Comparative study of Co_(3)O_(4)-ZSM-5 catalysts synthesized by different hydrothermal methods for the catalytic oxidation of dichloromethane

In this work,various Co_(3)O_(4)-ZSM-5 catalysts were prepared by the microwave hydrothermal method(MH-Co_(3)O_(4)@ZSM-5),dynamic hydrothermal method(DH-Co_(3)O_(4)@ZSM-5),and conventio nal hydrothermal method(CH-Co_(3)O_(4)/ZSM-5).Their catalytic oxidation of dichloromethane(DCM)was analyzed.Detailed characterizations such as X-ray diffractometer(XRD),scanning microscopy(SEM),X-ray photoelectron spectroscopy(XPS),Brunauer-Emmett-Teller(BET),H2 temperature-programmed reduction(H2-TPR),temperature-programmed desorption of O_(2)(O_(2)-TPD),temperature-programmed desorption of NH_(3)(NH_(3)-TPD),diffuse reflectance infrared Fourier-transform spectra with NH_(3)molecules(NH_(3)-DRIFT),and temperature-programmed surface reaction(TPSR)were performed.Results showed that with the assistance of microwave,MH-Co_(3)O_(4)@ZSM-5 formed a uniform core-shell structure,while the other two samples did not.MH-Co_(3)O_(4)@ZSM-5 possessed rich surface adsorbed oxygen species,higher ratio of Co^(3+)/Co^(2+),strong acidity,high reducibility,and oxygen mobility among the three Co_(3)O_(4)-ZSM-5 catalysts,which was beneficial for the improvement of DCM oxidation.In the oxidation of dichloromethane,MH-Co_(3)O_(4)@ZSM-5 presented the best activity and mineralization,which was consistent with the characterizations results.Meanwhile,according to the TPSR test,HCl or Cl_(2)removal from the catalyst surface was also promoted in MH-Co_(3)O_(4)@ZSM-5 by their abundant Bronsted acid sites and the promotion of Deacon reaction by Co_(3)O_(4)or the synergistic effect of Co_(3)O_(4)and ZSM-5.According to the results of in situ DRIFT studies,a possible reaction pathway of DCM oxidation was proposed over the MH-Co_(3)O_(4)@ZSM-5 catalysts.

Facile preparation of hydrogenated graphene by hydrothermal methods and the investigation of its ferromagnetism

In this paper,a hydrothermal approach is utilized for the first time in integrating graphene oxide(GO),acetic acid(HAc)and nickel foam to prepare hydrogenated graphene(HG).There are two primary aims of this study:one is to ascertain the structure of the as-prepared HG,and the other one is to investigate the ferromagnetism of the HG.Under hydrothermal conditions,GO was reduced and hydrogenated by HAc,while the nickel foam served as a catalyst.This work provides a novel and facile route for the synthesis of hydrogenated graphene,which may lead to the application of hydrogenated graphene in spin electronic devices.

Preparation of Spherical Tungsten Particles Assisted by Hydrothermal Method

We presented a strategy to prepare spherical tungsten powder by the combination of hydrothermal method and H2reduction process.In hydrothermal process,the micelle of tetraethylammonium bromide(TEAB)act as spherical templates for the deposition of tungsten oxide,whereas the excessive TEAB inhibit the formation of spherical tungsten oxide due to the dense molecular layer of TEAB on the tungsten oxide particles.Citric acid(CA)can control the formation rate and structure of the tungsten oxide when its concentration is more than 0.2 mol/L,because of its ability to coordinate with tungsten atoms.The synergistic effect of TEAB and CA facilitates the formation of spherical tungsten oxide with nanorod crown.After being treated by H_(2)at 600 and 650℃,the tungsten oxide particles are reduced to tungsten particles,which maintain the spherical structure of tungsten oxide and have porous structure.

Structural, Optical and Photocatalytic Properties of Cu2+ Doped ZnO Nanorods with Using HMTA Solvent Prepared by Hydrothermal Method

In this experiment, Cu2+ doped ZnO (Cu-ZnO) nanorods materials have been fabricated by hydrothermal method. Cu2+ ions were doped into ZnO with ratios of 2, 5 and 7 mol.% (compared to the mole’s number of Zn2+). The hexamethylenetetramine (HMTA) solvent used for the fabrication of Cu-ZnO nanorods with the mole ratio of Zn2+:HMTA = 1:4. The characteristics of the materials were analyzed by techniques, such as XRD, Raman shift, SEM and UV-vis diffuse reflectance spectra (DRS). The photocatalytic properties of the materials were investigated by the decomposition of the methylene blue (MB) dye solution under ultraviolet light. The results show that the size of Cu-ZnO nanorods was reduced when the Cu2+ doping ratio increased from 2 mol.% to 7 mol.%. The decomposition efficiency of the MB dye solution reached 92% - 97%, corresponding to the Cu2+ doping ratio changed from 2 - 7 mol.% (after 40 minutes of ultraviolet irradiation). The highest efficiency for the decomposition of the MB solution was obtained at a Cu2+ doping ratio of 2 mol.%.

Characterization of ZnSe microspheres synthesized under different hydrothermal conditions

ZnSe microspheres were synthesized via a facile hydrothermal method under mild conditions using aqueous zinc nitrate and sodium selenite as raw materials. The effects of hydrothermal temperature, reaction time, concentration of NaOH and amount of hydrazine hydrate on the phase structure, morphology and size of final products were carefully investigated. The phase structures, morphologies and optical properties of the final products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy. ZnSe microspheres assembled by average size (about 20 nm) nanocrystals were prepared using 20 mL of 1 mol/L NaOH solution and 10 mL of hydrazine hydrate at 180 °C for 4 h. The results show that the products obtained at low hydrothermal temperature and short reaction time have poor crystallinity and contain impurity phases. The appropriate NaOH concentration and amount of hydrazine hydrate ensure to obtain pure ZnSe with spherical morphology and better luminescence property.

Hydrothermal synthesis of silver nanoparticles in Arabic gum aqueous solutions

Finely divided silver nanoparticles were synthesized via the hydrothermal method. Arabic gum （AG） was used as both the reductant and steric stabilizer without any other surfactant. By adjusting the reaction temperature, mass ratio of AG to AgNO3, and reaction time, silver nanoparticles with different morphological characteristics could be obtained. The products were characterized by UV-Vis, FTIR, TEM, SEM, and XRD measurements. It was found that temperature and AG played an important role in the synthesis of mono-disperse silver nanoparticles. Well dispersed and quasispherical silver nanoparticles were obtained under the optimal synthesis conditions of 10 mmol/L AgNO3, m（AG）/m（AgN03）= l：1, 160 ℃ and 3 h.

Integrated process of large-scale and size-controlled SnO_2 nanoparticles by hydrothermal method

SnO2 nanoparticles with the average particle size of 5-30 nm were synthesized using SnCl4·5H2O as the precursor and NH3·H2O as the mineralizing agent by hydrothermal method.In the case of 1 kg/batch production,the effects of synthesis conditions including solution concentration,reaction temperature,pressure,time and pH value on the grain size,particle morphology and crystal structure of SnO2 were systematically studied.The particles were characterized by X-ray diffraction（XRD） and transmission electron microscopy（TEM）.The results show that,the particle size can be well controlled in the range of 5-30 nm by adjusting the processing parameters such as reaction temperature and time when the crystal structure and particle morphology remain unchanged.The previous reports,the unusual dependences of the grain size of SnO2 on reaction temperature and time were found.The mechanism for such abnormal grain growth behavior was tentatively elucidated.

Facile H2O2 Hydrothermal Synthesis of Bimodal Mesoporous Silica MCM-48 Spheres

The ordered bimodal mesoporous silica MCM-48 spheres were facile synthesized by mild- temperature post-synthesis H2O2 hydrothermal treatment of as-synthesized MCM-48. The results showed that H2O2 is indispensable for simultaneously removing organic templates and forming ordered bimodal mesoporous silica MCM-48 spheres. The bimodal mesoporous MCM-48 was characterized by X-ray diffraction, transmission electron micrographs, FT-IR, and N2 adsorption-desorption, and a possible mechanism was proposed for the formation of bimodal mesoporous MCM-48.

Recent advances in hydrothermal modification of calcium phosphorus coating on magnesium alloy

Magnesium(Mg) and its alloys have emerged as a favored candidate for bio-regenerative medical implants due to their superior biocompatibility, biodegradability and the elastic modulus close to that of human bone. Unfortunately, the rapid and uncontrollable degradation rate of Mg alloys in chloride-rich body microenvironments limits their clinical orthopedic applications. Recently, Calcium Phosphate(Ca-P)biomaterials, especially Hydroxyapatite(HA), have been broadly applied in the surface functional modification of metal-based biomaterials attributed to their excellent bioactivity and biocompatibility. Hydrothermal modification of Ca-P coatings on Mg alloys has been extensively exploited by researchers for its significant superiorities in controlling coating structure and improving interfacial bonding strength for better osseointegration and corrosion resistance. This work focuses on the up-to-the-minute advances in Ca-P coatings on the surface of Mg and its alloys via hydrothermal methods, including the strategies and mechanisms of hydrothermal modification. Herein, we are inclined to share some feasible and attractive hydrothermal surface modification strategies. From the perspectives of hydrothermal manufacturing technique innovation and coating structure optimization, we evaluate how to foster the corrosion resistance, coating bonding strength, osseointegration and antibacterial properties of Mg alloys with Ca-P coatings synthesized by hydrothermal method. The challenges and future perspectives on the follow-up exploration of Mg alloys for orthopedic applications are also elaborately proposed.

Phase composition,conductivity,and sensor properties of cerium-doped indium oxide

The hydrothermal synthesis of In_(2)O_(3)and CeO_(2)–In_(2)O_(3)is investigated as well as the properties of sensor layers based on these compounds.During the synthesis of In_(2)O_(3),intermediate products In(OH)_(3)and InOOH are formed,which are the precursors of stable cubic(c-In_(2)O_(3))and metastable rhombohedral(rh-In_(2)O_(3))phases,respectively.A transition from c-In_(2)O_(3)to rh-In_(2)O_(3)is observed with the addition of CeO_(2).The introduction of cerium into rh-In_(2)O_(3)results in a decrease in the sensor response to hydrogen,while it increases in composites based on c-In_(2)O_(3).The data on the sensor activity of the composites correlate with XPS results in which CeO_(2)causes a decrease in the concentrations of chemisorbed oxygen and oxygen vacancies in rh-In_(2)O_(3).The reverse situation is observed in composites based on c-In_(2)O_(3).Compared to In_(2)O_(3)and CeO_(2)–In_(2)O_(3)obtained by other methods,the synthesized composites demonstrate maximum response to H_(2)at low temperatures by 70–100℃,and have short response time(0.2–0.5 s),short recovery time(6–7 s),and long-term stability.A model is proposed for the dependence of sensitivity on the direction of electron transfer between In_(2)O_(3)and CeO_(2).

Engineering of Self-Supported Electrocatalysts on a Three-Dimensional Nickel Foam Platform for Efficient Water Electrolysis

Economical water electrolysis requires highly active non-noble electrocatalysts to overcome the sluggish kinetics of the two half-cell reactions,oxygen evolution reaction,and hydrogen evolution reaction.Although intensive efforts have been committed to achieve a hydrogen economy,the expensive noble metal-based catalysts remain under consideration.Therefore,the engineering of self-supported electrocatalysts prepared using a direct growth strategy on three-dimensional(3D)nickel foam(NF)as a conductive substrate has garnered significant interest.This is due to the large active surface area and 3D porous network offered by these electrocatalysts,which can enhance the synergistic eff ect between the catalyst and the substrate,as well as improve electrocatalytic performance.Hydrothermal-assisted growth,microwave heating,electrodeposition,and other physical methods(i.e.,chemical vapor deposition and plasma treatment)have been applied to NF to fabricate competitive electrocatalysts with low overpotential and high stability.In this review,recent advancements in the development of self-supported electrocatalysts on 3D NF are described.Finally,we provide future perspectives of self-supported electrode platforms in electrochemical water splitting.

High-stable and High-capacity Sn/SnO_(2)@C as Anode of Lithium-ion Batteries

We synthesized size-controllable nanoparticles with homogeneous distribution of carbon and Sn/SnO_(2)by a solvothermal method.The effects of different carbon content and hydrothermal time on the composition,morphology and electrochemical properties of the materials were investigated.Compared with bulk materials,nanoparticles materials not only have high specific surface area,but also can provide abundant reaction sites,thus enhancing the electrochemical activity of electrode materials.More importantly,the optimized microspheres Sn/8C-24 delivers a superior electrochemical performance,achieving a specific discharge capacity of 700.4 mAh·g^(-1)after 150 cycles at 0.5 A·g^(-1),and the Coulomb efficiency reaches 98.65%,which is promising for anode of LIBs.

Hydrothermal Synthesis of Rhombus-like SmCO3OH Microplates and Its Photoluminescence Property Doped with Eu^3＋

Rhombus-like SmCO3OH microplates with the edge lengths ranging from 5 μm to 10 μm and the thickness about 1.5 μm were synthesized through a simple hydrothermal method using urea as the precipitance. The structure and properties of the rhombus-like SmCO3OH microplates were characterized by X-ray diffraction, field-emission scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The optical property of the rhombus-like SmCO3OH microplates doped with Eu^3＋ was investigated by photoluminescence. A broad and strong emission band at 677 nm was obtained, which can be contributed to producing light conversion film.

Upconversion Luminescence Properties of Ho^(3+),Tm^(3+),Yb^(3+) Co-Doped Nanocrystal NaYF_4 Synthesized by Hydrothermal Method

Nanocrystal of upconversion （UC） phosphor Ho^3＋, Tm^3＋ , and Yb^3＋ co-doped NaYF4 was prepared by the hydrothermal method in the presence of the complexing agent EDTA. Under 980 nm diode laser excitation, the impact of different concentrations of Ho^3＋ ion on the UC luminescence intensity was discussed. The law of luminescence intensity versus pump power shows that the 474 nm blue emission, 538 nm green emission, and 642 nm red emission are all due to the two-photon process, while the 450 nm blue emission is a three-photon process. The UC mechanism and processes were also analyzed. The sample was characterized by transmission electron microscopy （TEM） and X-ray diffraction （XRD）. The result shows that Ho^3＋ ,Tm^3＋ , and Yb^3＋ co-doped NaYF4 prepared by the hydrothermal method exhibits a hexagonal nanocrystal.

Synthesis and electrochemical performance of LiCoPO_4 micron-rods by dispersant-aided hydrothermal method for lithium ion batteries

LiCoPO4 micron-rods with an average diameter of about 500 nm and length of about 5 μm were synthesized by dispersant-aided hydrothermal method. Poly(n-vinylpyrrolidone) (PVP) was used as dispersant in the hydrothermal method. The starting solution and the concentration of dispersant have significant influences on the morphology of LiCoPO4,and the electrochemical performance is improved via controlling the particle size and morphology by the hydrothermal method. The cell using smaller particle LiCoPO4 as cat...

Graphene oxide assisted facile hydrothermal synthesis of LiMn_(0.6)Fe_(0.4)PO_4 nanoparticles as cathode material for lithium ion battery

Assisted by graphene oxide（GO）,nano-sized LiMn0.6Fe0.4PO4 with excellent electrochemical performance was prepared by a facile hydrothermal method as cathode material for lithium ion battery.SEM and TEM images indicate that the particle size of LiMn0.6Fe0.4PO4（S2）was about 80 nm in diameter.The discharge capacity of LiMn0.6Fe0.4PO4 nanoparticles was 140.3 mAh-g^1 in the first cycle.It showed that graphene oxide was able to restrict the growth of LiMn0.6Fe0.4PO4 and it in situ reduction of GO could improve the electrical conductivity of LiMn0.6Fe0.4PO4 material.

Hydrothermal Synthesis and Crystal Structure of a Square Grid Coordination Copper(II) Polymer from 1,4-Bis(imidazole-1-ylmethyl)benzene

The title compound [Cu（bix）2（NO3）z·H2P]n 1 （bix = 1,4-bis（imidazole-1-ylme-thyl） benzene） has been synthesized by hydrothermal method. Its crystal structure is of monoclinic, space group P1^- with a = 8.3075（13）, b = 9.4725（13）, c = 10.0192（13） A, α = 91.088（4）, β = 104.063（6）, γ = 101.88（1）, V = 746.5（3） A^3, Z = 1, C28H30N10O7Cu1, Mr = 682.16, Dc = 1.518 g/cm^3, μ = 0.796 mm^-1, F（000） = 353, the final R = 0.0535 and wR = 0.0996 for 2921 observed reflections with I 〉 2σ（I）. Each bix ligand binds two Cu（Ⅱ） ions to form a 2-D（4,4） square grid layer, which is connected by hydrogen bonds showing large channels occupied by solvated water molecules and nitrate anions.

N-doped NaTaO3 synthesized from a hydrothermal method for photocatalytic water splitting under visible light irradiation

NaTaONcatalysts were synthesized by a hydrothermal（H） and a solid-state（S） methods in this study.The H-and S-NaTaONsamples were characterized by X-ray diffraction（XRD）, scanning electron microscopy（SEM）, transmission electron microscopy（TEM）, UV–visible（UV–vis） diffuse reflectance spectroscopy, and photoluminescence（PL） spectroscopy. The XRD patterns of the H-and S-samples showed peaks indexed to the pure phase of perovskite NaTaOand minor peaks assignable to TaNat various synthesis temperatures. Substitution of oxygen by nitrogen ions causes the light absorption of the H-and S-NaTaONsamples to be extended to the 600–650 nm region, thus making the samples visible-light active. The NaTaONsamples exhibited photocatalytic activity for Hand Oevolution from aqueous methanol and silver nitrate solutions under visible-light irradiation. The UV–vis and PL spectra of the Hand S-catalysts revealed the presence of cationic vacancies and reduced metallic species, which acted as recombination centers. These results demonstrated that the preparation method plays a critical role in the formation of defect states, thereby governing the photocatalytic activity of the NaTaONcatalysts.

Hydrothermal synthesis and enhanced photocatalytic activity of hierarchical flower-like Fe-doped BiVO_4

Fe-doped BiVO4with hierarchical flower-like structure was prepared via a hydrothermal method using sodium dodecylbenzene sulfonate(SDBS)as structure directing agent.X-ray diffraction(XRD),scanning electron microscope(SEM),transmissionelectron microscope(TEM),high resolution transmission electron microscope(HRTEM),X-ray photoelectron spectroscopy(XPS)and UV-Vis were applied for characterization of the as-prepared samples.The formation mechanism of flower-like structure wasproposed based on the evolution of morphology as a function of hydrothermal time.Fe-doped into substitutional sites of BiVO4effectively improved the migration and separation of photogenerated carrier and enhanced the utilization of visible light.Flower-likeFe-doped BiVO4showed much higher visible-light-driven photocatalytic efficiency for degradation of methyl blue compared withthe pristine BiVO4.And the sample with a Fe/Bi mole ratio of2.5%showed the highest photocatalytic efficiency.

Microstructure and photocatalytic activity of Ni-doped ZnS nanorods prepared by hydrothermal method

Pure ZnS and Ni^2+-doped ZnS nanorods (Zn1-xNixS, x=0, 0.01, 0.03, 0.05 and 0.07, mole fraction,%) were synthesized by hydrothermal method. The effects of Ni2+ doping on the phase-structure, morphology, elemental composition and optical properties of the samples were investigated by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), X-ray energy dispersive spectrometry (EDS) and ultraviolet–visible spectroscopy (UV-Vis), respectively. The photocatalytic activity of Zn1-xNixS nanorods was evaluated by the photodegradation of organic dyes Rhodamine B (RhB) in aqueous solution under UV light irradiation. The results show that all samples exhibit wurtzite structure with good crystallization. The morphologies are one-dimensional nanorods with good dispersion, and the distortion of the lattice constant occurs. The band gap of Zn1-xNixS samples is smaller than that of pure ZnS, thus red shift occurs. Ni^2+-doped ZnS nanocrystals can enhance photocatalytic activities for the photodegradation of RhB. Especially, Zn0.97Ni0.03S sample exhibits better photocatalytic performance and photocatalytic stability for the decomposition of RhB.