Efficient Preparation and Electrochemical Properties of BiOCl/Graphite by One-step Solvothermal Method

We used the surface-pretreated graphite paper(Gp)as a carrier and loaded BiOCl with high selectivity to Cl^(-)on its surface by solvothermal method to form BiOCl@Gp electrode.The morphology,structure,and composition of the materials were characterized by scanning electron microscopy and nitrogen adsorption/desorption,and the results showed that the spherical BiOCl particles were uniformly dispersed on the surface of the Gp,forming a mesoporous BiOCl@Gp composite with a specific surface area of 22.82 m^(2)/g and a pore volume of 0.043 cm3/g.Furthermore,cyclic voltammetry and electrochemical impedance spectroscopy were used to test the electrochemical properties of the composites,and the stability of BiOCl and the high conductivity of Gp were synergistic,the BiOCl@Gp exhibited a specific capacitance of 30.2 F·g^(-1) at a current density of 0.5 A·g^(-1),and the selectivity of the BiOCl@Gp materials for Cl^(-)was significantly higher than that of SO_(4)^(2-),NO_(2)^(-),and HCO_(3)^(-).Therefore,BiOCl@Gp composite electrode materials can be used for the selective adsorption of Cl^(-)in wastewater,in order to achieve efficient wastewater recycling.

Synthesis of Yttrium Oxide Nanocrystal via Solvothermal Process

Y2O3 nanomaterials have been widely used in transparent ceramics and luminescent devices. Recently there are many studies focusing on controlling the size and morphology of Y2O3 in order to obtain better materials performance. In present study, yttrium oxyhydroxide precursor was synthesized via a facile solvothermal process through the dissolution-recrystallization mechanism of Y2O3 raw powders in the ethylenediamine solvent, then nanosized yttrium oxide crystal was prepared from the precursor through post heat treatment process. The effects of solvothermal treatment temperature, holding time, solvent kinds and post heat treatment parameters on crystalline structure, grain shape and size of nanocrystal were investigated by XRD, TEM and TGA-DTA measurements. TEM images reveal that the morphology of product after post heat treatment at 460 ℃ for 12 h is rice-like nanocrystal. XRD shows that this product is pure cubic Y2O3 cphase. Present study reveals that high purity Y2O3 with rice-like morphology can be easily prepared with average size around 30 nm under suitable post heat treatment parameters. In addition, the effects of solvents such as water and ethanol etc. on the crystal structure and morphology were also investigated. It is suggested that dissolution-recrystallization process may be the main mechanism for the formation of nano-sized YOOH precursors under solvothermal reaction condition, and the ethylenediamine solvent is likely to play an important role in controlling the transformation process of yttria precursors to theY2O3 nanocrystal.

Solvothermal Synthesis and Characterization of HgTe Nanoplatelets Using Mercury(I) Source

Mercury telluride （HgTe） nanoplatelets were obtained via a facile solvothermal reaction of mercury（I） chloride and tellurium powder in ethylenediamine （en）. Mercury（I） was first applied as the mercury sources to prepare nanocrystal HgTe; moreover, the proposed mechanism for the fabrication of the sample was discussed in detail. The HgTe nanoplatelets were characterized by powder X-ray diffraction （PXRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, high-resolution transmission electron microscopy （HRTEM） and Fourier transform infrared spectroscopy （FT-IR）. The absence of IR absorption may render the title nanocrystal useful as an IR transparent material in the region.

Layered double hydroxide nanosheets via solvothermal delamination

A new solvothermal post-synthesis treatment for preparing high aspect ratio magnesium aluminium layered double hydroxides(Mg Al–LDHs) has been developed. Treating laurate-intercalated Mg Al–LDHs in pure ethanol in an autoclave for 48 h at 150 °C was found to produce delaminated MgA l–LDH nanosheets with a thickness of ~2.6 nm and an aspect ratio of ~105. It is proposed that the high pressure solvothermal process promotes the insertion of ethanol molecules into the LDH interlayer space, thereby facilitating delamination. This new post-synthesis treatment provides the opportunity for a facile, large scale route to highly delaminated high aspect ratio LDHs, which might be of interest towards novel nanomaterials for energy conversion and storage.

Preparation of Copper Phthalocyanine Crystals Using Solvothermal Synthesis

A novel solvothermal synthesis method for the direct growth of B-form crystals of copper phthalocyanine（CuPc） is presented in this article. With quinoline as solvent, crystals were grown after cooling the reaction mixture of 1,3-diiminoisoindoline and copper oxide, heated for 9 h at 270 ℃, to room temperature in an autoclave. These high quality crystals were suitable for characterization measurements. The single-crystal diffraction data show a monoclinic system unit cell： a=1.4668（3） nm, b=0.48109（10） nm, c=1.9515（7） nm, a=90°, B=121.04（2）°, r=90°, where the corresponding cell volume is 1.17991 nm^3. Needle-like single crystals of CuPc up to 10.5 mm in length were obtained. The influences of different temperatures, reaction time and solvent volume on the crystal yields were also discussed. Optimum reaction conditions were 10 mL of quinoline, at 270 ℃ for 8 h.

Solvothermal Synthesis, Structure and the Secondorder NLO Properties of a Novel Non-metal 3-D Borophosphate:（NH4）2[B2P2O8（OH）2]

A new non-metal 3-D borophosphate compound formulated as(NH4)2[B2P2O8(OH)2](1)has been synthesized by a solvothermal method and characterized by elemental analysis,energy-dispersive X-ray spectroscopy(EDS),IR spectrum and single-crystal X-ray diffraction.The borophosphate(NH4)2[B2P2O8(OH)2]crystallizes in the cubic system,space group P213 with Z=2,a=b=c=7.586(4)?,V=436.6(4)?3,Mr=281.64,Dc=2.127 g/cm^3,λ=0.71073?,μ=0.551 mm^-1,F(000)=284,R=0.0277 and wR=0.0758 for 262 observed reflections with I>2σ(I)and S=1.082.Its structure is constructed by the connection of PO4 and BO3(OH)tetrahedra to form a 3-D anionic framework containing 4-and 8-membered rings(MRs),with two NH4+cations located in the channels of the 8-membered rings.The N–H…O hydrogen bonds are observed in its packing structure and enhanced the stability of crystal structure.In addition,its thermal stability,UV spectrum and second-order NLO properties have been also investigated.

Solvothermal Synthesis and Characterization of (NH_3CH_2CH_2NH_3)HgSnS_4 with a Column Structure

A compound （NH3 CH2 CH2 NH3 ）HgSnS4 with a column structure was synthesized solvothermally and characterized by X-ray single-crystal diffraction. This compound crystallizes in the monoclinic space group C2/c with a = 1. 3863 （6） nm, b = 0. 6640 （ 3 ） nm, c = 2. 3198 （10） nm, β = 106. 168 （ 7 ）° and Z = 8. It consists of anionic columns of [ HgSnS4 ]^2- that are interrupted by cationic columns of [ EnH2 ]^2＋ . Its thermal and optical properties were studied.

Synthesis of Nickel Sulfide Particles by Solvothermal Process

Pyrite nickel disulfide and millerite nickel monosulfide have been successfully prepared by solvothermal method based on the reaction of Ni(NO3)2.6H2O and H2NC(S)NH2 in benzene and ethylenediamine (EDA). The final products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM). The effects of the solvent, reaction temperature and time on the morphology and phase of the products have been discussed.

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b = 11.919（2）, c =14.879（3）A, α = 108.791（3）, β= 102.441（3）, γ = 92.846（2）°, V= 1140.1（3）A3, Mr = 859.71, Z= 2, Do = 2.504 g/cm^3 ,μ = 5.324 mm^-1, F（000） = 804, S = 1.013, the Final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with Ⅰ 〉 2 σ（Ⅰ）. 1 consists of [C4HgNH3]＋ cations and two-dimensional [Sb4ST]n^2n- anion which is composed of three SbS3 trigonal pyranaids and one SbS4 unit joined by sharing common comers. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]^＋ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.

Solvothermal Synthesis of ZnIn2S4 by Alcohol Solvents and Visible Light Photocatalytic Activity on Selective Oxidation and Dye Degradation

A series of hexagonal ZnIn2S4 samples with different morphologies have been successfully prepared via a facile solvothermal approach using different alcohol solvents with the optimum synthesis time and temperature. X-ray diffraction, field emission scanning electron microscopy, UV-vis diffuse reflection spectroscopy and photoelectrochemical measurements are employed to determine the properties of the samples. It is found that the solvent has a significant influence on the morphology, optical properties and electronic nature of the samples. The photocatalytic activities of the samples have been evaluated by selective oxidation of benzyl alcohol to benzaldehyde to benzaldehyde and the degradation of methyl orange（MO） under visible light irradiation. The results reveal that the photocatalytic activities of ZnIn2S4 are closely related to the reaction solvent. The ethanol-mediated ZnIn2S4 exhibits the best photocatalytic performance toward selective oxidation of benzyl alcohol to benzaldehyde and the degradation of dye MO compared to the samples prepared in other solvents, which can be attributed to the integrative effect of the enhanced light absorption intensity and the prolonged lifetime of photogenerated carriers. In addition, a possible mechanism is proposed and discussed. It is expected that our current research could promote further interest on the synthesizing efficient ternary chalcogenides semiconducting materials for environment remediation and organic transformation.

Synthesis of the Complex Fluoride LiBaF_(3) through a Solvothermal Process

The complex fluoride LiBaF3 is solvothermally synthesized at 180℃ and characterized by means of X-ray powder diffraction, scanning electron microscopy, thermogravimetric analysis and infrared spectroscopy. In the solvothermal process, the solvents, mole ratios of initial mixtures and reaction temperature play important roles in the growth of the single crystal.

Surfactant assisted solvothermal synthesis of LiFePO4 nanorods for lithium-ion batteries

Well-shaped and uniformly dispersed LiFePOnanorods with a length of 400–500 nm and a diameter of about 100 nm, are obtained with participation of a proper amount of anion surfactant sodium dodecyl sulfonate（SDS） without any further heating as a post-treatment. The surfactant acts as a self-assembling supermolecular template, which stimulated the crystallization of LiFePOand directed the nanoparticles growing into nanorods between bilayers of surfactant（BOS）. LiFePOnanorods with the reducing crystal size along the b axis shorten the diffusion distance of Liextraction/insertion, and thus improve the electrochemical properties of LiFePOnanorods. Such prepared LiFePOnanorods exhibited excellent specific capacity and high rate capability with discharge capacity of 151 mAh/g, 122 mAh/g and 95 mAh/g at 0.1C, 1 C and 5 C, respectively. Such excellent performance of LiFePOnanorods is supposed to be ascribed to the fast Lidiffusion velocity from reduced crystal size along the b axis and the well electrochemical conductivity. The structure, morphology and electrochemical performance of the samples were characterized by XRD, FE-SEM, HRTEM, charge/discharge tests, and EIS（electrochemical impedance spectra）.

Synthesis and characterization of BaCeO_3 nanocrystals via solvothermal-based method

A facile approach to preparing well-dispersed nanocrystals of BaCeO3 was developed by a combination of solvothermal and annealing processes. The precursor consisted of amorphous BaCO3 and CeO2, and the conversion of the precursor to crystalline BafeO3 nanocrystals occurred upon heat treatment at a relatively low temperature. The as-processed BaCeO3 had an orthorhombic structure and the average size of such crystals was approximately 80 nm. The obtained products were characterized by Fourier Transform Infrared （FT-IR）, X-Ray Diffraction （XRD）, Laser Raman Spectroscopy （LRS）, Scanning Electron Microscopy （SEM）, Energy Dispersive X-Ray Spectrometry （EDS）, and Transmission Electron Microscopy （TEM）. This preparation process could also be used to synthesize doped barium cerate complex oxides Bafe0.95M0.05O3-δ （M=Y, Nd, Gd, and Sm）.

Preparation of Sn-doped In_2O_3 nanopowders by a solvothermal process

Sn-doped In2O3（ITO） nanopowders in square shape were prepared in ethylene solvent by a solvothermal process,using In（4N） and SnCl4·5H2O as starting materials.The effects of solvothermal temperature and coprecipitation pH on the products were investigated using XRD,XPS,and TEM.Mixtures of InOOH crystals and In4Sn3O12 crystals were prepared at 210°C or 230°C and ITO nanopowders with cubic structure were obtained at 250°C or above 250°C.When the coprecipitation pH was 6,the product was ITO with impurity Sn3O4.When the pH was 9,the product was single phase ITO.

Synthesis and fluorescence properties of cerium-KMgF_3 through a solvothermal process

Phosphor of KMgF3：Ce^3＋ is synthesized through solvothermal method at 180 ℃ and characterized by means of X-ray powder diffraction （XRD） and environment scanning electron microscopy （ESEM）. X-ray photoelectron spectroscopy （XPS） is applied to the study of the energy band structure of KMgF3：Ce^3＋ and confirms the oxygen content of the product is very low. The fluorescence spectra of the rare-earth ion-doped KMgF3 is investigated by the fluorescence spectrophotometer. In the emission spectra, there is a broadband emission with a maximum center located at 306 nm arising from d-f transition of Ce^3＋ in the host. This will be useful for ultraviolet tunable lasers.

Solvothermal Syntheses of (H_2en)_2Sn_2S_6·en and[(H_2hmda)_3(Hhmda)_2](Sn_2S_6)_2Using SnCl_4 and S_8 as Starting Materials

Three thiostannates （H2en）2Sn2S6· en 1, （Hen）4Sn2S6 2 （en = ethylenediamine, a known compound）and [（H2hmda）3（Hhmda）2]（Sn2S6）2 3 （hmda = hexamethylenediamine） were prepared using SnCl4.5H2O and S8 as starting materials in alkylenediamine solutions under mild solvothermal conditions. Compound 1 crystallizes in the triclinic system, space group P1^- with a = 8.7491（17）, b = 10.704（2）, c = 12.2031（19） A, a = 74.888（13）, β= 72.998（12）, γ= 89.032（15）°, V = 1052.9（3） A^3, Mr = 614.08, Z= 2, De = 1.937 g/cm^3, p = 2.966 mm^-1, F（000） = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 observed reβections with I 〉 2σ（I）; while 3 crystallizes in the triclinic system, space group P1^- with a = 9.8075（13）, b = 10.8266（16）, c = 14.303（2） A, a = 88.611 （10）, β = 81.030（9）, γ = 74.609（9）°, V = 1446.1 （4） A^3, Mr = 1448.78, Z = 1, Dc = 1.664 g/cm^3, μ = 2.173 mm^-1, F（000） = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 observed reβections with I 〉 2σ（I）. The compounds are composed of dimeric [Sn2S6]^4- anions and protohated alkylenediamine cations.

Alcohol Solvent Effect on Fluorescence Properties in the Solvothermal Synthesis of Carbon Quantum Dots

Highly monodisperse carbon quantum dots(CQDs)were synthesized by a solvothermal method using L-ascorbic acid as carbon source and different simple alcohols(methanol,ethanol,ethylene glycol,and isopropanol)as reaction solvents at 180℃for 4 hours.The performance of CQDs was characterized by transmission electron microscope(TEM),Fourier infrared spectrometer(FTIR),UV-visible spectrophotometer,and fluorescence spectrophotometer.The results show that the prepared CQDs are wavelength-dependent,and have good hydrophilicity and similar surface compositions.However,there are more carbon and oxygen-containing functional groups on the surface of CQDs prepared with ethanol(CQDs-ET),and the type and number of functional groups will directly affect the fluorescence emission of CQDs.Also,it is found that the luminescence mechanisms of CQDs prepared by this solvothermal method are mainly based on the defect state of the oxygen group surface.And alcohol solvents do not directly participate in the formation of carbon nuclei during the reaction process,but it will affect the number and type of surface groups.Therefore,the influence of surface groups on the CQDs performance is greater than that of carbon nuclei in this experiment.

Solvothermal Synthesis and Structure Characterization of a 3D Hydrogen-bonded Copper Compound [Cu(H_2dhpmc)_2]·2H_2O

The solvothermal reaction of H3dhpmc (H3dhpmc = 2, 4-dihydroxypyrimidine- 5-carboxylic acid), CuCl2稨2O and NaVO3 results in the formation of a discrete mononuclear Cu(Ⅱ) complex [Cu(H2dhpmc)2]?H2O. It crystallizes in monoclinic system, space group P21/c with a = 5.0497(9), b = 10.0196(6), c = 13.715(2) ? b = 96.237(1)? V = 689.8(2) 3, Z = 2, Dc = 1.973 g/cm3, ?= 1.654 mm-1, F(000) = 414, R = 0.0736 and wR = 0.1351. Each Cu(Ⅱ) is coordinated to four oxygen atoms of two 2, 4-dihydroxypyrimidine-5-carboxylic acid ligands in the equatorial position and two oxygen atoms of two water molecules in the axial position to form an axially elongated octahedral geometry. The title complex is further linked into a three-dimensional structure through the weak interactions of hydrogen bonds between the oxygen atoms and the nitrogen atoms.