Hydrothermal Synthesis Research Articles

The Formation Mechanism of Carbonized Polymer Dots: Crosslinking-Induced Nucleation and Carbonization.

Carbon dots (CDs), as a kind of zero-dimensional nanomaterials, have been widely synthesized by bottom-up methods from various precursors. However, the formation mechanism is still unclear and controversial, which also brings difficulty to the regulation of structures and properties. Only some tentative formation processes were postulated by analyzing the products obtained at different reaction times and temperatures. Here, the effect of crosslinking on the formation of carbonized polymer dots (CPDs) is explored. Crosslinking-induced nucleation and carbonization (CINC) is proposed as the driving force for the formation of CPDs. Under hydrothermal synthesis, the precursors are initiated to polymerize and crosslink. The crosslinking brings higher hydrophobicity to generate the hydrophilic/hydrophobic microphase separation, which promotes dehydration and carbonization resulting in the formation of CPDs. Based on the principle of CINC, the influence factors of size are also revealed. Moreover, the dissipative particle dynamics (DPD) simulation is employed to support this formation mechanism. This concept of CINC will bring light to the formation process of CPDs, as well as facilitate the regulation of CPDs' size and photoluminescence.

Microwave hydrothermal synthesis and characterization of aluminum substituted tobermorite

Microwave hydrothermal synthesis and characterization of aluminum substituted tobermorite

Enhancing Bioactivity and Mechanical Properties of Nano-Hydroxyapatite Derived from Oyster Shells through Hydrothermal Synthesis

Nano-hydroxyapatite (nHA) demonstrates favorable biological activity, cell adhesion, cell proliferation, and osteoconductivity, making it highly valuable in biomedicine. It is extensively used as a bone substitute and in bone transplantation within the dental and orthopedic fields. This study employed oyster shells as a calcium source to synthesize nHA at 150 °C with various hydrothermal reaction durations (10 min, 1 h, 6 h, and 12 h). As a control, HA synthesized via a wet precipitation method for 1 h at room temperature was utilized. Subsequent material analyses, including XRD, FE-SEM, FTIR, and ICP-MS, were conducted, followed by comprehensive evaluations of the bioactivity, cell attachment, cell proliferation, and sintering properties of the synthesized nHA. The results indicated that nHA synthesized through the hydrothermal reaction produced nanoscale crystals, with the aspect ratio of nHA particles increasing with the duration of hydrothermal treatment. Notably, rod-like nHA particles became prominent with hydrothermal durations exceeding 6 h. nHA particles derived from oyster shells contained carbonate and trace elements (Na, Mg, K, and Sr), similar to constituents found in human hard tissue such as bone and teeth. The immersion of nHA synthesized at 150 °C for 1 h (HT2) in simulated body fluid (SBF) for 28 d led to the formation of a bone-like apatite layer on the surface, indicating the excellent bioactivity of the synthesized nHA. The cell culture results revealed superior cell attachment and proliferation for nHA (HT2). Following the sequential formation and sintering at 1200 °C for 4 h, HT2 ceramics exhibited enhanced microhardness (5.65 GPa) and fracture toughness (1.23 MPa·m0.5), surpassing those of human tooth enamel.

Direct Hydrothermal Synthesis and Characterization of Zr–Ce-Incorporated SBA-15 Catalysts for the Pyrolysis Reaction of Algal Biomass

In recent years, algae have emerged as a promising feedstock for biofuel production, due to their eco-friendly, sustainable, and renewable nature. Various methods, including chemical, biochemical, and thermochemical processes, are used to convert algal biomass into biofuels. Pyrolysis, a widely recognized thermochemical technique, involves high temperature and pressure to generate biochar and bio-oil from diverse algal sources. Various pyrolytic processes transform algal biomass into biochar and bio-oil, including low pyrolysis, fast pyrolysis, catalytic pyrolysis, microwave-assisted pyrolysis, and hydropyrolysis. These methods are utilized to convert a range of microalgae and cyanobacteria into biochar and bio-oil. In this publication, we will discuss catalytic pyrolysis using mesoporous materials, such as SBA-15. Mesoporous catalysts have earned significant attention for catalytic reactions, due to their high surface area, facilitating the better distribution of impregnated metal. Pyrolysis conducted in the presence of a mesoporous catalyst is viewed more as efficient, compared to reactions occurring within the smaller microporous cavities of traditional zeolites. SBA-15 supports with incorporated Zr and/or Ce were synthesized using the direct hydrothermal synthesis method. The catalyst was characterized using structural and morphological technical analysis and utilized for the pyrolysis reaction of the algal biomass.

Temperature-Sensitive Template for Preparation of ZnO/CeO2 Composite Photocatalytic Materials and Its Catalytic Performance

In this work, a series of thermosensitive ionic liquid functionalized polymers, PNx(IL)y, with controllable morphology and particle size were prepared by free radical polymerization. Then, using the polymer PN64(IL)8 with uniform morphology as a templating agent, the ZnO composite photocatalytic materials doped with rare earth metal Ce were prepared in combination with a microwave-assisted and templated hydrothermal reaction method. Series different Ce-doping amount photocatalytic materials ZnO-Ce-x‰ were characterized by XRD, SEM, TEM, XPS, and other methods. The results demonstrated that the templated materials PN64(IL)8 can prepare ZnO-Ce-2‰ with uniform petaloid ambulacra shape, good distribution of elements, and excellent photocatalytic performance. Photocatalytic degradation experiments of methyl orange (MO) showed that when the Ce-doping amount is only 2‰, the degradation rate of organic dyes can reach 96.5% by reacting the photocatalytic materials in water for 1 h. In addition, this kind of photocatalyst can be used for the degradation of high-concentration MO, as well as being easily recovered and effectively reused by simple filtration. Therefore, the structure of this kind of photocatalyst is controllable in the preparation process with an extremely low Ce-doping amount compared with current reports, and it has a good application prospect in the field of wastewater treatment technology.

Boosting the Electrical Transfer by Molybdenum Doping for Robust and Flexible NiSe-Based Supercapacitor.

NiSe is a promising electrode material for enhancing the energy density of supercapacitors, but it faces challenges such as sensitivity to electrolyte anions, limited specific capacity, and unstable cycling. This study employs a strategy of metal atom doping to address these issues. Through a hydrothermal reaction, Mo-doped NiSe demonstrates significant improvement in electrochemical performance, exhibiting high capacity (799.90Cg-1), splendid rate performance, and excellent cyclic stability (90% capacity retention). The introduction of Mo induces charge redistribution in NiSe, leading to a reduction in the band gap. Theoretical calculation reveals that Mo doping can effectively enhance the electrical conductivity and the adsorption energy of NiSe. A flexible printed hybrid Mo-doped NiSe-based supercapacitor is fabricated, demonstrating superior electrochemical performance (367.04mFcm-2) and the ability to power timers, LEDs, and toy fans. This research not only deepens the understanding of the electrochemical properties of metal-doped NiSe but also highlights its application potential in high-performance supercapacitors.

One-pot hydrothermal synthesis of transition metal sulfides-decorated CuS microflower-like structures for electrochemical CO2 reduction to CO

Electrochemical CO2 reduction (ECR) to value-added products is regarded as a sustainable strategy to mitigate global warming and energy crisis, and designing highly efficient and robust catalysts is essential. In this work, transition metal sulfides (TMS)-decorated CuS microflower-like structures were prepared via the one-pot hydrothermal synthesis method for ECR to CO, and the influence of TMS doping on ECR performance was demonstrated. Characterization of the catalysts was performed using XRD, FESEM-EDS, N2 physisorption, and XPS, revealing the successful loading of TMS, the formation of microflower-like architectures and the generation of sulfur vacancies. Electrochemical tests demonstrated that doping ZnS, Bi2S3, CdS and MoS2 improved the intrinsic CO2 reduction activity of the CuS catalyst. Particularly, the MoS2-CuS composite catalyst with imperfect petal-like structure showed uniform distribution of edge Mo sites, which worked synergistically with the formed grain boundaries (GBs) and undercoordinated S vacancy sites in promoting CO2 activation, stabilizing *COOH adsorption, facilitating *CO desorption, and lowering the energy barrier of the potential-limiting step for improved CO selectivity. The MoS2-CuS catalyst achieved a maximum CO selectivity of 83.2% at –0.6 V versus the reversible hydrogen electrode (RHE) and a high CO cathodic energetic efficiency of 100%. At this potential, the catalyst maintained stable catalytic activity and CO selectivity during a 333-min electrolysis process. The findings will offer a promising avenue for the development of efficient and stable catalysts for CO production from ECR.

Enhanced non-enzymatic multicomponent detection via one-step hydrothermal synthesis of widely dispersed Zn-SnO2 nanoparticles on nitrogen-doped reduced graphene oxide

ABSTRACT Herein, we report a new type of non-enzymatic nanostructured biosensor designed for the concurrent determination of dopamine, cholesterol, and glucose in human blood samples. The prepared biosensor using low-temperature one-pot hydrothermal processing is a Zn-doped SnO2-dispersed nitrogen-doped reduced graphene oxide (N-rGO)/Zn-SnO2 nanocomposite. This modified electrode allows direct electron transfer and thus offers electrochemical techniques to detect target molecules in analytes without the use of enzymes. The biosensor displayed good voltammetric responses within the human reference range: 20–70 nM for dopamine, 1–8 mM for cholesterol, and 1–10 mM for glucose. It also showed excellent reusability and can be restored by washing with ethanol. Due to the use of Zn-doped SnO2 nanoparticles for enhanced catalytic activity and N-rGO for high conductivity and active sites, sensitive and selective detection can be achieved. This hybrid composite demonstrates excellent catalytic activity, repeatability, stability, and clinical comparability for real-time measurement of dopamine, cholesterol, and glucose simultaneously.

Enhanced removal of sulfamethoxazole via adsorption and photodegradation using biochar-modified iodine-doped TiO2 photocatalysts under simulated sunlight

This study aimed to prepare a biochar-modified iodine-doped titanium dioxide composite photocatalyst (B/I-TiO2) via hydrothermal reaction and evaluate its performance in sulfamethoxazole (SMX) degradation under simulated sunlight. Biochar was prepared from four agricultural wastes using hydrothermal and pyrolysis technologies, resulting in 3–30 graphite layers with a d-spacing of 0.35 nm. Hydrothermal activation transformed the disordered structure into a graphite microcrystalline structure, producing biochar with a quasi-three-dimensional graphene structure. Doping with 1–15 wt% of this biochar shifted the characteristic wavelength of B/I-TiO2 to 423–426 nm and increased the specific surface area by 1.25–1.94 times. The 5LB700H2I1T composite photocatalyst found the highest SMX removal efficiency of 40 %, and the 5WB900H2I1T composite photocatalyst found the highest SMX photodegradation efficiency of 30 %, respectively, irradiated with simulated sunlight of 3 hours. The wavelength redshift and degradation performance enhancement primarily resulted from iodine doping and the biochar's excellent crystallinity and high surface area. SMX removal was achieved through adsorption and photodegradation, with hydroxyl radicals and electron holes playing a significant role compared to superoxide radicals.

Comparative microstructural analysis of V2O5 nanoparticles via X-ray diffraction (XRD) technique.

Vanadium Pentoxide (V2O5) nanoparticles exhibit diverse properties and have been studied for a wide range of applications, including energy storage, catalysis, environmental remediation, and material enhancement. In this work, we have reported the synthesis of Vanadium Pentaoxide (V2O5) nanoparticles using hydrothermal method. Ammonium metavanadate (NH4VO3) was used as a source of Vanadium. These syntheses were carried out at four different concentrations of Vanadium source. The hydrothermal reaction was conducted at a temperature of 180°C for a duration of 24 hours, followed by an additional 24-hour period of natural cooling. Four samples were annealed in air using a muffle furnace at 500 °C for five hours. The X-ray diffraction (XRD) technique was used to study the structural aspects. A comparative analysis of the microstructure was conducted utilizing the Scherrer method, the Williamson-Hall method and its various models, Size-Strain analysis, and the Halder-Wagner method. The crystallite size and microstrain were determined using these distinct methods, revealing a systematic correlation between the crystallite size and microstrain obtained through the different techniques.&#xD.

Synthesis and characterizations of zinc oxide nanorods by cost effective aqueous hydrothermal technique for solid state lighting applications

Zinc oxide (ZnO) is recognized as the most promising and often utilized semiconducting material due to its exceptional physical, chemical, optical, and relatively low-cost production features, as well as its ecologically beneficial nature. ZnO is a prominent candidate owing to its wide band gap (3.37 eV at room temperature) as well as its high exciton binding energy (60 meV) for the next generation of ultraviolet and blue optoelectronic devices. This would be achieved through the development of hybrid heterostructured LED devices with low manufacturing costs by blending gallium nitride (GaN) with zinc oxide (ZnO), which serves as the most efficient opto-electronic device. Due to its high electron mobility, high transparency in the visible wavelength spectrum, and low work function, ZnO is also a highly investigated transparent conducting oxide thin film for several applications. Besides, their incredible optical capabilities, ZnO-based optical devices, such as light-emitting diodes (LEDs) and laser diodes (LDs), have drawn a great deal of interest. This reported research work demonstrates the growth of high-density, high-aspect-ratio ZnO nanorod (NR) arrays on p-type gallium nitride substrates employing low-cost facial aqueous hydrothermal syntheses with optimised growing conditions. Additionally, a top-down chemical etching technique is adapted for fabricating zinc oxide nanotubes. High-quality ZnO nanorods with high intensity that were a few microns long were found across the GaN substrate with FESEM analysis. The chemical composition of the grown nanorods is confirmed with EDAX analysis. The wurtzite crystalline structure and c-axis orientation of the grown ZnO NR-arrays were identified in X-ray diffraction studies. A Schimadzu UV–Vis–NIR spectrophotometer was used to record the optical curve, and the energy gap was determined to be 3.24 eV by plotting the Tauc curve. The good optical quality of the harvested nanorods is ensured by the narrow near-band-edge (NBE) emission at 384 nm and defect emission peaks detected through photoluminescence analyses. Grown specimens are also subjected to Raman spectrum analyses, and the obtained results are presented.

Synthesis, intercalation reactions, and electrochemical studies for VO2/PEO/Chitosan

VO2 obtained by hydrothermal synthesis from V2O5 was used as a matrix to obtain hybrid compounds containing different proportions of polyethylene oxide and chitosan. The XRD results demonstrate that monoclinic VO2 was obtained, and hybrid compounds showed variation in the displacement of the lamella peak, indicating an intercalation of polymers into the matrix. The stretching and vibration bands show a variation towards higher wavelength values of the hybrid compounds, which indicates that the intercalation of the polymers occurred into the matrix. The UV–Vis spectra show the absorptions that can be attributed to the transitions of each material. Absorption in the visible region decreases for hybrid compounds in relation to VO2. The hybrid compounds presented lower bandgap values compared to VO2. From cyclic voltammetry, it was possible to observe anodic and cathodic peaks linked to the redox process of the VIV/VIII pair for both VO2 and VO2/polymers, which is derived from the insertion/disinsertion process of lithium ions, where the hybrid compound presented a different voltammetric profile compared to VO2. The total charge curves as a function of the number of cycles demonstrate better cycling stability and a greater total charge of the hybrid compounds compared to VO2. These results demonstrate that hybrid compounds have potential as cathode materials for lithium-ion batteries.

Conventional Hydrothermal Synthesis of MFI Zeolite in Methanol Solution

Conventional Hydrothermal Synthesis of MFI Zeolite in Methanol Solution

Binary transition metal oxide: A novel and efficient catalyst for the synthesis of boron nitride nanotubes

AbstractA novel binary transition metal oxide (NiFe2O4) nanosphere catalyst with a diameter of 500 nm has been synthesized by the hydrothermal reaction, which can efficiently catalyze the formation of hexagonal boron nitride nanotubes (BNNTs) with high‐yield and large aspect ratio. Based on the temperature dependence of the product phase composition and microstructure, combined with results generated using single‐component catalysts, the BNNTs formation process can be summarized as follows: NiFe2O4 reacts with NH3 to generate Fe0.64Ni0.36, which dissolves to form a liquid‐phase Ni‐Fe alloy at high temperatures, where the B component in the precursor and the N atom formed by the decomposition of NH3 diffuse on the surface of the Ni‐Fe alloy; when the concentration of B and N exceed the saturation threshold, hollow BNNTs containing catalyst at the tips are precipitated. The formation process is dominated by a vapor‐liquid‐solid mechanism with tip‐growth mode, where the synergistic catalytic effect of the Ni‐Fe binary system promotes a high yield of large aspect ratio BNNTs.

Exploring Synthesis Strategies and Interactions between MOFs and Drugs for Controlled Drug Loading and Release, Characterizing Interactions Through Advanced Techniques.

This study explores various aspects of Metal-Organic Frameworks (MOFs), focusing on synthesis techniques to adjust pore size and key ligands and metals for crafting carrier MOFs. It investigates MOF-drug interactions, including hydrogen bonding, van der Waals, and electrostatic interactions, along with kinetic studies. The multifaceted applications of MOFs in drug delivery systems are elucidated. The morphology and structure of MOFs are intricately linked to synthesis methodology, impacting attributes like crystallinity, porosity, and surface area. Hydrothermal synthesis yields MOFs with high crystallinity, suitable for catalytic applications, while solvothermal synthesis generates MOFs with increased porosity, ideal for gas and liquid adsorption. Understanding MOF-drug interactions is crucial for optimizing drug delivery, affecting charge capacity, stability, and therapeutic efficacy. Kinetic studies determine drug release rates and uniformity, vital for controlled drug delivery. Overall, comprehending drug-MOF interactions and kinetics is essential for developing effective and controllable drug delivery systems.

Hydrothermal Synthesis of Fe-Doped Nickel Cobalt Phosphate Nanofibers for High-Stability Electrochemical Overall Water Splitting

Hydrothermal Synthesis of Fe-Doped Nickel Cobalt Phosphate Nanofibers for High-Stability Electrochemical Overall Water Splitting

Hydrothermally synthesized Ag2Te on metallic 2D templates

Silver telluride, Ag2Te, was synthesized on various 2D templates of carbon nanotubes (CNT) and transition-metal dichalcogenides (WTe2 and VTe2) via hydrothermal synthesis. X-ray diffraction (XRD) and Raman spectroscopy revealed that Ag2Te was synthesized on the 2D templates under optimal synthesis conditions. Differential scanning calorimetry (DSC) confirmed that the structural phase transition of Ag2Te underwent endothermic and exothermic reactions at approximately 410 and 425 K, respectively. Among various metallic templates, a large amount of Ag2Te has been synthesized on strongly acidic CNT. X-ray absorption near-edge structure (XANES) revealed that the chemical state of the metallic support influenced the electronic structure of the as-grown Ag2Te on the metallic supports. Our findings demonstrated that the hybrid 2D catalysts with an appropriate 2D metallic template can be a promising strategy for achieving efficient catalysis.

Comparative Study on the Proton Conduction Behaviors of Two Acidic Amphiphilic and Hydrophilic Coordination Compounds in Nafion Composite Membranes.

The acidic amphiphilic compound H[Co(H2L1)(HL1)(phen)]·3H2O (H4(Co-L1), H3L1 = 5-(3', 5'-dicarboxylphenyl)-pyridine-2-carboxylic, phen = phenanthroline) and the hydrophilic compound [Ni(HL2)(H2O)5]·H2O (H(Ni-L2), H3L2 = 5-(3',5'-dicarboxylphenyl)-pyridine-3-carboxylic) were synthesized via hydrothermal reactions at acidic conditions. The acidity of H4(Co-L1) is stronger than of H(Ni-L2); while the hydrogen bond continuity in H4(Co-L1) extended monodirectionally, which is smaller compared to the three-directional extension observed in H(Ni-L2). The proton conduction behaviors of these two compounds as fillers of Nafion composite membranes have been investigated. The results indicate that the optimal doping amounts of H4(Co-L1) and H(Ni-L2) are 2 and 1%, respectively; the proton conductivities of H4(Co-L1)/Nafion-2 and H(Ni-L2)/Nafion-1 composite membranes are 0.243 and 0.212 S·cm-1, respectively, which are approximately 50.2 and 30.6% higher than that of pure Nafion membrane, respectively. A higher doping amount of H4(Co-L1) can be attributed to its hydrophobic phen ligand, which promotes compatibility with Nafion membrane and reduces aggregation. Hydrogen bond continuity has a more significant effect on proton conductivity than acidity at relatively low doping amounts; conversely, this relationship reverses at relatively high doping amounts.

Optimization of cerium-based metal–organic framework synthesis for maximal sonophotocatalytic tetracycline degradation

Wastewater treatment is inevitably required to alleviate the pollution of water resources by various contaminants such as antibiotics. MOFs are novel materials with photocatalytic activities. In this study, sonophotocatalytic degradation of tetracycline (TC) by the Cerium-based MOF (Ce-MOF) is optimized by modification of its synthesis route. Ce-MOF synthesis by room temperature (RT), hydrothermal (HT), and sonochemical synthesis (SC) are studied. TC degradation experiments revealed the superiority of SC synthesis. The interplay of main synthesis parameters, namely, initial ligand concentration, ultrasound (US) power and time on sonophotocatalytic activity of Ce-MOF, were investigated by response surface methodology model (RSM) utilizing the central composite experimental design (CCD). The optimum SC synthesis conditions are an initial ligand concentration of 8.4 mmol/L, a sonication power of 50 amplitude, and a US time of 60 min. The optimally synthesized Ce-MOF was characterized by infrared spectroscopy, FTIR, XRD, FE-SEM, TEM, zeta potential analysis, diffuse reflectance spectroscopy, particle size analysis, Mott-Schottky analysis, photocurrent analysis, electrochemical impedance spectra, and photoluminescence spectroscopy. The findings indicate that the removal efficiency of TC can reach up to 81.75% within 120 min in an aqueous solution containing an initial TC concentration of 120 ppm and 1 g/L Ce-MOF at pH of 7. Mineralization efficiency of the process is 71% according to COD measurements. The Ce-MOF catalyst retained its chemical stability and remained active upon TC degradation which makes it a promising candidate for wastewater treatment.

Hydrothermal synthesis of pore-expanded hydroxyapatite for enhanced Cu2+ adsorption from aqueous solutions

This paper describes the hydrothermal synthesis of a pore-expanded hydroxyapatite (PE-HAp) from fine–grained calcareous sludge using a cetyltrimethylammonium bromide (CTAB) as a template and 1,3,5-trimethylbenzene (TMB) as a pore expander for the removal of Cu2+ ions from aqueous solutions. The PE-HAp was characterized using XRD, SEM, DTA/TGA and BET surface analysis. Adsorption behavior was assessed using Langmuir, Freundlich, Dubinin–Radushkevich, Temkin and Sips isotherms. In a solution with an initial Cu2+ concentration of 200 mg L-1 and a pH of 5.0, the highest Cu2+ removal efficiency was achieved using PE-HAp synthesized at a hydrothermal temperature of 180 °C at a concentration of 15 g/L over a period of 60 min. Using Langmuir isotherms, the highest single-layer adsorption capacity value was 9.90 mg g-1. Gibbs free energy (ΔG°), changes in enthalpy (ΔH°), and changes entropy change (ΔS°) revealed that the adsorption of Cu2+ on PE-HAp was spontaneous and exothermic. The PE-HAp synthesized in this study is a promising material for the removal of Cu2+ from aqueous solutions.