Synthesis Of Materials Research Articles

Dealloyed nickel skeleton hosting in-situ formed multimetallic phosphides for enhanced electrochemical energy storage

Transition metal phosphides (TMPs) exhibit considerable potential in supercapacitors (SCs) electrodes fabrication due to their high power densities and conducive ion transport, positioning them as quintessential candidates for such application. Despite their promise, monometallic phosphides require further electrochemical performance enhancements. This work unveils an innovative strategy for synthesizing complex cobalt/nickel phosphides directly on a nickel skeleton (Ni@NCP), achieved by the selectively leaching copper from a Ni–Cu alloy via a dealloying process after electrodeposition, significantly improving electrochemical performance through increased electroactive sites and optimized ion diffusion channels. The Ni@NCP electrode exhibits an impressive specific capacitance of 612 F g−1 at a high current density of 20 A g−1. Furthermore, the unique hollow nanotube structure greatly enhances cyclic stability, maintaining 80.1 % capacity after 10,000 cycles at 10 A g−1. This research presents a methodical approach to electrode material synthesis, emphasizing the construction of supportive frameworks and active sites, thereby underscoring the substantial potential for advancements in SC electrode technology.

Development and synthesis of anthracene-based fluorescence material for non-doped OLEDs

Efficient organic blue materials are essential to develop highly efficient organic light-emitting diodes. However, there is a challenge to commercialize efficient blue compounds due to the fundamentally wide band gap and the lack of pure blue emitters. In this study, the new anthracene-based fluorescent emitter, (4-(10-(4-(9H-carbazol-9-yl)-2-methylphenyl)anthracen-9-yl)-3-methylphenyl)diphenylphosphine oxide (CZm-AN-mPO) was designed and synthesized. The thermal, photophysical and electrochemical properties of the CZm-AN-mPO were systematically investigated. The CZm-AN-mPO exhibits a deep-blue emission at 425 nm and AIE property with a relatively narrow full-width at half maximum of 34 nm. The CZm-AN-mPO based non-doped devices show pure blue emission. The optimized OLEDs indicated maximum external efficiencies of 4.3% and 4.2% at emission layer thickness of 20 nm and 40 nm, respectively.

Towards sustainable construction: Performance evaluation of slag-cenosphere geopolymers under different NaOH concentrations

The incorporation of industrial wastes into construction materials, such as geopolymers, is highly desirable to improve their environmental impact. The choice of source materials, such as slag and cenosphere, and the amount of activator used significantly impact the properties of geopolymers. For instance, including high-reactivity precursors and optimizing activator composition may enhance mechanical strength and durability. However, no studies have evaluated the effect of cenosphere addition on the properties of geopolymer composites. This research study aims to unveil the synthesis of a binary geopolymer material by integrating slag and cenosphere as precursors, activated by sodium silicate (Na2SiO3) and sodium hydroxide (NaOH). Geopolymer composites were prepared to assess the impact of cenosphere addition (by substituting the slag with cenosphere in different percentages of 25, 50, and 75 %) and NaOH concentration (specifically 6 M, 9 M, and 12 M) on the material's properties. Additionally, one conventional mortar with a water-to-cement ratio of 0.5 was also prepared. Compressive strength, ultrasonic pulse velocity (UPV), electrical resistivity, water absorption, density, and thermogravimetric analysis were conducted. Results showed that increasing the cenosphere percentage increased the water absorption and decreased the compressive strength, UPV, electrical resistivity, and density compared to the geopolymer mixture with 100 % slag content. However, up to 50 % substitution of cenosphere, the geopolymer mix performed better than conventional mortar. Notably, results suggest a potential increase in CO2 uptake due to the addition of cenosphere, further enhancing the environmental performance of geopolymer composites. The findings of this study suggest the potential use of slag-cenosphere geopolymer as an alternative and sustainable construction material.

Blue Lead‐Free Perovskite Derivatives: Structural Diversity, Luminescence Properties and Light‐Emitting Diode Applications

AbstractHalide perovskite light‐emitting diodes (LEDs) have made remarkable advancements in both efficiency and stability. However, when compared to green and red LEDs, blue perovskite LEDs still lag behind in terms of efficiency and stability. Presently, efficient blue LEDs primarily rely on lead‐based perovskites, which goes against the environmentally friendly practices and restricts potential industrial applications. Consequently, there has been a surge of interest in academic research toward developing blue LEDs using lead‐free perovskites. This paper provides a comprehensive review of the structural diversity of lead‐free perovskite derivatives used for blue emission, encompassing Sn‐, Zr‐, Bi‐, Sb‐, Cu‐, Zn‐based halides as well as double perovskites. Various material synthesis techniques are discussed, such as nanocrystal preparation and film preparation. Additionally, the photoluminescence properties for different energy band structures are outlined, along with the luminescence mechanism involving energy transfer and strategies for enhancing luminous efficiency. The advancement in efficiency and stability of lead‐free perovskite LEDs is also examined in this review. Finally, the current challenges and future opportunities in advancing research on blue lead‐free perovskite derivatives and their potential application in LED technology is emphasized.

Propagation of nanosecond discharge in an air gap containing a water droplet: modelling and comparison with time-resolved images

The plasma-water interface is a complex medium characterized by interesting physical and chemical phenomena useful for many applications such as water processing or material synthesis. In this context, optimizing the transport of reactive species from plasma to water is crucial, and it may be achieved by increasing the surface-to-volume ratio of the processed object. Herein, we study the characteristics of a streamer produced by nanosecond discharge in air gap with a droplet of deionized water. The discharge is characterized experimentally by electrical measurements as well as by 1 ns-intergated ICCD images. To report plasma properties that are not accessible through experiment, such as the spatio-temporal evolution of electron density, electric field, and space charge density, a 2D fluid model is developed and adapted to the experimental geometry. Due to the fast propagation of the ionization front, the droplet is considered as a solid dielectric. The model solves Poisson’s equation as well as the drift-diffusion equation for electrons, positive ions, and negative ions. The utilized transport coefficients are tabulated as a function of the reduced electric field. Helmholtz equations are also included in the model to account for photoionization. The electron impact ionization source obtained from the model is compared to experimental 1 ns-integrated ICCD images, and a good agreement is observed. Finally, the model is used to investigate the influence of droplet dielectric permittivity and wetting angle (the angle between a liquid surface and a solid surface) on the properties of the discharge. Overall, the data reported herein demonstrate that the model can be used to investigate plasma properties under different conditions.

A thermodynamic theory coupling photo-chemo-mechano interactions for light-responsive hydrogel

Light-responsive hydrogel, as a typical functional hydrogel, is composed of crosslinked hydrophilic polymer chains, photosensitive molecules and water. Under illumination, the photosensitive molecules exhibit a transition in hydrophilic/ hydrophobic properties, leading to migration of water molecules and deformation of the hydrogel based on the temporal and spatial distribution of light. In this study, we propose a nonequilibrium thermodynamic framework to study the photo-chemo-mechano behaviors of light-responsive hydrogel. We firstly describe the light propagation in the hydrogel and the photochemical reaction kinetics. New free energy functions to expound the relationship between the photochemical reaction and thermodynamic process are established, and the constitutive equations are derived. Subsequently, we implant the model into a multi-field coupling analysis software, COMSOL, to conduct a spatio-temporal analysis of the hydrogel's response under uniform light exposure. Finally, we simulate the inhomogeneous deformation of light-responsive hydrogel strips under different illumination conditions and compare the results with experiments. The results highlight the importance of the photochemical reaction rate and the redistribution of light field caused by deformation. The present research holds potential for the precise manipulation and optimal design of light-responsive hydrogel in prospective applications, and offers insights for the synthesis of similar materials as well as the design of pertinent devices.

Iron(III) Monoglycerolate: A Potential Hemostatic Agent for Topical Application

Background: Glycerolates of biogenic elements are of interest because of their pharmacological activity. Some of them are used as active substances in agents for topical application and as biocompatible precursors in sol-gel synthesis of bioactive materials. Objective: In this work, morphostructural feature, ability to hydrolyze, and the pharmacological activity of previously synthesized iron(III) monoglycerate were studied. Methods: Analytical techniques, including SEM, TEM, XRD, TGA, IR spectroscopy, DLS and ELS, were used. Hemostatic activity was studied in vivo, and primary toxicological studies were carried out on experimental animals. Antimicrobial activity was studied using the agar diffusion method. Results: When dispersed in glycerol, solid crystalline iron(III) monoglycerolate transforms into an amorphous state, forming aggregates with an average particle size of 250 nm (according to DLS data). It slowly hydrolyzes in water at room temperature, while hydrolysis does not take place in an aqueous glycerol media. Iron(III) monoglycerolate is nontoxic and exhibits pronounced hemostatic activity and low antibacterial activity (relative to the strain S. аureus). Conclusion: Iron(III) monoglycerolate can be considered a potential hemostatic agent, showing promise for topical application in medical and veterinary practice, as well as a novel biocompatible precursor in the sol-gel synthesis of practically useful substances.

Efficient Removal of Water Soluble Fraction of Diesel Oil by Biochar Sorption Supported by Microbiological Degradation

The contamination of the water bodies by diesel oil (DO) and its water-soluble fraction (WSF) represents one of the most challenging tasks in the management of polluted water streams. This paper contains data related to the synthesis and characteristics of the plum stone biochar material (PmS-B), which was made from waste plum stones (PmS), along with its possible application in the sorption of the WSF of DO from contaminated water. Techniques applied in sample characterisation and comparisons were: Elemental Organic Analysis (EOA), Scanning Electron Microscopy−Energy Dispersive X-ray Spectroscopy (SEM-EDX), Fourier Transform Infrared Spectroscopy (FTIR), pH (pHsus) and point of zero charge (pHpzc). In order to increase the overall efficiency of the removal process, sorption and bioremediation were subsequently combined. Firstly, PmS-B was used as a sorbent of WSF, and then the remaining solution was additionally treated with a specific consortium of microorganisms. After the first treatment phase, the initial concentration of diesel WSF was reduced by more than 90%, where most of the aromatic components of DO were removed by sorption. The sorption equilibrium results were best fitted by the Sips isotherm model, where the maximum sorption capacity was found to be 40.72 mg/g. The rest of the hydrocarbon components that remained in the solution were further subjected to the biodegradation process by a consortium of microorganisms. Microbial degradation lasted 19 days and reduced the total diesel WSF concentration to 0.46 mg/L. In order to confirm the non-toxicity of the water sample after this two-stage treatment, eco-toxicity tests based on a microbial biosensor (Aliivibrio fischeri) were applied, confirming the high efficiency of the proposed method.

Printed Thick Film Resistance Temperature Detector for Real-Time Tube Furnace Temperature Monitoring.

Accurately acquiring crucial data on tube furnaces and real-time temperature monitoring of different temperature zones is vital for material synthesis technology in production. However, it is difficult to achieve real-time monitoring of the temperature field of tube furnaces with existing technology. Here, we proposed a method to fabricate silver (Ag) resistance temperature detectors (RTDs) based on a blade-coating process directly on the surface of a quartz ring, which enables precise positioning and real-time temperature monitoring of tube furnaces within 100-600 °C range. The Ag RTDs exhibited outstanding electrical properties, featuring a temperature coefficient of resistance (TCR) of 2854 ppm/°C, an accuracy of 1.8% FS (full scale), and a resistance drift rate of 0.05%/h over 6 h at 600 °C. These features ensured accurate and stable temperature measurement at high temperatures. For demonstration purposes, an array comprising four Ag RTDs was installed in a tube furnace. The measured average temperature gradient in the central region of the tube furnace was 5.7 °C/mm. Furthermore, successful real-time monitoring of temperature during the alloy sintering process revealed approximately a 20-fold difference in resistivity for silver-palladium alloys sintered at various positions within the tubular furnace. The proposed strategy offers a promising approach for real-time temperature monitoring of tube furnaces.

Continuously Adjustable Thickness of Bi2MoO6 Nanosheets Enhances Photocatalytic Oxidation.

In this study, two-dimensional (2D) nanosheet photocatalysts of Bi2MoO6 with varying thicknesses were synthesized by adjusting the temperature during the hydrothermal reaction. The thinnest Bi2MoO6 nanosheet reached an approximate thickness of ∼4 nm, while the thickest nanosheet measured only ∼16 nm. The photocatalytic performance for Rhodamine B (RhB) degradation was found to be the most effective for the thinnest Bi2MoO6 nanosheet, displaying a degradation rate constant of 0.11 min-1. This rate was 2.5 times higher than that observed for the ∼16 nm thick Bi2MoO6 photocatalyst. The enhanced performance of the thinner two-dimensional nanostructure can be attributed to improved separation and migration of photogenerated charges. Additionally, the study identified hydroxyl radicals (•OH) and superoxide radicals (•O2-) as crucial oxidative species, contributing to the efficient mineralization of RhB dye. This work highlights the controllable synthesis of 2D materials with varying thicknesses and their specific applications in photocatalytic oxidation.

Chiral Janus emulsions with gold nanocomposite for enantioselective catalysis

Chiral emulsions, with the chiral center of chiral-surfactant as the emulsifier, provide opportunities for selective catalysis and inorganic material synthesis. Janus emulsion draws researcher’s attention due to excellent multiple chambers, advanced structures and diverse interfaces. Chiral Janus emulsions are prepared with two immiscible oils of vegetable oil (VO)/dimethyl phthalate (DMP) and 2-(Perfluorooctyl)ethyl methacrylate (PFOEMA)/Ethoxylated trimethylolpropane triacrylate (ETPTA) as inner phases, by emulsified by chiral-surfactant [H-G-C16]FeCl4, in batch-scale by traditional vortex mixing. AuNPs as functional nanomaterials with peroxidase activity are then applied as active centers, adsorbing at the oil/water interface due to the electrostatic interactions between the positive charge of [H-G-C16]FeCl4 at Janus emulsion interfaces and the negative charge of AuNPs modified by SDS. Chiral Janus emulsion is endowed with catalytic activity and enantioselectivity. Catalytic results show two AuNPs@ Janus emulsions show better affinity to catalyze the oxidation of L-DOPA than D-DOPA. By investigating two AuNPs@ Janus emulsions with different inner phases, chiral Janus emulsion of AuNPs@ETPTA/PFOEMA/[H-G-C16]FeCl4(aq) has better catalytic activity and enantioselectivity than AuNPs@DMP/VO/[H-G-C16]FeCl4 (aq) because of the smaller droplets have larger interface areas could adsorb more [H-G-C16]FeCl4 molecules and AuNPs. The findings open an avenue in the production of chiral Janus emulsions with catalytic effect and enantioselectivity, which would push forward future applications in selective catalysis and inorganic material synthesis.

Electrochemistry of 2D-materials for the remediation of environmental pollutants and alternative energy storage/conversion materials and devices, a comprehensive review

This review article explores into the complicated relationship between electrochemistry and 2D materials, exploring their mutual influences and the consequential advancements in energy conversion, storage, and environmental applications. Electrochemical reactions, manifested through oxidations and reductions at submerged electrodes, form the linchpin connecting the electrochemistry of 2D materials with their practical utility. Various electrochemical cell topologies are investigated for their role in enhancing material flexibility, operational states, energy conversion efficiency, and device design adaptability. The comprehensive discussion extends to diverse applications, emphasizing the pivotal roles of 2D materials in environmental remediation, alternate energy storage and conversion, and chemical reactivity. Noteworthy applications include pollutant detection, adsorption and absorption of pollutants, elimination of both organic and inorganic pollutants, and photocatalytic degradation. The review also addresses materials synthesis via electrochemical processes, detailing functionalization, handling, and deposition techniques. Particular focus is directed towards local electrochemical techniques enabling the analysis and local alteration of 2D materials. Moreover, this paper concludes the article published in the recent years with this topic and most significant trends observed in 2022 and 2023 with electrochemistry of materials for the remediation of environmental pollutants. While the trends of article publishing increased from 2020 to 2023 with topic alternative energy storage/conversion materials. Finally, offering a comprehensive overview of the synergistic relationship between electrochemistry and 2D materials and their transformative potential in sustainable technologies. Broader contextThe decreasing availability of energy resources and the contamination of the environment are two significant worldwide concerns that need immediate attention. The focus on 2D materials and associated technologies is important for the efficient conversion of solar energy into chemical energy. These materials have diverse applications in fields such as energy (e.g., water splitting), synthesis (e.g., production of valuable chemicals and N2 reduction), and the environment (e.g., CO2 reduction and environmental remediation). Furthermore, Electrochemical energy storage and conversion (EESC) technologies are widely acknowledged as the most viable solutions to address the escalating energy crisis and environmental degradation because to their exceptional energy efficiency and little environmental footprint. Currently, there have been several reports discussing the use of 2D-materials in energy applications and wastewater treatment. However, there is a lack of comprehensive reviews that summarize the electrochemistry of 2D-materials, their preparation strategies, modification techniques, and related properties. Furthermore, there is a need for detailed analysis of the progress in applying 2D-materials for environmental pollution remediation, electrocatalytic performance, energy storage, and conversion technologies and devices. In this paper, we systematically and comprehensively review the electrochemistry of 2D-materials and innovatively analyze the design principles and difficulties of 2D-materials. We discussed comprehensively the remediation of environmental pollutants through 2D-materials in water treatment fields such as photocatylsts, adsorption/absorption and dyes removal as an entry point and provide an in-depth knowledge and outlook on the current status and development potential of specific applications of energy storage and conversion materials and devices.

Novel Penetrated Nucleation Mechanism for Controlled Synthesis of 2D Materials on Metal Substrates

Abstract2D materials have attracted considerable attention in the past decades for their unique properties, making the understanding of their nucleation process key to effective synthesis. Traditional explanations of thin‐film growth, focusing on the competition between atom interactions at the interface and within layers, often fall short of explaining real experimental results. Herein, a penetrated nucleation mechanism is proposed for 2D materials growth on metal substrates, taking into account the role of metal substrate atoms. This approach leads to a better understanding of how the surface shape evolves in two specific ways during growth in real experimental findings. Supported by detailed first‐principles simulations of boron on metal substrates and thermodynamic analyses of other studies involving metals and nonmetals, the above‐proposed mechanism is validated. Moreover, a broad strategy for growing large‐scale 2D materials on metal surfaces without creating undesired alloy layers is also presented, by adjusting the interfacial interactions by surface passivation, validated by existing experiments.

CH3COOLi-assisted lithium source on the synthesis of high-performance single-crystal Ni-rich cathode material

CH3COOLi-assisted lithium source on the synthesis of high-performance single-crystal Ni-rich cathode material

Application of hyperbranched polysiloxanes in biomedical materials based on AIE polymer properties

Application of hyperbranched polysiloxanes in biomedical materials based on AIE polymer properties

Unveiling the potential of cellulose, chitosan and polylactic acid as precursors for the production of green carbon nanofibers with controlled morphology and diameter

Carbon nanofibers (CNFs) are very promising materials with application in many fields, such as sensors, filtration systems, and energy storage devices. This study aims to explore the use of eco-friendly biopolymers for CNF production, finding novel, suitable and sustainable precursors and thus prioritising environmentally conscious processes and ecological compatibility.Polymeric nanofibers (PNFs) using cellulose acetate, polylactic acid, and chitosan as precursors were successfully prepared via electrospinning. Rheological testing was performed to determine suitable solution concentrations for the production of PNFs with controlled diameter and appropriate morphology. Their dimensions and structure were found to be significantly influenced by the solution concentration and electrospinning flow rate. Subsequently, the electrospun green nanofibers were subject to stabilisation and carbonisation to convert them into CNFs. Thermal behaviour and chemical/structural changes of the nanofibers during stabilisation were investigated by means of thermogravimetric analysis and Fourier-transform infrared spectroscopy, while the final morphology of the fibers after stabilisation and carbonisation was examined through scanning electron microscopy to determine the optimal stabilisation parameters. The optimal fabrication parameters for cellulose and chitosan-based CNFs with excellent morphology and thermal stability were successfully established, providing valuable insight and methods for the sustainable and environmentally friendly synthesis of these promising materials.

Synthesis of lead-free piezoelectric potassium sodium niobates for the preparation of anti-fouling KNN porous membrane

Potassium sodium niobates (KNNs) have garnered significant attention owing to their lead-free nature and potential for use in self-cleaning membranes. This paper presents the synthesis of (K0.5Na0.5)NbO3 materials for the fabrication of porous membranes, which enable in situ ultrasonic resonance to effectively eliminate contaminants from the membrane surface. KNN powder was synthesized via solid-state reactions, and the membranes were prepared using conventional sintering techniques. The effects of ball-milling time and calcination temperature on the phase structure, pore size, permeance, flexural strength, chemical stability, and piezoelectric properties were comprehensively investigated. The optimal membranes exhibited an average pore size of approximately 300 nm, a porosity of 23 %, and permeance of 220 L m−2 h−1 bar−1 at a sintering temperature of 1050 °C. A polarized electrical field with a strength of 1 kV/mm was applied to the membranes, resulting in an ultrasonic response of 20 mV at an excitation voltage of 20 V with a frequency of 200 kHz. Furthermore, the in situ anti-fouling performance was evaluated by conducting filtration tests on a 500 ppm oil-in-water (O/W) emulsion, demonstrating that the stationary flux increased by 46.7 % when subjected to an excitation voltage of 60 V.

Recycling lithium-ion battery graphite: Synthesis of adsorbent materials for highly efficient removal of dye and metal ions from wastewater

The fate of residual graphite derived from hydrometallurgical treatment of spent Lithium-ion batteries remains uncertain. This study dwells on the aim of identifying the potentialities of recycling residual graphite for wastewater treatment. Graphite was recovered hydrometallurgically, and new adsorption materials: graphite oxide (GO) and graphene oxide (GrO) were synthesized from the residual graphite using the chemical oxidization method. Synthesized materials showed higher interlayer spacings (GO = 0.81 nm, GrO = 0.78 nm) than the commercially available similar materials. Adsorption studies revealed higher adsorption capacities for both dye (>550 mg/g in all cases) and metal ions (highest ∼93 mg/g for Ni2+ and lowest ∼68 mg/g for Zn2+). GrO showed superior results than GO due to its high surface area and porosity despite GO having more functional groups. Moreover, produced materials showed about 97 % removal of dye and about 94 % removal of contaminated metals which are higher performance than existing commercial or similar materials. These findings highlight the promising recycling capabilities of waste graphite and suggest its potential as a substitute for natural graphite.

Enantioselective synthesis of chiral α,α-dialkyl indoles and related azoles by cobalt-catalyzed hydroalkylation and regioselectivity switch

General, catalytic and enantioselective construction of chiral α,α-dialkyl indoles represents an important yet challenging objective to be developed. Herein we describe a cobalt catalyzed enantioselective anti-Markovnikov alkene hydroalkylation via the remote stereocontrol for the synthesis of α,α-dialkyl indoles and other N-heterocycles. This asymmetric C(sp3)−C(sp3) coupling features high flexibility in introducing a diverse set of alkyl groups at the α-position of chiral N-heterocycles. The utility of this methodology has been demonstrated by late-stage functionalization of drug molecules, asymmetric synthesis of bioactive molecules, natural products and functional materials, and identification of a class of molecules exhibiting anti-apoptosis activities in UVB-irradiated HaCaT cells. Ligands play a vital role in controlling the reaction regioselectivity. Changing the ligand from bi-dentate L6 to tridentate L12 enables CoH-catalyzed Markovnikov hydroalkylation. Mechanistic studies disclose that the anti-Markovnikov hydroalkylation involves a migratory insertion process while the Markovnikov hydroalkylation involves a MHAT process.

Stability, Chemical Bonding, and Electron Lone Pair Localization in AsN at High Pressure by Density Functional Theory Calculations.

The covalent bonding framework of crystalline single-bonded cubic AsN, recently synthesized under high pressure and high temperature conditions in a laser-heated diamond anvil cell, is here studied by means of density functional theory calculations and compared to single crystal X-ray diffraction data. The precise localization of the nonbonding electron lone pairs and the determination of their distances and orientations are related to the presence of characteristic structural motifs and space regions of the unit cell dominated by repulsive electronic interactions, with the relative orientation of the electron lone pairs playing a key role in minimizing the energy of the structure. We find that the vibrational modes associated with the expression of the lone pairs are strongly localized, an observation that may have implications for the thermal conductivity of the compound. The results indicate the thermodynamic stability of the experimentally observed structure of AsN above ∼17 GPa, provide a detailed insight into the nature of the chemical bonding network underlying the formation of this compound, and open new perspectives to the design and high pressure synthesis of new pnictogen-based advanced materials for potential applications of energetic and technological relevance.