Solution Synthesis Research Articles

Synthesis and properties of antimony sulfoiodide doped with tin (II) cations

Antimony sulfoiodide (SbSI) is a highly efficient energy conversion piezoelectric material. We obtained SbSI doped with tin (II) ions according to the formula Sb[Formula: see text]SnxSI[Formula: see text] ([Formula: see text]–0.1). This heterovalent doping has been performed by the novel method of synthesis in an aqueous solution. The introduction of tin cations leads to a material Curie point increase of more than 10[Formula: see text]K. The samples containing 5[Formula: see text]mol.% of the dopant possess the best piezoelectric properties: piezomodule [Formula: see text][Formula: see text]pC/N, dielectric constant at a frequency of 1[Formula: see text]kHz — 1758, dielectric loss tangent — 0.054, and piezosensitivity — 50[Formula: see text]mV[Formula: see text]×[Formula: see text]m/N. Thus, tin-doped SbSI is a promising material for highly efficient electromechanical transducers and sensors.

Growth and Dispersion Control of SnO2 Nanocrystals Employing an Amino Acid Ester Hydrochloride in Solution Synthesis: Microstructures and Photovoltaic Applications.

Tin oxide (SnO2) is a technologically important semiconductor with versatile applications. In particular, attention is being paid to nanostructured SnO2 materials for use as a part of the constituents in perovskite solar cells (PSCs), an emerging renewable energy technology. This is mainly because SnO2 has high electron mobility, making it favorable for use in the electron transport layer (ETL) in these devices, in which SnO2 thin films play a role in extracting electrons from the adjacent light-absorber, i.e., lead halide perovskite compounds. Investigation of SnO2 solution synthesis under diverse reaction conditions is crucial in order to lay the foundation for the cost-effective production of PSCs. This research focuses on the facile catalyst-free synthesis of single-nanometer-scale SnO2 nanocrystals employing an aromatic organic ligand (as the structure-directing agent) and Sn(IV) salt in an aqueous solution. Most notably, the use of an aromatic amino acid ester hydrochloride salt-i.e., phenylalanine methyl ester hydrochloride (denoted as L hereafter)-allowed us to obtain an aqueous precursor solution containing a higher concentration of ligand L, in addition to facilitating the growth of SnO2 nanoparticles as small as 3 nm with a narrow size distribution, which were analyzed by means of high-resolution transmission electron microscopy (HR-TEM). Moreover, the nanoparticles were proved to be crystallized and uniformly dispersed in the reaction mixture. The environmentally benign, ethanol-based SnO2 nanofluids stabilized with the capping agent L for the Sn(IV) ions were also successfully obtained and spin-coated to produce a SnO2 nanoparticle film to serve as an ETL for PSCs. Several SnO2 ETLs that were created by varying the temperature of nanoparticle synthesis were examined to gain insight into the performance of PSCs. It is thought that reaction conditions that utilize high concentrations of ligand L to control the growth and dispersion of SnO2 nanoparticles could serve as useful criteria for designing SnO2 ETLs, since hydrochloride salt L can offer significant potential as a functional compound by controlling the microstructures of individual SnO2 nanoparticles and the self-assembly process to form nanostructured SnO2 thin films.

Morphophysiological changes in Bauhinia cheilantha (Bong.) Steud. (Fabaceae) caused by water deficit

Drought-induced alterations often result in plant acclimation responses, though the extent to which these traits adjust, and their true significance remain species-specific and subject to debate. In order to discern which traits exhibit plasticity and essentiality for the species' survival, we studied the morpho-physiological responses of Bauhinia cheilantha seedlings subjected to varying water regimes. We examined modifications in growth patterns, resource allocation and partitioning, morphological traits, organic solute synthesis, relative water content in leaves and roots, and the plasticity index for each trait under different water supply levels. Several traits linked to plant growth were reduced under stress, but those changes were not considered to be plastic. The concentration of organic solutes increased under stress and exhibited a reversible behavior by reducing their levels after re-irrigation. These alterations underscored the significance of such compounds for survival during water deficit periods and the high degree of adaptability. B. cheilantha exhibits morpho-physiological plasticity, as demonstrated by alternating high levels of plasticity in physiological and morphological features, which are associated with moderate drought stress. The study discusses how these changes affect the growth and survival of the species.

Arthrospira promotes plant growth and soil properties under high salinity environments.

Salt stress detrimentally impacts plant growth, imperiling crop yield and food quality. Ameliorating plant resilience and productivity in saline environments is critical for global food security. Here, we report the positive effect of Arthrospira (Spirulina) on plant growth and salt tolerance in Arabidopsis and sweet sorghum. Arthrospira application greatly promotes seed germination and seedling growth in both species under salt stress conditions in a dosage-dependent manner. Application of 6 mg Arthrospira per plate significantly enhances K+/Na+ equilibrium and reactive oxygen species (ROS) scavenging in Arabidopsis, reducing salt-induced toxicity. The primary root length, survival rate, chlorophyll content, photosynthesis, plant height, biomass and yield were all improved in both species. Concurrently, Arthrospira demonstrated the synthesis of compatible solutes, such as trehalose (Tre) and glucosylglycerol (GG), contributing to heightened stress tolerance when co-cultivated with Arabidopsis on plates. Transcriptome analysis revealed dramatic up-/down- regulation of genes involved in phytohormone signal transduction, chlorophyll and photosynthesis metabolism, and phenylpropanoid metabolism in Arabidopsis. Furthermore, the application of Arthrospira exerted a positive influence on the rhizosphere bacteriome structure in sweet sorghum, crucial for nutrient cycling and soil health enhancement. Our findings uncovered the underlying mechanisms of algae-plants interaction in saline soil, proposing strategies to enhance crop productivity and soil quality, thereby addressing the urgent need for sustainable agriculture practices to mitigate salinity's repercussions amidst climate change challenges.

P-type NiOx ultrathin film as highly efficient hole extraction layer in n-type PbS quantum dots based NIR photodiode

Recently, the development of zero-dimensional (0D) materials has experienced significant growth. Among them, PbS colloidal quantum dots (CQDs) have received special attention due to their outstanding properties, including tunable optical absorption ranging from 600 to 2600 nm (size dependent bandgap) and easy solution synthesis. PbS CQDs are considered as one of the most promising materials for the next generation of infrared sensors. Hence, there is a growing interest in their use in industrial spheres. One of the major keys to obtaining high-performance devices is the realization of efficient charge extraction contacts on PbS CQDs films. In this work, we have demonstrated an efficient hole extraction layer (HEL) using NiOx ultra-thin film on infrared p-i-n photodiode based on only n-type PbS nanocrystals (CQDs). We compared the performance with the standard optimized MoOx. We obtained a significant gain in external quantum efficiency (EQE), a decrease of the operating bias, while keeping the same dark current level.

Synthesis of sodium hypochlorite solutions in coaxial flow cells in current reverse mode

Electrodes made of platinized titanium with a surface platinum content of 2–3 mg/cm2 can be used in non-diaphragm flow- and accumulative-type electrolyzers for the electrolysis of low-concentrated NaCl solutions in order to obtain pure NaClO solutions. If electrolysis of 0.15 M NaCl solution is carried out on platinized titanium electrodes in the usual mode at current densities of 20–40 mA/cm2, then the anode surface passes into an oxidized passive state. In this case, the current efficiency of hypochlorite does not exceed 40%, and the current efficiency of chlorate is more than 20%. During a short electrolysis on a preliminarily reduced surface of platinized titanium, the current efficiency of hypochlorite reaches 90% with almost no accumulation of chlorate. Carrying out the long-term electrolysis of low-concentrated NaCl solutions in the regime of periodic polarity reverse makes it possible to significantly (up to 10 times) reduce the content of chlorate in the resulting sodium hypochlorite solutions. The most promising is the synthesis of sodium hypochlorite solutions in flow-type electrochemical reactors consisting of several series-connected electrochemical modules with an undivided electrode space in the mode of periodic current reverse. The electrolyzer of two series-connected cells in the mode without current reverse allows obtaining a solution that contains 500 mg/L of sodium hypochlorite and 130 mg/L of sodium chlorate. Carrying out the electrolysis in the reverse current mode every 30 s reduces the content of sodium chlorate to 25 mg/L, which makes it possible to produce high-purity NaClO solutions.

Exothermic Synthesis of Binary Solid Solutions Based on Hafnium and Zirconium Carbides

Exothermic Synthesis of Binary Solid Solutions Based on Hafnium and Zirconium Carbides

Solution synthesis of two-dimensional zinc oxide (ZnO)/molybdenum disulfide (MoS2) heterostructure through reactive templating for enhanced visible-light degradation of rhodamine B

Solution synthesis of two-dimensional zinc oxide (ZnO)/molybdenum disulfide (MoS2) heterostructure through reactive templating for enhanced visible-light degradation of rhodamine B

Constructing green superhydrophilic and superoleophobic COFs-MOFs hybrid-based membrane for efficiently emulsion separation and synchronous removal of microplastics, dyes, and pesticides

Oil spills and micropollutants have become thorny environmental issues, posing serious threat to ecosystem and human health. To settle such dilemma, this study successfully constructed a robust and environmentally-friendly MOFs-COFs hybrid-based membrane (FS-50/COF(MATPA)-MOF(Zr)/PDA@PVDF) for the first time through solution synthesis and solvothermal method, combined with surface modification of FS-50 molecule. Importantly, we employed a simple two-step strategy to obtain the high-aspect-ratio MOFs fibers: (1) solvent regulation to generate smaller needle-like whiskers during the in-situ growth of MOFs on COFs; (2) high pressure induced directional crystallization in filtration process. The introduction of polydopamine (PDA) greatly improved the adhesion between coating and PVDF membrane. The in-situ growth of high length-diameter ratio MOFs fibers on blocky COFs greatly enhanced the specific surface area of MOFs-COFs hybrid, thus provided sufficient absorption sites. The functional groups of FS-50 endowed the hybrid membrane with superhydrophilicity and superoleophobicity, which facilitated to selectively penetrate water molecules and repel non-polar pollutants. The separation efficiency and decontamination mechanism of hybrid membrane to the simulated oily wastewater (containing various MPs, dyes, and pesticides) were investigated through experiments and theoretical calculations. The hybrid membrane could selectively and synchronously adsorb various dyes (20 mg/L–120 mg/L, almost 100% removal) and pesticides (10 mg/L for DIF and TET, adsorption rates 93.2% and 90.9%, respectively) from oil-water emulsion (50 mL). The large-scale coated sponge (6 cm × 4.5 cm × 3 cm) could quickly achieve separation of oil-water mixture (almost 100%) with a water permeability of more than 162 L m−2·h−1·bar−1, and simultaneously remove various MPs (PP-2000, PP-100, PE-2000, PS-100, 0.2 g/300 mL for each), Sudan Ⅲ (C0 = 200 mg/L), and DIF (C0 = 10 mg/L) from a simulant oily wastewater (300 mL), with the removal rates of almost 100% for MPs, 99.7% for Sudan Ⅲ, and 95.8% for DIF. Furthermore, we elucidated the removal mechanism of pesticide and dyes through simulating the theoretical adsorption energy and potential adsorption sites. The hybrid membrane not only provides a promising candidate for the removal of multiple pollutants from oil-water emulsion, but also opens a new strategy for achieving efficient and clean aquatic environment restoration.

Influence of the platinum surface state on the selectivity of the electrochemical synthesis of sodium hypochlorite

AbstractBACKGROUNDThe synthesis of sodium hypochlorite solutions by electrolysis of low‐concentration and isotonic NaCl solutions using the most available dimensionally stable anodes from platinized titanium is promising from the point of view of the economics of the process. However, such synthesis is seriously complicated by the formation of toxic sodium chlorate impurity.RESULTSIt is shown that in low‐concentration NaCl solutions under anodic polarization, the platinum surface rapidly passes into an oxidized passive state with a NaClO current efficiency (CE) of less than 30% and CE of NaClO3 of more than 20%. Carrying out short‐term electrolysis on the reduced surface of platinum makes it possible to increase the CE of NaClO to almost 90% in the absence of chlorate accumulation. Carrying out electrolysis in the mode of periodic change of electrode polarity (current reverse) allows solving the problem of anode passivation and significantly increasing the purity of the resulting sodium hypochlorite solutions.CONCLUSIONElectrolysis of an isotonic 0.15 mol L−1 NaCl solution in the current reverse mode allows increasing CE(NaClO) from 21% to 40% and significantly decreasing CE(NaClO3) from 21% to 4%. Based on the results obtained, a membraneless electrolyzer can be constructed to produce disinfectant solutions ‘on the spot’ using a commercially available pharmaceutical isotonic solution of NaCl. © 2023 Society of Chemical Industry (SCI).

Advances in advanced solution‐synthesis‐based structural materials for tactile sensors and their intelligent applications

AbstractIntelligent applications, with tactile sensors at their core, represent significant advancement in the field of artificial intelligence. However, achieving perception abilities in tactile sensors that match or exceed human skin remains a formidable challenge. Consequently, the design and implementation of hierarchical structural materials are considered the optimal solution to this challenge. In contrast to conventional methods, such as complicated lithography and three‐dimensional printing, the cost‐effective and scalable nature of advanced solution‐synthesis methods makes them ideal for preparing diverse tactile sensors with hierarchical structural materials. However, the process and applicability of advanced solution synthesis methods have yet to form a seamless system. Accordingly, the development and intellectualization of tactile sensors based on advanced solution synthesis methods are still in their early stages, and require a comprehensive and systematic review to usher in progress. This study delves into the advantages and disadvantages of various advanced solution synthesis methods, providing detailed insights. Furthermore, the positive effects of hierarchical structural materials constructed using these methods in tactile sensors and their intelligent applications are also discussed in depth. Finally, the challenges and future opportunities faced by this emerging field are summarized.image

Polyol Synthesis of Nanoparticles: A Decade of Advancements and Insights

This article presents a focused overview of advancements in the field of polyol synthesis of metal, metal oxide nanoparticles and nanocomposites, specifically those reported in the current decade. The aim of this article is to present the pertinent physico-chemical factors associated with nanoparticle synthesis in polyol solutions, highlighting their applications in both biological and industrial domains. The scope of this review article is selective rather than exhaustive, concentrating on noteworthy contributions to polyol nanoparticle synthesis that hold potential for refining synthesis methods. To comprehend the role of polyols in nanoparticle synthesis, an examination of the distinct physical properties of various polyols is crucial. Moreover, understanding the particular functions and mechanisms governing nanoparticle formation is imperative in this context.

Synergistic effects of sulphur vacancies and MoS2 on the photocatalytic activity of CdxZn1-xS for H2 evolution

Efficient photocatalysts nurture great potential for harnessing sunlight to produce chemical energy, a pivotal step towards sustainable fuel production. However, designing such systems poses significant challenges due to the complex interaction between light absorption and charge carrier dynamics. In an attempt to address these challenges, this study introduces a novel approach, combining bulk-twinned homojunction CdxZn1-xS photocatalysts with sulphur vacancies. These CdxZn1-xS photocatalysts are seamlessly integrated with molybdenum disulfide (MoS2) to optimize photocatalytic properties and enhance charge transfer via the formation of heterojunctions. Due to its unique crystal structure, the twinned homojunction in CdxZn1-xS enhances light absorption and charge carrier generation. The integrated sulphur vacancies perform several functions: they expediate light adsorption and inhibit electron-hole recombination. These vacancies were initially introduced into the bulk structure during CdxZn1-xS solid solution synthesis. Further, MoS2 provided an augmentation at the surface modification level, thus enhancing their functional role and amplifying their impact on the overall photocatalytic efficiency. The heterojunction formed between MoS2 and CdxZn1-xS provides an integrated efficient platform for overall performance. The composite nanocrystals, wurtzite/zinc-blende twinned MoS2/CdxZn1-xS, were synthesized via an N, N-dimethylformamide-assisted solvothermal method. Detailed characterization was conducted to establish correlations among activity, morphology, and surface properties. The resulting composite photocatalysts demonstrated improved solar hydrogen generation activity and stability, surpassing the performance of twinned crystal CdxZn1-xS.

A simple synthetic approach to BaZrS3, BaHfS3, and their solid solutions

AbstractA simple synthetic approach to BaZrS3, BaHfS3, and their solid solutions is presented and discussed here. The synthesis is performed under relatively mild conditions (T = 500°C) and is complete in a few hours. The reactants are powdered BaS, Me (Me: Zr, Hf) and S in a ratio 1:1:3, mixed and sealed under vacuum in borosilicate glass ampoules. No purification is usually required, and the yield is quantitative. The low synthesis temperature allows for the use of borosilicate glass as container material instead of silica glass, thus lowering the costs and simplifying the sealing of the reaction vessel; furthermore, the use of expensive ZrS2 and HfS2 is avoided. The same procedure was successfully used for the synthesis of solid solutions BaHf1‐xZrxS3 that were always obtained as crystalline single‐phase materials. The solid solutions display optical and structural properties that vary in a linear fashion with the composition and are intermediate between those of BaZrS3 and BaHfS3. The possibility of varying the band gap of the material between 1.78 (BaZrS3) and 2.11 eV (BaHfS3) in a continuous way by simply adjusting the Hf/Zr ratio is very intriguing for potential applications in multi‐junction and in‐door photovoltaic applications and light emitting devices.

Synthesis mechanism and electrical conductivity of NbCxO1-x solid solution

Niobium oxycarbide (NbCxO1-x) is an important soluble anode utilized primarily for the electrochemical preparation of metal Nb. Based on thermodynamic analysis, this study elucidates the controllable synthesis of single-phase NbCxO1-x solid solution by the carbothermal reduction of Nb2O5. The effects of synthesis temperature, holding time, forming pressure, and carbon content on the sintering behavior of NbCxO1-x solid solution are investigated. Under the optimum conditions (1400 °C of synthesis temperature, 4 h of holding time, 100 MPa of forming pressure, and 1/7 of molar ratio of Nb2O5 to carbon black), the single-phase NbCxO1-x solid solution with the similar crystal structure to NbC and 0.440 nm of the lattice parameter is obtained. The optimum resistivity of the solid solution is only 52.10 mΩ·cm, which is two orders of magnitude lower than that before sintering. This work provides crucial raw materials for the extraction of niobium by soluble anode electrolysis, improving the efficient electrolysis of niobium.

Photothermally heated colloidal synthesis of nanoparticles driven by silica-encapsulated plasmonic heat sources

Using photons to drive chemical reactions has become an increasingly important field of chemistry. Plasmonic materials can provide a means to introduce the energy necessary for nucleation and growth of nanoparticles by efficiently converting visible and infrared light to heat. Moreover, the formation of crystalline nanoparticles has yet to be included in the extensive list of plasmonic photothermal processes. Herein, we establish a light-assisted colloidal synthesis of iron oxide, silver, and palladium nanoparticles by utilizing silica-encapsulated gold bipyramids as plasmonic heat sources. Our work shows that the silica surface chemistry and localized thermal hotspot generated by the plasmonic nanoparticles play crucial roles in the formation mechanism, enabling nucleation and growth at temperatures considerably lower than conventional heating. Additionally, the photothermal method is extended to anisotropic geometries and can be applied to obtain intricate assemblies inaccessible otherwise. This study enables photothermally heated nanoparticle synthesis in solution through the plasmonic effect and demonstrates the potential of this methodology.

N = 8 Armchair Graphene Nanoribbons: Solution Synthesis and High Charge Carrier Mobility.

Structurally defined graphene nanoribbons (GNRs) have emerged as promising candidates for nanoelectronic devices. Low bandgap (< 1 eV) GNRs are particularly important when considering the Schottky barrier in device performance. Here, we demonstrate the first solution synthesis of 8-AGNRs through a carefully designed arylated polynaphthalene precursor. The efficiency of the oxidative cyclodehydrogenation of the tailor-made polymer precursor into 8-AGNRs was validated by FT-IR, Raman, and UV-vis-near-infrared (NIR) absorption spectroscopy, and further supported by the synthesis of naphtho[1,2,3,4-ghi]perylene derivatives (1 and 2) as subunits of 8-AGNR, with a width of 0.86 nm as suggested by the X-ray single crystal analysis. Low-temperature scanning tunneling microscopy (STM) and solid-state NMR analyses provided further structural support for 8-AGNR. The resulting 8-AGNR exhibited a remarkable NIR absorption extending up to ∼2400 nm, corresponding to an optical bandgap as low as ∼0.52 eV. Moreover, optical-pump TeraHertz-probe spectroscopy revealed charge-carrier mobility in the dc limit of ∼270 cm2 V-1 s-1 for the 8-AGNR.

N=8 Armchair Graphene Nanoribbons: Solution Synthesis and High Charge Carrier Mobility**

AbstractStructurally defined graphene nanoribbons (GNRs) have emerged as promising candidates for nanoelectronic devices. Low band gap (&lt;1 eV) GNRs are particularly important when considering the Schottky barrier in device performance. Here, we demonstrate the first solution synthesis of 8‐AGNRs through a carefully designed arylated polynaphthalene precursor. The efficiency of the oxidative cyclodehydrogenation of the tailor‐made polymer precursor into 8‐AGNRs was validated by FT‐IR, Raman, and UV/Vis‐near‐infrared (NIR) absorption spectroscopy, and further supported by the synthesis of naphtho[1,2,3,4‐ghi]perylene derivatives (1 and 2) as subunits of 8‐AGNR, with a width of 0.86 nm as suggested by the X‐ray single crystal analysis. Low‐temperature scanning tunneling microscopy (STM) and solid‐state NMR analyses provided further structural support for 8‐AGNR. The resulting 8‐AGNR exhibited a remarkable NIR absorption extending up to ∼2400 nm, corresponding to an optical band gap as low as ∼0.52 eV. Moreover, optical‐pump TeraHertz‐probe spectroscopy revealed charge‐carrier mobility in the dc limit of ∼270 cm2 V−1 s−1 for the 8‐AGNR.

Black Phosphorus-Based ZnO-Ag Nanocomposite for Antibacterial Activity against Tigecycline-Resistant Acinetobacter baumannii

Acinetobacter baumannii is a critically hard-to-treat gram-negative pathogen responsible for a range of infectious diseases. Tigecycline is a last-resort antibiotic for A. baumannii infection; however, tigecycline-resistant (TIG-R) A. baumannii has been increasingly reported. Therefore, new strategies must be developed to treat these detrimental infections. Nanoantibiotics composed of two-dimensional (2D) black phosphorus (BP) and its derived nanocomposites have emerged as excellent alternatives to current antibiotics. However, the development of unique materials to target specific pathogens is challenging. Here, we report the preparation of a BP-based ZnO-Ag (ZPBA) nanocomposite. A low-temperature solution synthesis method was used to prepare ZnO and Ag nanoparticles immobilized on BP nanosheets. X-ray diffraction, transmission electron microscopy, and X-ray photoelectron spectroscopy were used to characterize the ZPBA nanocomposite. The antibacterial activity of ZPBA nanocomposite was assessed by determining its minimum inhibitory concentration against type (ATCC 19606, ATCC 15150) and TIG-R (ATCC 19606-R) A. baumannii strains. From the assays, ZPBA showed superior activity against TIG-R A. baumannii strain with MIC of 12.5 µg·mL−1 compared to all other prepared samples. Finally, the combination of bacterial membrane disruption and ROS generation was demonstrated to be a potential antibacterial mechanism of ZPBA. Our results show that ZPBA could be a potential nanoantibiotic platform for eradicating TIG-R A. baumannii.

Synthesis, Structure, and Properties of Diboride Solid Solutions (Hf1 – xTax)B2

Synthesis, Structure, and Properties of Diboride Solid Solutions (Hf1 – xTax)B2