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Polyaniline (PANI) is a promising conductive polymer for use in energy storage applications. Here, a one-step hydrothermal method of PANI polymerization on carbon felt electrode was synthesized using an azo dye, a bisulfonated dichloro anionic dye molecule to enhance an efficient textile-based flexible supercapacitor electrode material for energy storage applications. The electrode material synthesized at concentration of 2 mM AY17 exhibits 814.1 F g-1 at the scan rate of 5 mV s-1 with multiwall carbon nanotubes (MWCNTs). Due to electrostatic interaction with the polymer, the presence of high electronegativity Cl atoms in the dye molecule significantly improves the PANI structure's electron donor/acceptor properties. A symmetric supercapacitor exhibits an energy density of 11.7 W h kg−1 at a power density of 300 W kg−1, and it is 4.5 W h kg−1 at 1800 W kg−1 in 3.0 M KCl aqueous electrolyte. The capacitance retention performance value of the symmetric supercapacitor exhibited 81.76% after 2500 cycles.

In this study, carbon dots are synthesized hydrothermally from loblolly pine using top-down and bottom-up processes. The bottom-up process dialyzed carbon dots from hydrothermally treated process liquid. Meanwhile, hydrochar was oxidized into carbon dots in the top-down method. Carbon dots from top-down and bottom-up processes were compared for their yield, size, functionality, and quantum properties. Furthermore, hydrothermal treatment temperature and residence time were evaluated on the aforementioned properties of carbon dots. The results indicate that the top-down method yields higher carbon dots than bottom-up in any given hydrothermal treatment temperature and residence time. The size of the carbon dots decreases with the increase in reaction time; however, the size remains similar with the increase in hydrothermal treatment temperature. Regarding quantum yield, the carbon dots from the top-down method exhibit higher quantum yields than bottom-up carbon dots where the quantum yield reaches as high as 48%. The only exception of the bottom-up method is the carbon dots prepared at a high hydrothermal treatment temperature (i.e., 260 °C), where relatively higher quantum yield (up to 18.1%) was observed for the shorter reaction time. Overall, this study reveals that the properties of lignocellulosic biomass-derived carbon dots differ with the synthesis process as well as the processing parameters.

Phenylketonuria (PKU) is a critical disease in the disorder of amino acid metabolism, which mostly emerges in children. The most common method used in PKU treatment is the detection of L-phenylalanine (PHEA) as the biomarker of PKU. In the present work, a new molecularly imprinted electrochemical electrode based on WS2 nanoflowers (NFs) on N,B-doped graphene (WS2 NFs/N,B-GR) is presented for PHEA assay in milk samples. First of all, WS2 NFs/N,B-GR was synthesized via a high-efficiency hydrothermal synthesis. Cyclic voltammetry was applied to the electrochemical cell, including PHEA as a template molecule and pyrrole as a monomer, to form PHEA-imprinted electrochemical electrodes. Then, the structural and morphological features of WS2 NFs and WS2 NFs/N,B-GR were investigated in detail by various analytical methods. The limit of quantification and limit of detection values were obtained as 1.0 × 10-11 and 3.0 × 10-12 M, respectively, by a PHEA-imprinted electrochemical electrode. Finally, a PHEA-imprinted electrochemical sensor having a high degree of selectivity, stability, and reusability is presented in the literature for early diagnosis of PKU. © 2022 American Chemical Society. All rights reserved.

Seeking for extremely active and durable bifunctional electrocatalysts towards the overall water splitting possesses a strategic significance on the development of sustainable and clean energy for the replacement of fossil fuels. Ir-based nanomaterials are deemed as one of the most high-efficiency oxygen evolution reaction electrocatalysts while the hydrogen evolution reaction performance is unfavorable. In this work, we report a one-pot hydrothermal synthesis of N-doped graphene anchored Ir nanoparticles (Ir/N-rGO) with ultrasmall particle size (∼2.0 nm). Apart from the predictably superior OER performance, the resultant Ir/N-rGO also displays excellent hydrogen evolution reaction (HER) performance, requiring merely 76 and 260 mV overpotentials to achieve the current density of 10 mA cm-2 towards HER and OER, respectively. When applied as the bifunctional electrodes for overall water splitting, Ir/N-rGO needs a lower overpotential (1.74 V) to achieve a current density of 50 mA cm-2 in alkaline solution, exceeding that of Pt/C and RuO2 couple (1.85 V). Thus, the as-fabricated Ir/N-rGO has a commendable prospect in the practical application of alkaline water electrocatalysis.

Monoclinic vanadium dioxide VO2(M) is a well-known thermochromic material, with its critical transition temperature (68 °C) being the closest to room temperature (RT). Among the variety of grown methods, hydrothermal synthesis is a simple and cost-effective technique to grow thermochromic VO2 in the form of powder. In the present work, VO2 nanoparticles were prepared by hydrothermal synthesis in mild conditions, followed by a thermal annealing process at 700 °C under nitrogen flow for two hours. Vanadium pentoxide (V2O5) was used as the vanadium precursor, while two different reducing agents, namely oxalic and succinic acid, were employed for the reduction of V2O5 to VO2. Additionally, urea as well as thiourea were used as additives, in order to investigate their effects on the thermochromic performance of VO2. As a result, the VO2 (M) phase was obtained after annealing the crystalline powder, grown hydrothermally using oxalic acid and thiourea as a reducing agent and additive, respectively. This synthesis had a high yield of 90%, and led to a VO2(M) powder of high purity and crystallinity. In particular, the VO2 (M) nanoparticles had an average crystallite size of approximately 45 nm, a critical transition temperature of approximately 68 °C and a hysteresis width of 11 °C.

Background: Crystal violet dye is stable and difficult to be biodegraded owing to the existence of the multiple aromatic rings of the crystal violet molecules. Removing crystal violet dye from the wastewater is a major challenge. Objective: The aim of the research is to synthesize barium carbonate/tin dioxide nanoparticles and investigate the photocatalytic performance for the degradation of crystal violet. Methods: Barium carbonate/tin dioxide nanoparticles were synthesized via a facile hydrothermal route without any surfactants. The crystal structure, micro-morphology, size and optical performance of the barium carbonate/tin dioxide nanoparticles were investigated by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy and solid ultraviolet-visible diffuse reflectance spectrum. Results : The size of the barium carbonate/tin dioxide nanoparticles is 20 nm to 200 nm with the band gap of 3.71 eV. The photocatalytic activity of the barium carbonate/tin dioxide nanoparticles was measured by the photocatalytic degradation of crystal violet. The crystal violet degradation efficiency reaches 92.1% with the ultraviolet-visible irradiation time of 8 h using 10 mg barium carbonate/tin dioxide nanoparticles. The crystal violet degradation ratio increases to 96.1% when the dosage of the barium carbonate/tin dioxide nanoparticles increases to 20 mg/10 mL crystal violet dye solution. Active species capture photocatalytic experiments showed that the holes, hydroxyl radicals and superoxide ion radicals are the main active species. Reusability experiments displayed that the barium carbonate/tin dioxide nanoparticles are stable for the crystal violet dye degradation. Conclusion: The barium carbonate/tin dioxide nanoparticles show good photocatalytic performance toward crystal violet under ultraviolet light irradiation.

In the present study, a Bi$_2$WO$_6$/ZnWO$_4$ photocatalyst was successfully constructed by a modified hydrothermal synthesis method with different molar concentrations of Bi$_2$WO$_6$ with respect to ZnWO$_4$. The variation in molar concentrations of Bi$_2$WO$_6$ changed the photocatalytic properties of the Bi$_2$WO$_6$/ZnWO$_4$ catalyst. The synthesized Bi$_2$WO$_6$/ZnWO$_4$ photocatalyst was characterized by various techniques to decipher its structural and spectral properties. The interaction of Bi$^{2+}$ ionic charge carriers and many-body effects cause the band gap to narrow in Bi$_2$WO$_6$/ZnWO$_4$, as shown by PL analysis. The decrease in band gap energies (E$_g$) from 4.7 eV (ZnWO$_4$) to 3.5 eV (30% Bi$_2$WO$_6$/ZnWO$_4$) is beneficial because less energy is required to excite the valence electrons. The maximum degradation of Plasmocorinth B dye was found with 30% Bi$_2$WO$_6$/ZnWO$_4$ under UV irradiation. This increased activity of 30% Bi$_2$WO$_6$/ZnWO$_4$ can be attributed to the (i) synergistic effect in the bicrystalline framework of Bi$_2$WO$_6$ and ZnWO$_4$, (ii) the high close contact between Bi$_2$WO$_6$ and ZnWO$_4$, and (iii) the small crystallite size. The photocatalytic activity of synthesized Bi$_2$WO$_6$/ZnWO$_4$ photocatalyst shows its significant potential in water/ wastewater treatment application.

Glycerol steam reforming (GSR) is one of the promising technologies that can realize renewable hydrogen production and efficient utilization of crude glycerol. To illuminate the functions of Ca content (3%, 6%, 9%, and 12 %, by mass) and preparation method for Ni/ATP catalyst structure and its catalytic behaviors, the Ni-xCa/ATP (x=3%, 6%, 9%, and 12%, by mass) catalysts are prepared by co-impregnation (ci) and hydrothermal synthesis (hs) method and then tested in GSR. Characterization results of XRD, N2 adsorption-desorption, H2-TPR, HRTEM, XPS, and NH3/CO2-TPD demonstrate that the combined effect between appropriate Ca additive (6%, by mass) and hs enhance catalyst reducibility, uniform distribution of Ca additive and nickel species over ATP, and adsorption for CO2. This attributes to hs method protects the ATP framework through suppressing the interaction of Ca with ATP and promotes the formation of Ni-CaOx interface sites. Therefore, Ni-6Ca/ATP-hs exhibits the highest conversion (86.77%) of glycerol to gas product and H2 yield (76.17%) and selectivity (58.56%) during GSR. Furthermore, XRD, HRTEM, TG-DTG and Raman analyses confirm that Ni-6Ca/ATP-hs also reveals outstanding anti-sintering and coke resistance. In addition, the structural evolution process of Ni/ATP catalyst with Ca introduction and hs method is presented. Considering the high performance, simple preparation process and low cost, the as-prepared catalyst providing new opportunities for utilization of glycerol derived from biodiesel industry.

In this work we investigate the characteristics and feasibility of a new class of magnetic particles that are optimized for possible biological applications as magnetic hyperthermia. These new nanostructures have the nanoring shape, being composed of iron oxides (magnetite or hematite). Such morphology gives the nanoparticles a peculiar magnetic behavior due to their magnetic vortex state. The iron oxide nanorings were obtained using hydrothermal synthesis. X-ray Diffraction confirmed the existence of the desired crystal structure and Scanning Electron Microscopy shows that the magnetite particles had nanometric dimensions with annular morphology (diameter ~250 nm). The nanorings also show intensified magnetic properties and a transition to a vortex state. This study showed that it is possible to obtain magnetic nanorings with properties that can be used in nanotechnological applications (mainly biotechnological ones aimed at the treatment and diagnosis of cancer), in large quantities in a simple synthesis route.

The utilization of coal fly ash derived from circulating fluidized bed combustion (CFBFA) still faces great challenges because of its unique characteristics. In this study, a zeolitic material with Na-P1 zeolite as the main phase was successfully synthesized via a hydrothermal method by using CFBFA as the raw material. The effects of hydrothermal temperature, time, and added CTAB amount on the characterizations of synthesized materials were investigated by XRD, SEM, and XPS. The properties of the optimal zeolitic material and its adsorption performance for Pb2+ in aqueous solution were evaluated. The influences of pH, initial concentration, dosage, and temperature on Pb2+ adsorption were also examined. Results revealed the following optimal parameters for the synthesis of zeolitic material: NaOH concentration of 2 mol·L-1, solid-to-liquid ratio of 1:10 g·ml-1, hydrothermal temperature of 110 °C, hydrothermal time of 9 h, and CTAB amount of 1 g (per 100 ml solution). The adsorption capacities of the zeolitic material reached 329.67, 424.69, and 542.22 mg·g-1 when the pH values of aqueous solution were 5, 6, and 7, respectively. The Pb2+removal efficiency can reach more than 99% in aqueous solution with the initial concentrations of 100–300 mg·L-1 under pH 6 and suitable adsorbent dosage. The adsorption and kinetics of Pb2+ on the zeolitic material can be described by Langmuir isotherm and pseudo-second-order kinetic models, respectively. The ion exchange between Pb2+ and Na+ and chemisorption are the main adsorption mechanism. All these findings imply that the synthesis of low-cost adsorbent for Pb2+ removal from weak acid and neutral aqueous solution provides a highly effective method to utilize CFBFA.

A microstructured cover flow mixer equipped with two cyclone structures was used for stable continuous hydrothermal synthesis of ZnO nanoparticles from Zn(NO$_3$)$_2$ and NaOH aqueous solutions in supercritical water. The effects of the NaOH/Zn(NO$_3$)$_2$ ratio, Zn(NO$_3$)$_2$ molality, and flow rate on Zn conversion, crystal structure, particle size, particle morphology, and mixer clogging were examined. The advantages of this mixer were identified by comparing with the results obtained using the same chemical conditions with tee-type, cross-type, and central collision-type mixers.

In the present research work, iodine-doped iron tungstate has been reported for first time as an active photo-Fenton heterogeneous catalyst for wastewater treatment. In Fenton-like process, the catalytic efficiency of FeWO4 was enhanced greatly by introducing reductive non-metal species (I−) into the crystal lattice. This introduction activated the H2O2 for the generation of hydroxyl radicals which were the most reactive species for the degradation of RhB. The non-metal doping has enhanced the visible light response of transition metal oxide. A hydrothermal method was used for synthesizing novel iodine-doped FeWO4. The prepared sample was characterized through scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction spectroscopy, Fourier transform infrared spectroscopy, and UV–Visible spectroscopy. The photoactivity of I-FeWO4 was evaluated through the degradation of RhB under sunlight. I-FeWO4 showed 93.8% degradation of RhB after 80 min.

In this study, metallic glass is designed tunable for promising functional applications via a facile and stable, one-step process. Creative approach about alloy design and process is based on the unique properties of the Ti-Cu-Ni-Sn metallic glass that are afforded by the varying oxygen affinities of the four constituent elements. This metallic glass exhibits homogeneous nucleation of oxides and uniform formation of the various metal oxides. The alloy design and hydrothermal synthesis to customize the metallic glasses are the most critical factors that determine the characteristics of the metal oxides and the resulting nanostructures and photoelectrode properties. This enables the desired element to be selectively grown via a facile single-step process. These results provide a promising road map for the application of metallic glasses to photoelectrochemical (PEC) solar water splitting, as well as various other new possibilities.

In this work, vanadium and lanthanum co-doped ZnO/CNTs (VL-ZnO/CNTs) composites of large surface area and enhanced light assimilation range were produced for boosted hydrogen evolution from water. The photocatalysts were investigated for their morphological, structural, optical and photocatalytical properties. The photocatalytic activity of the composites was evaluated in pure water and in a mixture of water and methanol under simulated sunlight and visible light illumination. Under simulated sunlight irradiation, the maximum hydrogen generation rate of 925 μmolh−1g−1 from a combination of water and methanol was attained, which is almost 7 times higher than hydrogen generation rate achieved with pure ZnO. The VL-ZnO/CNTs photocatalyst resulted in hydrogen production rate of 267 μmolh−1g−1 from the water-methanol medium when exposed to visible light. This rate was about 3.5 folds lower than that achieved under simulated sunlight illumination. This improvement in hydrogen production rate is attributed to large surface area, high photo-response, better separation/transportation of the charge carriers and synergistic impact of V, La and CNTs in the designed photocatalyst.

The photocatalytic performance of the semiconductor CdS can be improved with carbon materials capable of limiting photocorrosion and the fast recombination of photogenerated charges. For this purpose, carbon derived from biomass exhibit several advantages including low cost, high abundance, and renewability. Here, photocatalytic CdS nanorods modified with carbon derived from the leaves of Japanese raisin trees were synthesized via a single hydrothermal step. Composite CdS nanorods with 5% biomass-derived carbon photocatalyzed H2 evolution 1.8 times faster than unmodified CdS at a rate of 5.71 mmol g−1 h−1. The apparent quantum efficiency of 5%C/CdS nanorods was 14.96%. Furthermore, the addition of biomass-derived carbon to CdS nanorods augmented the stability of the semiconductor under visible light. The characterization of the composite PC indicated that a larger specific surface area, as well as upgraded charge separation caused by biomass-derived carbon, were involved in the acceleration of photocatalytic hydrogen production.

The use of organic additives presents the greatest versatility and control of zeolite synthesis in order to prepare novel architectures for desired applications. Despite this prospect, there is little clarity of how organic additives are involved in framework assembly and the range of behaviours that are available. To address this issue, we have considered zeolites RHO and ZK-5 which can both be prepared using 18-crown-6 ether as an additive. Previously, this additive has shown to employ different structure directing behaviours to assemble a variety of zeolites. We have used high resolution powder X-ray diffraction and Rietveld refinement to determine structural models for zeolites RHO and ZK-5 with 18-crown-6 ether occluded in the framework. In doing so, we can observe the identity, location and orientation of the occluded additive and reason the structure directing behaviour in synthesis. We report that the isolated 18-crown-6 ether molecule is involved in the assembly of zeolite RHO, and for zeolite ZK-5 it is the K+ coordinated macrocation. In both cases the relevant additive is disordered in the framework, suggesting that they behave as space-filling species that stabilise the formation of the α-cage.

Vanadium dioxide is considered to be a promising material in most fields because of its special reversible metal-insulator transition (MIT) near ambient temperature. Pure VO2(M) is usually synthesized by a hydrothermal method combined with a subsequent annealing process or one-step hydrothermal synthesis. Both synthetic routes have the disadvantages of long reaction times. In this report, a new synthesis method of VO2(M) nanoparticles was established under liquid conditions. First, the V2O4·2H2O precursor was prepared successfully by using N2H4·2HCl-reduced V2O5 under thermostatic stirring without any reagent auxiliary. Second, the V2O4·2H2O suspension in water transformed into VO2(M) nanocrystals under hydrothermal synthesis. The intermediate and final products were characterized by XRD, SEM, HRTEM, XPS and DSC. The morphology of prepared VO2(M) exhibits a snowflake-like structure (approximately 1.0–4.0 μm in length, 0.5–3.0 μm in width and 50–200 nm in thickness). The phase-transition temperature is 65.49 °C. In addition, the reaction route of "V2O4·2H2O →V2O4·xH2O → VO2(B) → VO2(M) transformation" and reaction mechanism were established by testing the precipitate at different times at the hydrothermal stage.

Textile wastewater contains highly toxic, nondegradable, carcinogenic organic pollutants, causing severe damage to the ecological environment. In this work, β-cyclodextrin carbon-sphere-based nanocomposite (CS/SiO2@β-CD) with a core–shell–shell configuration was prepared by hydrothermal synthesis and subsequent sedimentation-azeotropic distillation with SiO2 as intermediate layer for the removal of crystal violet (CV) and bisphenol A (BPA). The chemical structure and morphology of the CS/SiO2@β-CD were characterized by FT-IR, SEM and TEM. The effects of contact time, pH, temperature and initial concentration of the absorbates on the adsorption property were explored. The CS/SiO2@β-CD showed excellent adsorption capacity on CV and BPA, and the maximum adsorption capacity was 87.873 mg g–1 and 165.095 mg g–1, respectively. Their adsorption process was in line with the pseudo-second-order and pseudo-first-order kinetic models, respectively. The adsorption thermodynamics could be better fitted by Langmuir model than by Freundlich model. The calculated thermodynamic parameters (–ΔG0, ΔS0 and ΔH0) illustrated the adsorption of CV was endothermic, in contrast, the adsorption of BPA was exothermic process. Furthermore, the CS/SiO2@β-CD showed excellent recovery performance, making it a potential adsorbent for the practical treatment of textile wastewater.

Nano-zirconia has been widely applied due to its excellent physical and chemical properties (e.g., high strength, corrosion resistance, oxygen ion conductivity). Existing preparation methods of nano-zirconia tend to require long reaction time, and the sizes of final particles are large with uneven distributions. Sub-/supercritical hydrothermal synthesis of nanoparticles is favored by researchers owing to controllable reaction process, uniform particle size distribution, good reproducibility, short reaction time, high conversion rate and harmlessness to environment. In this paper, the characteristics and mechanisms of dissolution, crystallization and growth of nano-zirconia during sub-/supercritical hydrothermal synthesis are systematically reviewed. The influences of process and material parameters on the size and purity of particles are analyzed. Then, the reaction mechanism and product phase transition mechanism during hydrothermal synthesis of zirconia are summarized to provide a theoretical reference for the oriented preparation. Finally, the improvement and commercialization of sub-/supercritical hydrothermal synthesis technology are evaluated, and the future research topics are proposed.

A large surface area with high active site exposure is desired for the nano-scaled electrocatalysts fabrication. Herein, taking NiMoO4 nanorods for example, we demonstrated the advantages of the microwave-assisted hydrothermal synthesis method compared to the traditional hydrothermal approaches. Both monoclinic structured NiMoO4 in the nanorods morphology are found for these samples but it is more time-saving and efficient in the Ni-Mo synergism for the catalyst obtained by microwave-assisted hydrothermal syntheses method. When evaluated for urea oxidation, the current density can reach 130.79 mA/cm2 at 1.54 V, about 2.4 times higher than that of the counterpart catalyst (54.08 mA/cm2). Moreover, largely improved catalytic stability, catalytic kinetics and rapid charge transfer ability are found on the catalyst obtained by the microwave-assisted approach. The high catalytic performance can be attributed to the high surface area and active site exposure of NiMoO4 nanorods formed by microwave irradiation. Considering the less time, facile synthesis condition and efficient components synergism, the microwave-assisted hydrothermal synthesis method might work better for the nanostructure electrocatalysts fabrication.

Crystallization of DNL-6, a silicoaluminophosphate (SAPO) based molecular sieve with the RHO topology, was investigated under both the hydrothermal synthesis (HTS) and dry-gel conversion (DGC) conditions. Crystallization of DNL-6 under the HTS conditions is rather fast. But a combination of crystallization under the DGC conditions and reducing reaction temperature slow down the reactions, allowing for intermediates to be captured. Under the DGC conditions, DNL-6 crystallizes through a semi-crystalline layered phase. The nature of this intermediate is aluminophosphate (AlPO) rather than SAPO with most P atoms having a local environment of P(–O–Al)3(OH). The surfactant (cetyltrimethylammonium chloride) used for synthesis appears to be part of the layered intermediate. Si is directly incorporated in the DNL-6 framework via SM II mechanism when the semi-crystalline AlPO phase is transforming to DNL-6 with the assistance of a very small amount of water. Both the structure directing agent and the surfactant play a role in the formation of DNL-6, as they were found within the final synthesized products. SEM data show that hydrothermal synthesis produces a much more crystalline product. The facts that the semi-crystalline layered phase was also observed in the powder X-ray diffraction patterns of the solid samples obtained under the HTS conditions and that the evolution of the local structure around P and Al in the intermediate phases are similar imply that under the reaction conditions employed in the present study, the formation pathways of DNL-6 under the HTS and DGC conditions appear to have some similarities.

The design and construction of bifunctional electrocatalysts with high activity and durability is essential for overall water splitting. Herein, a unique 3D hierarchical NiMo3S4 nanoflowers with abundant defects and reactive sites were grown directly on carbon textiles (NiMo3S4/CTs) using a facile hydrothermal synthesis method. The defect-rich NiMo3S4 nanoflakes, prepared by doping Ni2+ in the lattice of Mo-S, displays extended d-spacing of (0 0 2) crystal plane, resulting in the electrocatalytic activity of hydrogen evolution and oxygen evolution reaction (HER and OER) was improved under alkaline conditions. The self-supported NiMo3S4/CTs electrode delivers a small overpotential of 149.5 mV for HER and 126.2 mV for OER at 10 mA cm−2, respectively. Based on detailed structure analysis and density functional theory (DFT) calculations, the excellent HER and OER activities can be attributed to the unique structure of the nanoflowers, where the metallic characteristics for Ni-doped Mo-S lead to the enhancement of intrinsic conductivity and the rich abundance of Ni3+ active sites. As a result, the NiMo3S4/CTs as efficient bifunctional electrocatalysts for overall water-splitting was performed in alkaline electrolyte, where the system required only 1.55, 1.66 and 1.76 V to deliver current densities of 10, 50 and 100 mA cm−2, respectively. This study provides a new method for improving the electrocatalysis properties of transition metal sulfides by metal-ion doping to generate more active defect sites, thus promoting the development of non-noble-metal electrocatalysts for overall water splitting.

FeOOH and FeOOH@ZnO were prepared by hydrothermal synthesis, and their structures and adsorption properties toward S2− were studied. The results showed that too high hydrothermal temperature was not conducive to the adsorption of S2−. However, using sodium dodecyl sulfate (SDS) for FeOOH preparation and adding nanometer ZnO (FeOOH@ZnO) could significantly improve the adsorption of S2− by FeOOH, and adsorption removal rate was close to 90.0% and adsorption amount was 87.5 mg·g−1. The structural analysis showed that the modification of FeOOH by SDS and the addition of nano-ZnO resulted in the reduction in size of the FeOOH particles, forming amorphous inclusion structure with ZnO present inside and FeOOH outside. The specific surface area of FeOOH@ZnO was found to be higher than that of FeOOH. Therefore, it is beneficial to the adsorption of S2−. XPS fitting results showed that ferrous deposits appeared in the process of adsorption of S2− by FeOOH@ZnO, and it was considered that the oxygen of Fe = O was replaced with sulfur.

ZnO nanorods combined with different concentrations of reduced graphene oxide were synthesized using the hydrothermal method. Structural properties of these nanocomposites were studied by X-ray diffraction analysis. Morphological studies on the shape and size of nanorods were carried out by scanning electron microscopy. X-ray diffraction results revealed highly-crystalline nanorods with a hexagonal wurtzite structure. The morphology of as prepared samples is characterized presence of one-dimensional rod-like nanostructures. Crystallite size, stress and lattice strain were determined by Scherrer equation and Williamson–Hall method. The average particle size of samples calculated from microstructural and morphological analyses are highly interrelated. Microraman spectra exhibited both characteristic bands of ZnO and reduced graphene oxide in the low frequency (300–500 cm−1) and high frequency (1300–1600 cm−1) ranges, respectively, furthermore confirming the efficiency of the hydrothermal synthesis of ZnO/reduced graphene oxide nanocomposites. The band gap of the nanocomposite is lower (2.96 eV).compared to that of ZnO (3.10 eV), as determined from the analysis of UV absorbance spectra.

Polypyrrole/Fe2O3 (PPy/Fe2O3) nano-seeds with distinctive electrochemical properties have been successfully synthesized using improved hydrothermal processes. The study highlights the nano-seed like morphology of polypyrrole/Fe2O3 achieved by lowering both the reaction temperature and time (150 ℃ for 4 h), which are appreciable for energy storage applications. The obtained PPy/Fe2O3, analyzed using different techniques like X-ray photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscopy (FESEM), Fourier Transform Infrared (FTIR) spectroscopy. Compositional and morphological studies confirmed the formation of interconnected PPy/Fe2O3 nano-seeds. Cyclic Voltammetry response displays superior electrochemical performance of the PPy/Fe2O3. The interconnected nanostructures with voids allow more electrolyte ions to contact the active material, which significantly increases conductivity and electrochemical performance. As compared to the reported hydrothermal methods, the optimized routes take 4 h to achieve a specific nano-seed like morphology which is favorable for energy storage application.

Transition metal molybdates/carbonates and hybrid nanomaterials have attracted great attention in energy storage applications because of their enriched redox activity, good electronic conductivity, and stable crystallinity. We synthesize a multicomponent MnMoO4/MnCO3 hybrid by a one-step hydrothermal method with urea as the reaction fuel. By controlling only the urea concentration in the initial precursor solution, the MnMoO4/MnCO3 molecular ratio is controlled effectively, which is found to have a profound effect on the electrochemical properties of the hybrid electrodes. The electrochemical measurements show that the specific capacitance of MnMoO4/MnCO3 hybrid is 1311 F/g, the energy density of 116.8 Wh/kg, and power density of 383 W/kg at a current density of 1 A/g with 79% capacitance retention over 5000 cycles. The fabricated asymmetric supercapacitor device exhibits good energy storage performance, including the specific capacitance of 97 F/g along with the energy density of 26.5 Wh/kg and the power density of 657 W/kg at a current density of 1 A/g and good reversibility with capacitance retention of 85% after 2000 cycles and 70% over 5000 cycles. The increase in the energy density of 900% with a mere 60% decrement in the energy density indicates its potential superior applications in high-power devices.

Niobium-based oxides can be used in several applications due to a diverse set of properties. In this work, Na2Nb2O6.H2O sodium niobate nanowires were obtained by hydrothermal synthesis at low temperature. Dehydrated sodium niobate (Na2Nb2O6) and sodium niobate with perovskite structure (NaNbO3) were obtained by submitting Na2Nb2O6.H2O to heat treatment (350 °C and 500 °C, respectively). To obtain protonic niobates, sodium niobates were immersed in nitric acid in order to promote ion exchange reactions. From this procedure, protonic niobates (H3O)2Nb2O6.H2O and (H3O)2Nb2O6 were obtained. The sample NaNbO3 did not undergo any transformation. Cyclic voltammetry tests carried out in a neutral aqueous solution 1 M Na2SO4 showed a wide potential window for both niobates (sodium and protonic). However, the protonic niobate samples (H3O)2Nb2O6.H2O and (H3O)2Nb2O6 presented much higher current density values than the sodium niobates. This result can be related to a structural rearrangement that allowed a significant increase in the intercalation of sodium Na + ions from the electrolyte into the structure of these protonic niobates, when polarized. Therefore, in this work, it was demonstrated that it is possible to obtain protonic niobates from sodium niobates, as well as, it was verified the distinct electrochemical behavior between these materials.

A novel nano-heterojunction photocatalysts of CdS/MoS2 with appropriate interfacial contact was successfully obtained by the facile two-step hydrothermal synthesis. The MoS2 ultrathin layer was well combined with CdS nanosheets and formed the interaction, which facilitated the transfer and separation of charges. The CdS/MoS2 15 wt% possessed much higher H2 evolution photocatalytic performance (35.24 mmol h−1 g−1), exhibiting an 85.95 times enhancement as compared to that of pure CdS (0.41 mmol h−1 g−1). Moreover, the photochemical stability of CdS/MoS2 heterojunctions was excellent, which showed no significant decrease in activity after four cycles of experiments. The finding provides a novel method to integrate the structure of MoS2 with CdS, which exhibits great potential in solar energy conversion.

In this investigation, ZnO nanostructures were coated via hydrothermal process on glass substrate surfaces, which were treated by acidic and alkaline solutions. Furthermore, the ZnO structure was doped by different amounts of Al+3 ions to investigate the microstructural variation. Characteristics of the samples by XRD and SEM analyses confirmed the formation of different morphologies and various crystal sizes for the nanostructured ZnO on the substrates including nanoflower, nanorod, and nanopanel morphologies. Furthermore, XRD results showed that the Zn2+ concentration was a crucial factor in changing the grain size. EDS analysis confirmed the uniform distribution of Al dopant, while the FTIR spectra revealed the presence of Al–O and Zn–O stretching bonds in the coatings. The results confirmed that the sample, which was etched by fused NaOH had a uniform and compacted structure. Moreover, it was evident the proposed treatment and synthesis process was successful in the formation of uniform nanostructured ZnO film on the glass substrate without the requirement for seed layer deposition.

This communication reports hydrothermal synthesis of molybdenum trioxide (MoO3) with long microsheets morphology and their gas sensing characteristics through clad-modified fiber optic gas sensor technique. Synthesized material is subjected to characterization analysis including XRD, SEM and Raman Spectra. Spectral analysis on the gas sensing characteristics reveal that MoO3 microsheets exhibit good gas response to methanol at room temperature. Gas sensing mechanism is also discussed.

We have developed an efficient strategy to synthesize an active and durable electrocatalyst of Pd hydride nanocubes (NCs). Instead of the traditional chemical method, the PdH0.43 NCs are firstly prepared via a hydrogen diffusion procedure, followed by hydrothermal synthesis of an amorphous CuO layer encapsulating the PdH0.43 NCs to prevent the hydrogen atoms from escaping. Obvious lattice expansion is demonstrated playing a pivotal role in the enhancement of their oxygen reduction reaction (ORR) activity and durability. The obtained PdH0.43@CuO NCs catalysts exhibit an ORR mass activity of 0.18 A mg−1 at 0.90 V versus reversible hydrogen electrode in an alkaline medium, which is about five times higher than that of commercial Pt/C. Accelerated durability tests show that there is only a 32 mV decay in half-wave potential even after 10,000 potential cycles, indicating the excellent stability of PdH0.43@CuO NCs. Density functional theory (DFT) calculations also indicate that, compared to Pd, PdH0.43 has a lower limiting barrier to form OH− during the ORR process. The present study illustrates the importance of lattice expansion caused by hydrogen and offers an available strategy to design highly efficient and durable Pd-based electrocatalysts for alkaline fuel cells.

The wide use of manganese dioxide (MnO2) as an electrode in all-solid-state asymmetric supercapacitors (ASCs) remains challenging because of its low electrical conductivity. This complication can be circumvented by introducing trivalent gadolinium (Gd) ions into the MnO2. Herein, we describe the successful hydrothermal synthesis of crystalline Gd-doped MnO2 nanorods with Ni(OH)2 nanosheets as cathode, which we combined with Fe3O4/GO nanospheres as anode for all-solid-state ASCs. Electrochemical tests demonstrate that Gd doping significantly affected the electrochemical activities of the MnO2, which was further enhanced by introducing Ni(OH)2. The GdMnO2/Ni(OH)2 electrode offers sufficient surface electrochemical activity and exhibits excellent specific capacity of 121.8 mA h g−1 at 1 A g−1, appealing rate performance, and ultralong lifetime stability (99.3% retention after 10,000 discharge tests). Furthermore, the GdMnO2/Ni(OH)2//PVA/KOH//Fe3O4/GO solid-state ASC device offers an impressive specific energy density (60.25 W h kg−1) at a high power density (2332 W kg−1). This investigation thus shows its large potential in developing novel approaches to energy storage devices.

Manganese dioxide compounds are widely used in electrochemical applications e.g. as electrode materials or photocatalysts. One of the most used polymorphs is gamma-MnO2 which is a disordered intergrowth of pyrolusite beta-MnO2 and ramsdellite R-MnO2. The presence of intergrowth defects alters the material properties, however, they are difficult to characterise using standard X-ray diffraction due to anisotropic broadening of Bragg reflections. We here propose a characterisation method for intergrown structures by modelling of X-ray diffraction patterns and pair distribution functions (PDF) using gamma-MnO2 as an example. Firstly, we present a fast peak-fitting analysis approach, where features in experimental diffraction patterns and PDFs are matched to simulated patterns from intergrowth structures, allowing quick characterisation of defect densities. Secondly, we present a structure-mining-based analysis using simulated gamma-MnO2 superstructures which are compared to our experimental data to extract trends on defect densities with synthesis conditions. We applied the methodology to a series of gamma-MnO2 samples synthesised by a hydrothermal route. Our results show that with synthesis time, the intergrowth structure reorders from a R-like to a beta-like structure, with the beta-MnO2 fraction ranging from ca. 27 to 82% in the samples investigated here. Further analysis of the structure-mining results using machine learning can enable extraction of more nanostructural information such as the distribution and size of intergrown domains in the structure. Using this analysis, we observe segregation of R- and beta-MnO2 domains in the manganese oxide nanoparticles. While R-MnO2 domains keep a constant size of ca. 1-2 nm, the beta-MnO2 domains grow with synthesis time.

An improved hydrothermal synthesis of shape-controlled, size-controlled 60 nm SrTiO3 nanocuboid (STO NC) supports, which facilitates the scalable creation of platinum nanoparticle catalysts supported on STO (Pt/STO) for the chemical conversion of waste polyolefins, is reported herein. This synthetic method (1) establishes that STO nucleation prior to the hydrothermal treatment favors nanocuboid formation, (2) produces STO NC supports with average sizes ranging from 25 to 80 nm with narrow size distributions, and (3) demonstrates how SrCO3 formation and variation in solution pH prevent the formation of STO NCs. The STO synthesis was scaled-up and conducted in a 4 L batch reactor, resulting in STO NCs of comparable size and morphology (m = 22.5 g, davg = 58.6 ± 16.2 nm) to those synthesized under standard hydrothermal conditions in a lab-scale 125 mL autoclave reactor. Size-controlled STO NCs, ranging in roughly 10 nm increments from 25 to 80 nm, were used to support Pt deposited through strong electrostatic adsorption (SEA), a practical and scalable solution-based method. Using SEA techniques and an STO support with an average size of 39.3 ± 6.3 nm, a Pt/STO catalyst with 3.6 wt % Pt was produced and used for high-density polyethylene hydrogenolysis under previously reported conditions (170 psi H2, 300 °C, 96 h; final product: Mw = 2400, Đ = 1.03). As a well-established model system for studying the behavior of heterogeneous catalysts and their supports, the Pt/STO system detailed in this work presents a unique opportunity to simultaneously convert waste plastic into commercially viable products while gaining insight into how scalable inorganic synthesis can support transformative manufacturing.

Die kontinuierliche hydrothermale Synthese (CHTS) stellt ein vielversprechendes Verfahren zur Herstellung metalloxidischer Nanopartikel dar. Das Prinzip beruht auf der Vermischung einer kalten wässrigen Metallsalzlösung mit einem nahe-/überkritischen Wasserstrom. Durch die außergewöhnlichen Eigenschaften des überkritischen Wassers kommt es zur Partikelbildung. Neben der Studie des Einflusses der Prozessparameter auf die resultierende Partikelgröße und -verteilung ist die Restkonzentration an gelöstem Metallsalz von Interesse. Diese kann mittels der Impedanzspektroskopie analysiert werden. Dazu werden an einer modifizierten CHTS-Anlage Vorversuche durchgeführt, um zukünftig die Restkonzentration direkt bestimmen zu können.

Developing environmentally friendly methods to produce hydrogen peroxide (H2O2) has received increasing attention. Photocatalysis has been proved to be a sustainable technology for H2O2 production. Herein, the novel non-metal elements (B, P, and S) doped g-C3N4 tubes (B-CNT, P-CNT, and S-CNT) photocatalysts were obtained via a hydrothermal synthesis followed by thermal polymerization. By adjusting the precursor, the yield of g-C3N4 tubes (CNT) materials has been greatly improved. The as-prepared B-CNT, P-CNT, and S-CNT photocatalysts show an enhanced photocatalytic H2O2 production with the formation rate constants values of 42.31 μM min−1, 24.95 μM min−1, and 24.22 μM min−1, respectively, which is higher than that of bulk CN (16.40 μM min−1). The doped B, P, S elements significantly enhanced the photocatalytic activity by adjusting their electronic structures and promoting the separation of electron-hole carriers. The results have shown great potential for the practical application of CNT photocatalysts.

Supercapacitor with high specific capacity is desirable for various energy storage and high powerdensity applications. Though Graphene has been the preferred material for high current density, nanocomposites have been attempted to increase the specific capacitance. Hydrothermal synthesis of cadmium sulfide/graphene (CdS/G) nanocomposite with CdS nanoparticles anchored/decorated over the graphene sheets is reported. The structural studies reveal the hexagonal phase of the prepared materials. The specific surface area (BET) and porosity is found to increase upon nanocomposite formation. The electrochemical characteristics such as cyclic voltammetry (CV), GCD and EIS of the CdS/G nanocomposite have been investigated. The capacitance of CdS/G nanocomposite almost doubled to 248 Fg−1 indicating the enhanced performance of the nanocomposite system and in addition it also showed excellent cycling stability of 74.8 percent after 1000 cycles. The supercapacitor investigated retained the initial energy density after charge-discharge, at 0.5 A/g for 1000 cycles. The graphene nanosheets increased the specific surface area and interfacial electron transfer of the composite material. It enhances the specific capacitance and cyclic stability of the supercapacitor device.

A series of Mo-containing MFI zeolites with different Mo loadings (Mo-MFI-n, n represent the initial Si/Mo molar ratio) was hydrothermally synthesized by using tetrapropylammonium hydroxide as the template and Mo-EDTA complex as the Mo source. Various characterization results demonstrated that the use of the Mo-EDTA complex is beneficial for the incorporation of more Mo species into the MFI-type zeolites. The special complexing capability of EDTA2– plays a critical role in adjusting the release rate of the Mo species to combine with the Si tetrahedron species during the zeolite growth process, thus leading to a uniform distribution of Mo in the MFI framework. In addition, a small portion of extra-framework Mo clusters may be distributed inside the channels or near the pore window of the zeolites. The catalytic properties of these Mo-containing MFI zeolites were evaluated for the epoxidation of cyclohexene with H2O2 as the oxidant. The composition-optimized catalyst, Mo-MFI-50, efficiently converted cyclohexene to the corresponding epoxide with a relatively high conversion (93%) and epoxide selectivity (82%) at 75 °C after 9 h of reaction. Moreover, the resultant Mo-containing MFI catalyst exhibited excellent structural stability and recoverability and was easily recycled by simple filtration without the need for calcination treatment.

Phosphorylated chitosan (P-CS) was successfully synthesized using a facile experimental setup of hydrothermal method that was applied to the adsorption of anionic Acid Red 88 (AR88) from aqueous media. The adsorption process obeyed the pseudo-second-order (PSO) kinetic model. In contrast, the adsorption isotherm conformed to the Langmuir model, with the maximum adsorption capacity (qm = 230 mg g−1) at 303 K. Both external and intraparticle diffusion strongly influenced the rate of adsorption. The insights from this study reveal that P-CS could be easily prepared and regenerated for reusability applications. The adsorption mechanism and intermolecular interaction between P-CS and AR 88 were investigated using Fourier transform infrared (FTIR) spectroscopy and calculations via Density Functional Theory (DFT). The key modes of adsorption for the P-CS/AR 88 system are driven by electrostatic attractions, H-bonding, and n-π interactions. The findings herein reveal that P-CS is a promising adsorbent for the removal of anionic dyes such as AR88 or similar pollutants from water.

In this paper, CeVO4 nanostructures were produced with controlled hydrothermal method using hydrazine, cerium nitrate, and ammonium vanadate as reactants. Reaction control was performed utilizing hydrazine and ethylenediamine as new reactants. Other effective parameters such as solvent and surfactant were also carefully studied and optimized. The products were then identified through XRD, EDS, FTIR, FESEM, and BET analyses. FESEM results showed that by adjusting the concentration of ethylenediamine, hydrazine, and PVP surfactant, a rod-shaped morphology with suitable porosity could be created. Due to the high potential of CeVO4 in electrochemical processes, it was first employed for electrochemical storage of hydrogen. The amount of hydrogen storage in nanostructures produced with rod-shaped morphology was about 2575 mAh/g, which is very significant compared to products obtained with sodium hydroxide with spherical morphology.

Propane dehydrogenation (PDH), employing Pt- or Cr-based catalysts, represents an emerging industrial route for propylene production. Due to the scarcity of platinum and the toxicity of chromium, alternative PDH catalysts are being pursued. Herein, we report the construction of Zn-containing zeolite catalysts, namely Zn@S-1, for PDH reaction. Well-isolated zinc cations are successfully trapped and stabilized by the Si-OH groups in S-1 zeolites via in-situ hydrothermal synthesis. The as-prepared Zn@S-1 catalysts exhibit good dehydrogenation activity, high propylene selectivity, and regeneration capability in PDH reaction under employed conditions. The in-situ partial reduction of zinc species is observed and the partially reduced zinc cations are definitely identified as the active sites for PDH reaction.

NiMoS2 is a promising material for various functional applications and highly compatible with GO to make hybrid nanocomposites with excellent characteristics for supercapacitor electrode material. Deposition of NiMoS2 was achieved on the rGO(reduced Graphene Oxide) surface to form a NiMoS2−rGO nanocomposite by the method of the facile hydrothermal synthesis process. XRD pattern shows the crystalline nature of composites. Raman and EPMA result interpreting the composites formation and elements compositions, respectively. The sheet-like morphology of rGO was found in the composites by FESEM images. Particles distribution was confirmed by HR-TEM. The electrochemical properties of the pure NiMoS2 and NiMoS2–rGO composites have been studied by cyclic voltammetry analysis. The results revealed that the NiMoS2/5% rGO nanocomposites exhibit high specific capacitance compared to pure NiMoS2 due to the synergistic effects of NiMoS2 and rGO in the composite material. The photocatalytic behavior of the prepared nanocomposites for dye degradation was tested. The quantity of rGO has significantly improved the photocatalytic behavior of NiMoS2/rGO composites. The studies on degradation mechanism, the N2 adsorption/desorption isotherms, pore size distribution behavior and % of removal of MB reveal the enhanced photocatalytic performance of sysnthesised composites.

Zeolites are the most used solid catalysts in the chemical industry. The hydrothermal synthesis of these porous aluminosilicate crystals is a multistep process that involves the polymerization of s...

The synthesis of magnetic iron–carbon composites (Fe/C) from waste avocado seeds via hydrothermal carbonization (HTC) has been demonstrated for the first time. These materials are shown to be effective in adsorption and catalytic applications, with performances comparable to or higher than materials produced through conventional processing routes. Avocado seeds have been processed in high-temperature water (230 °C) at elevated pressure (30 bar at room temperature) in the presence of iron nitrate and iron sulfate, in a process mimicking natural coalification. Characterization of the synthesized material has been carried out by X-ray diffraction (XRD), atomic absorption spectroscopy (AAS), X-ray fluorescence (XRF), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma-optical emission spectrometry (ICP-OES), Fourier-transform infrared spectroscopy (FT-IR), magnetometry, and through surface area measurements. The supported iron particles are observed to be predominately magnetite, with an oxidized hematite surface region. The presence of iron catalyzes the formation of an extended, ordered polymeric structure in the avocado seed-derived carbon. The magnetic Fe/C has been demonstrated as an adsorbent for environmental wastewater treatment using methylene blue and indigo carmine. Kinetic analysis suggests that the adsorbates are chemisorbed, with the positive surface charge of Fe/C being preferential for indigo carmine adsorption (49 mg g–1). Additionally, Fe/C has been evaluated as a heterogeneous catalyst for the hydroalkoxylation of phenylacetylene with ethylene glycol to 2-benzyl-1,3-dioxolane. Product yields of 45% are obtained, with 100% regioselectivity to the formed isomer. The solid catalyst has the advantages of being prepared from a waste material and of easy removal after reaction via magnetic separation. These developments provide opportunities to produce carbon-based materials for a variety of high-value applications, potentially also including energy storage and biopharmaceuticals, from a wide range of lignocellulosic biomass feedstocks.

The high energy demand of CO2 absorption-desorption technologies has significantly inhibited their industrial utilization and implementation of the Paris Climate Accord. Catalytic solvent regeneration is of considerable interest due to its low operating temperature and high energy efficiency. Of the catalysts available, heterogeneous catalysts have exhibited relatively poor performances and are hindered by other challenges, which have slowed their large-scale deployment. Herein, we report a facile and eco-friendly approach for synthesizing water-dispersible Fe3O4 nanocatalysts coated with a wide range of amino acids (12 representative molecules) in aqueous media. The acidic properties of water-dispersible nanocatalysts can be easily tuned by introducing different functional groups during the hydrothermal synthesis procedure. We demonstrate that the prepared nanocatalysts can be used in energy-efficient CO2 capture plants with ease-of-use, at very low concentrations (0.1 wt %) and with extra-high efficiencies (up to ∼75% energy reductions). They can be applied in a range of solutions, including amino acids (i.e., short-chain, long-chain, and cyclic) and amines (i.e., primary, tertiary, and primary-tertiary mixture). Considering the superiority of the presented water-dispersible nanocatalysts, this technology is expected to provide a new pathway for the development of energy-efficient CO2 capture technologies.