One-step hydrothermal synthesis of 2,5-PDCA-containing MgAl-LDHs three-layer composite coating with high corrosion resistance on AZ31

The addition of 2,5-pyridinedicarboxylic acid(2,5-PDCA)to the Mg-Al LDH coating,which was prepared by one-step hydrothermal synthesis,had extremely enhanced the corrosion protection of AZ31 Mg alloy,although the 2,5-PDCA could not be intercalated into the interlayer spacing.The corrosion current density of 0.05 mol L^(−1)2,5-PDCA LDH containing LDH coating is 3.18 nA cm^(−2),reduced by two orders of magnitude compared to the LDH coating without inhibitor,and the corrosion inhibition efficiency of the coating is 98.05%.The coating formed on the surface of AZ31 was peeled off from the substrate by using a mechanical method and SEM observation of the cross-section showed that the coating consisted of three different layers.The innermost layer is a thick layer that consists of Mg(OH)_(2)and the intermediate layer is LDH,which is vertical to the substrate and the outmost layer is a thin but very dense deposit layer of LDH agglomerates with complexes of 2,5-PDCA and Mg.This kind of sediment/LDH/Mg(OH)_(2)three-layer composite structure was accountable for the increase in the corrosion resistance of AZ31 Mg alloy.

Hydrothermal Synthesis and Characterization of a Novel Supramolecular Network Compound [Co(IN)_2(H_2O)_4](IN=Isonicotinate)

A novel supramolecular compound, [Co(IN)2(H2O)4](1), was synthesized by means of the hydrothermal method and its structure was characterized with elemental analysis, FT-IR spectrum, TGA and X-ray diffraction. Though the unit cell structure of the title compound is only monomeric, all these units as building blocks are assembled into a novel three-dimensional supramolecular network via the widely hydrogen-bonding and π-π stacking interactions.

Hydrothermal synthesis and fluorescence of YF_(3):Eu^(3+)

Europium(Ⅲ)-doped YF_(3) is prepared by a hydrothermal process at 200℃.X-ray diffraction(XRD) pattern identifies the formation of YF_(3) phase without detectable impurity.Environment scanning electron microscopy(ESEM) image shows the even size distribution of the samples with cubic morphology.The excitation and emission spectra of the rare earth ions doped YF_(3) are investigated by fluorescence spectrophotometer.The excitation spectrum for 591 nm emission has several excitation bands at 320, 365,386,397 and 467 nm,and the main peak value was 397 nm.Typical Eu^(3+) emission peaks at 591 nm (^(5)D_(0)→^(7)F_(1)) and 612 nm (^(5)D_(0)→^(7)F_(2)) are observed when excited by 397 nm,and the strongest emission is 591 nm,demonstrating that the rare earth ions occupy the centrosymmetrical sites in YF_(3).

Hydrothermal Synthesis,Crystal Structure and Spectral Characterization of a New Copper Isopolytungstate: [Cu(phen)_3][W_6O_(19)]

An unusual inorganic-organic hybrid hexatungstate complex [Cu(phen)3][W6O19] 1 (C36H24 CuN6O19W6, Mr = 2011.20) was hydrothermally synthesized and characterized by single- crystal X-ray diffraction, IR spectrum, UV-VIS spectrum and elemental analyses. This compound crystallizes in the monoclinic system, space group C2/c with a = 19.1005(11), b = 11.2585(11), c = 20.2867(15) , β = 102.177(2)o, V = 4264.4 3, μ(MoKa) = 16.691 mm–1, Dc = 3.133 g/cm3, Z = 4, F(000) = 3628, the final R = 0.0338 and wR = 0.0798 for 4090 observed reflections with I > 2σ(I). The result of structure determination shows that the crystal structure is constructed from [W6O19]2– cluster anions and [Cu(phen)3]2+ complex fragments, which are held together into a three-dimen- sional network through hydrogen-bonding interactions.

Hydrothermal Synthesis and Structure of [CH3NH3]2[(VⅣO)2(VⅤO4)2]:A New Layered Mixed-valence Vanadium Oxide Incorporated with Organic Cations

A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. It crystallizes in a triclinic system with space group P 1, a =0 625 59(8) nm, b =0 639 84(9) nm, c =0 747 19(10) nm, α =78 718(2)°, β =80 099(2)°, γ =77 100(2). The compound contains mixed valence V 4+ /V 5+ vanadium oxide layers constructed from VO 4 tetrahedra, pairs of edge sharing VO 5 square pyramid and methylamine with protonated organic amines occupying the interlayer space.

Influence of the fly ash fraction after grinding process on the hydrothermal synthesis efficiency of Na-A,Na-P1,Na-X and sodalite zeolite types

The fly ashes(Class F and C)have been successfully used as the main substrates in the hydrothermal syntheses of Na-A,Na-P1,Na-X and sodalite zeolites.Both ashes and their derivatives after milling with magnetic field grinder were used.The paper investigates the effect of fly ash fraction size on the syntheses efficiency and physicochemical properties of the obtained zeolites.The starting material and obtained zeolites were subjected to physicochemical characteristics using X-ray diffraction,X-ray fluorescence,particle size analysis,and scanning electron microscopy methods.The paper showed a significant effect of the used fly ash fractions on the quantity,purity,quality and level of crystallinity of the zeolites phase obtained.The application of the grinding process prior to the syntheses of zeolites,with a relatively small financial outlay,significantly increases their application potential.Obtained zeolites are a promising material in the context of their use,inter alia,in environmental protection.

One-step hydrothermal synthesis of S-defect-controlled ZnIn_(2)S_(4) microflowers with improved kinetics process of charge-carriers for photocatalytic H_(2) evolution

Engineering lattice defects in two-dimensional(2 D) sulfide semiconductors has been accepted as an effective strategy to enhance the efficiency of the solar-to-fuels conversion.Although many researches have proven the lattice defect-mediated photocatalytic activity of ZnIn_(2)S_(4),the artificial control of Sdefects for optimizing the charge-carrier kinetics process in ZnIn_(2)S_(4) has long been a challenging task.Herein,we report a facile one-step method to modulate the lattice S-content of ZnIn_(2)S_(4) microflowers(MFs) only through adjusting the used amount of S-precursor in the hydrothermal solution that contains the metal precursors with a fixed Zn/In stoichiometric ratio at 1:2.We also demonstrated that the Svacancies at the In facets were the main type of lattice defects in the formed ZnIn_(2)S_(4) MFs,which could enhance both the separation and migration processes of the photoinduced charge-carriers due to the existence of discrete defect energy-levels(DELs) and the reduced effective mass of electrons,as evidenced by the first-principles calculations and the electron spectra analyses.The ZnIn_(2)S_(4) MFs with the optimal content of S-vacancy obtained by a hydrothermal treatment of the precursors with the Zn/In/S stoichiometric ratio of 1:2:8 possessed the long-lived photoinduced electron(~94.64 ns) for contributing to the photo-physical and-chemical processes.Thus,upon visible light irradiation,the H_(2)-evolution rate of this sample reached ~2.40 mmol h^(-1) g^(-1) with an apparent quantum efficiency of ~0.16% at 420 nm even though only using 5 mg of photocatalysts without any cocatalysts.

Hydrothermal Synthesis and Characterization of PEG-Mn_3O_4 Nanocomposite

Here, we report on the synthesis of PEG-Mn_3O_4 nanocomposite(NP's) via a hydrothermal route by using Mn(acac)2, ethanol, NH3 and PEG-400. The crystalline phase was identified as Mn_3O_4. The crystallite size of the PEG-Mn_3O_4 nanocomposite was calculated as 12±5 nm from X-ray line profile fitting and the average particle size from TEM was obtained as 200 nm. This reveals polycrystalline character of Mn_3O_4 NP's. The interaction between PEG-400 and the Mn_3O_4 NP's was investigated by FTIR. Temperature independent AC conductivity of PEG-Mn_3O_4 nanocomposite beyond 20 k Hz provides a strong evidence of ionic conduction through the structure. The conductivity and permittivity measurements strongly depend on the secondary thermal transition of nanocomposite beyond 100. Above that temperature, Mn_3O_4 particles may interact with each other yielding a percolated path that will facilitate the conduction. On the other hand, the relatively lower activation energy(Ea=0.172 e V) for relaxation process suggests that polymer segmental motions of PEG and electrons hopping between Mn2+and Mn3+may be coupled in the sample below 100. Room temperature magnetization curve of the sample does not reach to a saturation, which indicates the superparamagnetic character of the particles. As the temperature increases, the frequency at which(ε′′) reaches a maximum shifted towards higher frequencies. The maximum peak was observed at 1.4 k Hz for 20 while the maximum was detected at 23.2 k Hz for 90.

Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H_3NC_2H_4NH_2]VOPO_4

An inorganic-organic hybrid compound, [H3NC2H4NH2]VOPO4 was synthesized by meansof the hydrothermal method. It was crystallized in a monoclinic system, a space group P21/c,with the crystal cell parameters: a=0. 922 85(11) nm, b=0. 729 94(9) nm, c=0. 984 95(11)nm, β=101. 280(3)°, V=0. 650 67(13) nm3, Mr=223.02 g/mol, Dc=2. 277 g/cm3, Z=4,R= 0. 031 5, ωR= 0. 086 5, GOF = 1. 085. The VO5N octahedra chains are corner-linked byPO4 tetrahedra; the VOsN octahedra are all trans-linked with V-O bonds being alternately short and long. The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO4 from a neighboring sheet. The elementary analysis, infrared spectrum characters and thermal stability were also given.

Mild Hydrothermal Synthesis and Optical Properties of the Complex Fluoride KMgF_3 Doped with Eu

KMgF3 doped with Eu was synthesized by mild hydrothermal method at 240C for the first time. The excitation and emission spectra of the KMgF3 : Eu2+ phosphor were measured. Comparing with the sample synthesized through solid state reaction, the variation in the excitation spectra at 360 nm resulted from the existences of VK color centers; the low emission intensity was due to Eu2+ having transferred part energy to VK color centers.

Hydrothermal Synthesis of V-Cr-Al-O Nanospheres and Their Effect on Decomposition of Ammonium Perchlorate

V-Cr-Al-O nanospheres were successfully synthesized using V2O5, Al(OH)3, CrO3, and H2C2O4·H2O as the starting materials by a facile one-pot hydrothermal approach. Several techniques containing X-ray powder diffraction, hydrogen temperature programmed reduction, scanning electron microscopy were used to characterize the composition, morphology and redox property of V-Cr-Al-O nanospheres. The catalytic behavior of prepared nanospheres on the thermal decomposition of AP was investigated by the thermogravimetric analysis and differential thermal analysis(TG/DTA). The experimental results show that the thermal decomposition temperature of AP in the presence of V-Cr-Al-O nanospheres is to 395 ℃(decreased by 35 ℃), which proves better catalyst for the thermal decomposition of AP.

Effects of Processing Conditions on Hydrothermal Synthesis of K_(0.5)Bi_(0.5)TiO_3 Nano-Powders

Potassium bismuth titanate nanosized powders were prepared by the hydrothermal method using Ti(C_4H_9O)_4 and Bi(NO_3)_3·5H_2O as raw materials in alkaline solution.The phase composition,particle size and morphology of the powders were studied by XRD and TEM analysis.The results showed that the powders were well crystallized and dispersed.The crystal phase of the powders was K_(0.5)Bi_(0.5)TiO_3 with the grain size of about 50 nm～100 nm.Hydrothermal temperature and alkaline concentrations had great effects on the phase composition and morphology of the resultant powders.Pure K_(0.5)Bi_(0.5)TiO_3 powders could be synthesized at 170℃～180℃with KOH concentration of 8 mol/L～12 mol/L.

Hydrothermal Synthesis and Structure of[{Mo_8V_4O_(36)(VO_4)(VO)_2}n]^(7n-)Bi-capped α-Keggin Fragments Linked to a Chain

The title compound, (H2en)3H3O{Mo8V4O36(VO4) (VO)2} ?4H2O, was hydrothermally synthesized and structurally characterized by means of IR, ESR spectrum and single crystal X-ray diffraction. It crystallized in a monoclinic system with space group P21/c, a=1. 980 4(4) nm, 6=2. 063 4(4) nm, c=l. 192 0(2) nm, =94. 76(3)?and deep black colour. The compound contains V-centered bi-capped a-Keggin fragments {Mo8V7O42} that are linked together by edge-shared units V O5 via V-O-V bonds, forming a chain.

Hydrothermal synthesis and characterization of carbon-doped TiO2 nanoparticles

We report the hydrothermal growth of pure and doped TiO2 nanoparticles with different concentrations of carbon.The microstructure of the as-synthesized samples is characterized by x-ray diffraction(XRD),field emission scanning electron microscopy(FESEM),energy dispersive x-ray spectroscopy(EDX),and Raman spectroscopy to understand the structure and composition.The XRD patterns confirm the formation of anatase phase of TiO2 with the average crystallite size is calculated to be in the range of 13 nm to 14.7 nm.The functional groups of these nanostructures are characterized by Fourier transformed infrared(FT-IR)spectroscopy,which further confirms the single anatase phase of the synthesized nanostructures.UV-visible absorption spectroscopy is used to understand the absorption behavior,which shows modification in the optical bandgap from 3.13 eV(pure TiO2)to 3.74 eV(1.2 mol%C-doped TiO2).Furthermore,the Ti^3+centers associated with oxygen vacancies are identified using electron paramagnetic resonance spectroscopy(EPR).

Hydrothermal Synthesis of Pb_(1-1.5x)La_xZr_(0.5)Ti_(0.5)O_3 (x = 0.01-0.06) Nanocrystallites

Nanocrystalline Pb1-1.5xLaxZr0.5Ti0.5O3 (x = 0.01-0.06, PLZT) powders with particle size from 30 to 150 nm were hydrothermally synthesized from the gels under mild conditions. The reaction conditions such as La content, reaction temperature and time were studied in detail and optimal conditions were established for synthesizing PLZT powders with different La contents. The effects of La content, alkali concentration, reaction temperature and time on the particle size were studied.

Hydrothermal Synthesis and Crystal Structure of a New Supramolecular Channel Framework Based on Cu Complexes and Polyoxovanadate:[Cu(I)(phen)_2]_5[HV_(15)O_(36)(Cl)]_(0.65)[H_3V_(16)O_(38)(Cl)]_(0.35)·2H_2O

A new compound [Cu(I)(phen)2]5[HV15O36(Cl)]0.65[H3V16O38(Cl)]0.352H2O 1 (phen = 1,10-phenanthroline) has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O42H2O, THMAM (tris(hydroxymethyl)aminomethane) and H2O in the molar ratio of 3:1:1:0.5:2.5:1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009(8), c = 28.401(2) , V = 13129.5(12) 3, Z = 4, Dc = 1.800 g/cm3, μ(MoKα) = 1.932 mm-1, λ(MoKα) = 0.71073 , F(000) = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR = 0.1320 for 7761 observed reflections (I > 2σ(I)). Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.

Hydrothermal Synthesis,Crystal Structure and Fluorescent Property of a Novel Mo(V) Phosphate [Zn(Mo^v_6P_4O_(31)H_(10))_2(C_4H_(14)N_3)_2]·2C_4H_(13)N_3·8H_2O

A new molybdenum phosphate [Zn(Mov6P4O31H10)2(C4H14N3)2](2C4H13N3(8H2O 1 (C4H13N3 = diethylenetriamine) has been synthesized under hydrothermal condition. Single-crystal X-ray diffraction reveals that compound 1 crystallizes in the monoclinic, space group P21/n, a = 13.1679(3), b = 22.1240(6), c = 13.6146(3) , β = 103.4847(7)(, V = 3856.95(16) 3, C16H90N12O70P8ZnMo12, Mr = 3035.41, Z = 2, Dc = 2.614 g/cm3, μ = 2.483 mm-1, F(000) = 2968, S = 1.014, the final R = 0.0196 and wR = 0.0506 for 7486 observed reflections (I > 2((I)). Compound 1 consists of two identical rings of six edge-sharing MoO6 octahedra interconnected by one ZnO6 octahedron, whereas the PO4 tetrahedra which share their apices with the MoO6 octahedra are only located on one side of each Mo6 ring. The 2-charge of polyanion [Zn(Mov6P4O31H10)2]2- unit is compensated in the crystal by two mono-protonated diethylenetriamines (C4H14N3)+. By hydrogen bonding interactions the polyanion of compound 1 is interconnected to form pseudo three- dimensional molybdophosphate. Other characterizations by elemental analyses, IR spectrum and fluorescent spectrum are also described.

Hydrothermal Synthesis of Ordered ZnO Nanorod Arrays by Nanosphere Lithography Method

Ordered ZnO nanorod arrays were hydrothermally synthesized on a patterned GaN substrate formed by a nanosphere lithography method.Firstly,polystyrene(PS)nanospheres were used to self-assemble a close-packed monolayer on the surface of water.Then the monolayer was transferred onto a GaN substrate.Subsequently,magnetron sputtering of SiO2 was used to reduce the size of PS nanospheres and cover the interstitial space between PS nanospheres by SiO_(2) at the same time.After removing the PS nanospheres,periodic seed sites were accomplished on the GaN substrate for ZnO growth.Finally,ordered ZnO nanorod arrays,perpendicular to the substrate,were grown on GaN substrates by a hydrothermal method.This work provides a potential low-cost hydrothermal method for the preparation of ordered semiconductor nanorod arrays.

Hydrothermal Synthesis of Orthorhombic LiMnO_(2)Nano-Particles and LiMnO_(2)Nanorods and Comparison of their Electrochemical Performances

Orthorhombic LiMnO_(2)nanoparticles and LiMnO_(2)nanorods have been synthesized by hydrothermal methods.LiMnO_(2)nanoparticles were synthesized by simple one-step hydrothermal method.To obtain rod-like LiMnO_(2),γ-MnOOH nanorods were first synthesized and then the H+ions were completely replaced by Li+resulting in LiMnO_(2)nanorods.Their electrochemical performances were thoroughly investigated by galvanostatic tests.Although the LiMnO_(2)nanoparticles have smaller size than LiMnO_(2)nanorods,the latter exhibited higher discharge capacity and better cyclability.For example,the discharge capacities of LiMnO_(2)nanorods reached 200 mA·h/g over many cycles and remained above 180 mA·h/g after 30 cycles.However,the maximum capacity of LiMnO_(2)nanoparticles was only 170 mA·h/g and quickly decreased to 110 mA·h/g after 30 cycles.Nanorods with one-dimensional electronic pathways favor the transport of electrons along the length direction and accommodate volume changes resulting from charge/discharge processes.Thus the morphology of LiMnO_(2)may play an important role in electrochemical performance.