron-microscopy morphological images, and focus-ion-beam/energy-dispersive mapping demonstrated that the formation of the intermetallic, elemental distribution, homogeneity, and dezincification is involved with the addition of Al, super p carbon, and etching additive NH4Cl. Super p carbon avoided the formation of Cu–Si, while Al made the more homogenous distribution of Si/Cu. The two synthesized types of Si/Cu composites deliver specific capacity/retention rates of 608 mAhg−1/66.4% (Si/Cu from pure Si) and 707 mAhg−1/81.1% (Si/Cu from Al80Si20) after 200 cycles, respectively. The higher stability of the galvanostatic cycling and capability performance resulted from the homogeneity of Si and Cu.

Mechanochemistry uses mechanical force to break, form, and manipulate chemical bonds to achieve functional transformations and syntheses. Over the last years, many innovative applications of mechanochemistry have been developed. Specifically for the synthesis and activation of carbon‐rich π‐conjugated materials, mechanochemistry offers reaction pathways that either are inaccessible with other stimuli, such as light and heat, or improve reaction yields, energy consumption, and substrate scope. Therefore, this review summarizes the recent advances in this research field combining the viewpoints of polymer and trituration mechanochemistry. The highlighted mechanochemical transformations include π‐conjugated materials as optical force probes, the force‐induced release of small dye molecules, and the mechanochemical synthesis of polyacetylene, carbon allotropes, and other π‐conjugated materials. [ABSTRACT FROM AUTHOR]

Rational synthesis of hydrogen‐bonded organic frameworks (HOFs) with predicted structure has been a long‐term challenge. Herein, by using the efficient, simple, low‐cost, and scalable mechanosynthesis, we demonstrate that reticular chemistry is applicable to HOF assemblies based on building blocks with different geometry, connectivity, and functionality. The obtained crystalline HOFs show uniform nano‐sized morphology, which is challenging or unachievable for conventional solution‐based methods. Furthermore, the one‐pot mechanosynthesis generated a series of Pd@HOF composites with noticeably different CO oxidation activities. In situ DRIFTS studies indicate that the most efficient composite, counterintuitively, shows the weakest CO affinity to Pd sites while the strongest CO affinity to HOF matrix, revealing the vital role of porous matrix to the catalytic performance. This work paves a new avenue for rational synthesis of HOF and HOF‐based composites for broad application potential. [ABSTRACT FROM AUTHOR]

The possibility of obtaining polymer–drug conjugates as prolonged-action antibacterial systems by mechanochemical synthesis using the copolymer of maleic anhydride with vinyl acetate or oxidized potato starch as polymer matrices and sulfanilamide as the antimicrobial drug was studied. It is established that drug conjugation with the polymer results from covalent bonding, the degree of sulfanilamide conversion depends on the magnitude of active force and the time of the solid-phase reaction, and the product continues to accumulate after the load is removed. The conjugate with the polysaccharide matrix, from which the drug release due to cleavage of an azomethine bond was slower than its removal from the body if the initial dosage form was used, was most promising. [ABSTRACT FROM AUTHOR]

For the first time, a spinel-type high entropy oxide (Zn0.25Cu0.25Mg0.25Co0.25)Al2O4 as well as its derivative lithiated high entropy oxyfluoride Li0.5(Zn0.25Cu0.25Mg0.25Co0.25)0.5Al2O3.5F0.5 and oxychloride Li0.5(Zn0.25Cu0.25Mg0.25Co0.25)0.5Al2O3.5Cl0.5 are prepared in the nanostructured state via high-energy co-milling of the simple oxide precursors and the halides (LiF or LiCl) as sources of lithium, fluorine and chlorine. Their nanostructure is investigated by XRD, HR-TEM, EDX and XPS spectroscopy. It is revealed that incorporation of lithium into the structure of spinel oxide together with the anionic substitution has significant effect on its short-range order, size and morphology of crystallites as well as on its oxidation/reduction processes. The charge capacity of the as-prepared nanomaterials tested by cyclic voltammetry is found to be rather poor despite lithiation of the samples in comparison to previously reported spinel-type high entropy oxides. Nevertheless, the present work offers the alternative one-step mechanochemical route to novel classes of high entropy oxides as well as to lithiated oxyfluorides and oxychlorides with the possibility to vary their cationic and anionic elemental composition. [ABSTRACT FROM AUTHOR]

Nanostructured materials can show considerably different properties as compared to their coarse-grained counterparts. Especially prepared by high-energy ball milling they are to be characterized by a large fraction of point defects in the bulk and structurally disordered interfacial regions. Here, we explored how the overall conductivity of SmF3 can be enhanced by mechanical treatment and to which degree aliovalent substitution is able to further enhance anion transport. For this purpose nanocrystalline (hexagonal) SmF3 was prepared by high-energy ball milling; mechanosynthesis helped us to replace Sm3+ in SmF3 by Ba2+ and to create vacancies in the F anion sublattice. We observed a remarkable increase in total (direct current) conductivity when going from nano-SmF3 to Sm1−xBaxF3−x for x = 0.1. Electrical modulus spectroscopy was used to further characterize the corresponding increase in electrical relaxation frequencies. [ABSTRACT FROM AUTHOR]

In the first stage of this work, the master nanocomposite of niobium carbide (NbC)–Cu (ceramic‐based nanocomposite) was synthesized by a mechanically induced magnesiothermic combustion in the Nb2O5/CuO/Mg/C system. Ignition time in this system was recorded to be ∼28 min of milling. In the second stage, appropriate amounts of NbC–Cu nanocomposite powder were mixed with pure copper powder to prepare Cu‐based nanocomposite with 0, 5, 10, 15, and 20 volume fraction of NbC. The final metal matrix nanocomposite powder was sintered by spark plasma sintering method. The density of nanocomposite specimens decreased with increasing the percentage of NbC nanoparticles, while the microhardness of specimens increased with increasing nano‐NbC content. Regarding the tensile test, the sample Cu–10 vol.% NbC nanocomposite with a strength of 372 MPa (∼63% higher than that of nonreinforced copper) was the best composition, and the nanocomposite strength decreased at higher NbC concentrations, mostly due to the agglomeration and nonhomogeneous distribution of reinforcing nanoparticles. [ABSTRACT FROM AUTHOR]

Abstract—When studying the microstructure of carbon steel by the example of steel 10 and steel 45, inclusions of gold and silver were found on the surface hardened by shockwave deformation, which were confirmed by experimental and quantitative studies. The formation hypothesis of synthetic gold and silver in the structure of deformed steel is proposed on the basis of cold nuclear fusion (CNF) or low-energy nuclear reactions (LENR) in the deformation core zone. It is shown that the CNF nuclear chain reaction is triggered only when an amorphous core emerges in the deformation zone. The splitting of the amorphous steel structure into iron clusters and degenerate electron gas leads to a collapsing self-compression of the system due to the pressure of the degenerate electron gas and electromagnetic interaction of iron clusters. As a result of the collapse of iron clusters, the CNF of the gold and silver proceeds in them. The leading stage of iron-silver transmutation is shown. It was proved that in the process of silver CNF, an additional proton flux is introduced into the system that leads to their recombination with free electrons and the formation of a significant amount of hydrogen. Hydrogen saturation of the steel causes the well-known effect of anomalous spontaneous deformation of iron, which activates amorphization of steel in the core deformation zone accelerating the CNF process. The development of experimental studies to confirm the course of CNF in the processes of the shockwave deformation of steel during its surface hardening is shown. [ABSTRACT FROM AUTHOR]

Different stoichiometries of lead-free BaZr 0.2 Ti 0.8 O 3 –Ba 0.7 Ca 0.3 TiO 3 (BCZT) prepared by mechanosynthesis and sintered by either conventional sintering (CS) or hot pressing (HP) techniques were studied to establish the dependence of piezoelectric and dielectric properties on sintering parameters and microstructure. All synthesized stoichiometries showed a pseudocubic perovskite phase with homogeneously distributed A- and B-cations in the structure. The BCZT retained the pseudocubic symmetry after sintering and an average grain size <1.8 µm was obtained in all cases. HP sintering hindered the secondary phase segregation observed in the CS ceramics and increased the relative density. Piezoelectric coefficients (d 33) ranging from 5.1 to 21 pC/N and from 10.0 to 88.0 pC/N were obtained for CS and HP ceramics, respectively, despite the pseudocubic symmetry and the fine grain size. The higher d 33 values for the HP ceramics are a consequence of the higher density, better chemical homogeneity and lower sintering temperature and time required for the mechanosynthesized BCZT powders with high sintering activity. • BCZT were successfully formed by high-energy mechanosynthesis after 120 min. • Fine-grained BCZT were obtained by either conventional sintering or hot pressing. • HP sintering favored the presence of different crystal structures and higher density. • d 33 values ranged from 5.1 to 88.0 pC/N, depending on stoichiometry and sintering. [ABSTRACT FROM AUTHOR]

• This paper explored mechanosynthesis of anionic-substituted HA nanopowders. • Rietveld refinement was used to describe the structural features. • Insights into how milling time and dopants affect HA crystal structure were provided. • Particle morphology evolution during milling was observed in TEM analysis. • Intermediate phases emerged as a pivotal factor influencing the advancement of reactions. An investigation into the microstructural properties and mechanosynthesis mechanisms of three distinct calcium phosphate compounds, namely, carbonate-substituted hydroxyapatite (CHA), fluorapatite (FA), and carbonate- and fluoride-substituted hydroxyapatite (CFHA), was undertaken in this study. Significant insights into the crystalline structures of CHA, FA, and CFHA were revealed through Rietveld refinement analysis. In the CaCO 3 ‒Ca(OH) 2 ‒P 2 O 5 ternary system, the transformation of the biphasic structure composed of CHA and dicalcium phosphate anhydrous (DCPA) into a single-phase A-type CHA was observed as milling duration increased. In the CaO‒Ca(OH) 2 ‒CaF 2 ‒P 2 O 5 quaternary system, the formation of FA was influenced by milling time, and within 1‒5 h, a composite structure was formed. The progression from a composite structure to the formation of fully crystalline nanosized CFHA was also observed over the same milling periods in the CaCO 3 ‒Ca(OH) 2 ‒CaF 2 ‒P 2 O 5 quaternary system. The central finding highlights the substantial influence of milling time on the structural properties of the mechanosynthesized nanopowders, with marked changes in crystallite size, micro-strain, and unit cell volume being observed over different milling durations. The atomic coordinates and displacement parameters of the refined structures were also provided, revealing the presence of apatitic groups. Moreover, a detailed examination of the mechanochemical synthesis processes uncovered intricate sub-reactions that occur during ball milling. This work sets the stage for future investigations, facilitating a better grasp of their distinctive attributes and potential applications across various domains of regenerative medicine. [Display omitted] [ABSTRACT FROM AUTHOR]

[Display omitted] • Ball milling is a cost-effective, one-step, and solvent-free approach to preparing electrode materials and shows advantages such as no use of heat treatment, harmful solvents, long processes, and high energy consumption required by the common methods such as solvothermal, sol–gel, hydrothermal, and precipitation. • Functional materials applied in supercapacitors can be produced via planetary ball milling. • Transition metal carbonates and nanocomposite were mechanochemically synthesized without additional process. • MnCO 3 and CoCO 3 resulted in excellent performance in 1 M KOH electrolyte. • High storage, remarkable rate capability, and outstanding capacitance retention were achieved. Transition metals are known for their enormous potential as electrode materials for supercapacitor applications, however anhydrous carbonate minerals, namely Mn-carbonate, and Co-carbonate, are less explored and exhibit competitive energy storage performance compared to oxide and hydroxide forms. For the first time, MnCO 3 (Rhodochrosite), CoCO 3 (Spherocobaltite) and MnCo mixture (Mn 1-x Co x CO 3) were synthesized via mechanochemistry by a one-pot approach and used to prepare pseudocapacitive electrode materials for electrochemical energy storage. In this work, these materials were tested in alkaline electrolyte, and the morphological and structural features of the materials were examined using SEM (Scanning Electron Microscope), Transmission Electron Microscopy (TEM) and X-ray Diffraction (XRD). The surface composition was studied by X-ray photoelectron spectroscopy (XPS). After milling, the microstructures showed an increase in dislocations and microstrains in their crystal lattices which influenced the electrochemical performance. The crystallinity of the carbonate materials was also affected by grinding. In 1 M KOH electrolyte, milled MnCO 3 evidenced the highest specific capacitance (354.3 F/g at 1.0 A/g), while milled CoCO 3 , revealed impressive capacitance retention of 94.8 % after 20000 continuous charge–discharge cycles at 10 A/g. Interestingly, the composite (Mn-Co)CO 3 evidenced superior rate capability (58.8 %) and enhanced capacitance retention under cycling compared to the individual cobalt and manganese carbonates. The results evidence the excellent electrochemical behavior of Mn and Co carbonates prepared by a simple, low-cost, and green route and prove their potential as electroactive electrode materials for electrochemical energy storage applications, particularly pseudocapacitors. [ABSTRACT FROM AUTHOR]

Abstract Mechanochemistry uses mechanical force to break, form, and manipulate chemical bonds to achieve functional transformations and syntheses. Over the last years, many innovative applications of mechanochemistry have been developed. Specifically for the synthesis and activation of carbon‐rich π‐conjugated materials, mechanochemistry offers reaction pathways that either are inaccessible with other stimuli, such as light and heat, or improve reaction yields, energy consumption, and substrate scope. Therefore, this review summarizes the recent advances in this research field combining the viewpoints of polymer and trituration mechanochemistry. The highlighted mechanochemical transformations include π‐conjugated materials as optical force probes, the force‐induced release of small dye molecules, and the mechanochemical synthesis of polyacetylene, carbon allotropes, and other π‐conjugated materials.