Synthesis and Characterization of La（OH）3 Nanorods by Hydrothermal Microemulsion Method

La（OH）3 nanorods with diameters of 20-40 nm and lengths of 200-300 nm were synthesized by a hydrothermal microemulsion method. The structure and morphology of the final products were characterized by X-ray powder diffraction （XRD）, transmission electron microscopy （TEM）, and field emission scanning electron microscope （FESEM）.     

Fabrication of Cu(OH)<Subscript>2</Subscript> Nanowires Blended Poly(vinylidene fluoride) Ultrafiltration Membranes for Oil-Water Separation

Cu(OH)2 nanowires were prepared and incorporated into poly(vinylidene fluoride) (PVDF) to fabricate Cu(OH)2-PVDF ultrafiltration (UF) membrane via immersion precipitation phase inversion process.The effect of Cu(OH)2 nanowires on the morphology of membranes was investigated by X-ray photoelectron spectroscopy (XPS),Fourier transform infrared (FTIR) spectroscopy,atomic force microscopy (AFM),scanning electron microscopy (SEM) and X-ray diffraction (XRD) measurements.The results showed that all the Cu(OH)2-PVDF membranes had wider fingerlike pore structure and better hydrophilicity,smoother surface than pristine PVDF membrane due to the incorporation of Cu(OH)2 nanowires.In addition,water flux and bovine serum albumin (BSA) rejection were also measured to investigate the filtration performance of membranes.The results indicated that all the Cu(OH)2-PVDF membranes had high water flux,outstanding BSA rejection and excellent antifouling properties.It is worth mentioning that the optimized performance could be obtained when the Cu(OH)2 nanowires content reached 1.2 wt％.Furthermore,the membrane with 1.2 wt％ Cu(OH)2 nanowires showed outstanding oil-water emulsion separation capability.     

Synthesis of Mg5(CO3)4(OH)2·4H2O with Flower-like Microstructure and Its Catalytic Activity for Transesterification of Dimethyl Carbonate with Phenol

A novel flower-like hydrated magnesium carbonate hydroxide,Mg_5(CO_3)_4(OH)_2·4H_2O,with micro-structure composed of individual thin nano-sheets was synthesized using a facile solution route without the use of template or organic surfactant.Reaction time has an important effect on the final morphology of the product.The micro-structure and morphology of Mg_5(CO_3)_4(OH)_2·4H_2O were characterized by means of X-ray diffractometry(XRD),field-emission scanning electron microscopy(FE-SEM).Brunauer-Emmett-Teller(BET)surface areas of the samples were also measured.The probable formation mechanism of flower-like micro-structure was discussed.It was found that Mg_5(CO_3)_4(OH)_2·4H_2O with flower-like micro-structure was a novel and efficient catalyst for the synthesis of diphenyl carbonate(DPC)by transesterification of dimethyl carbonate(DMC)with phenol.     

Synthesis and Characterization of SnO2 One-dimensional Nanostructures

Single-crystalline SnO2 nanowires have been successfully prepared in large scale on Au-coated silicon substrate by heating the mixture of self-made high-purity SnO2 powders and graphite powders at 900℃. Besides the line type nanowires some more features were observed. The products were characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED) and Raman spectrum techniques. The results indicate that the tin dioxide nanowires have a rutile structure with diameters ranging from 30 to 120 nm and lengths up to several tens of micrometers. The possible mechanism of the growth and reaction for the nanowires was also discussed.     

Preparation and Characterization of Cu_3V_2O_7(OH)_2·2H_2O Hollow Spheres from Na_2V_6O_16·3H_2O Nanobelts

Monoclinic Cu3V2O7(OH)2·2H2O(copper polyvanadate) hollow spheres were prepared with Na2V6O16· 3H2O nanobelts as V-precursor by hydrothermal method. The purity and structure of the products were characterized by X-ray powder diffraction(XRD), Fourier transform infrared(FTIR) spectroscopy, Raman spectroscopy, thermogra-vimetric analysis(TGA) and X-ray photoelecton spectroscopy(XPS). The morphology and size were observed by scanning electron microscopy(SEM). We found that the Kagomé staircase-structural copper...     

Preparation and characterization of gadolinium hydroxide single-crystalline nanorods by a hydrothermal process

The Gd(OH)3 nanorods with diameters of ca.40-60 nm and lengths of more than 400-550 nm have been prepared by a novelhydrothermal technique.The structural features and chemical composition of the nanorods were investigated by X-ray diffraction(XRD),transmission electron microscopy(TEM),and field emission scanning electron microscope(FESEM),selected areaelectron diffraction(SAED),and high resolution transmission electron microscopy(HRTEM).The possible mechanism for theformation of Gd(OH)3 nanorods was proposed.     

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)26H2O 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.     

Synthesis of three-dimensional hierarchical cobalt hydroxide microstructures

β-Co(OH)2 with three-dimensional (3-D) structures was prepared by a simple hydrothermal method. It was found that the amount of cetyltrimethylammonium bromide (CTAB), the pH value, and the reaction time all had an important influence on the formation of this morphology. The products were characterized by X-ray diffraction, energy-dispersive X-ray analysis, and scanning electron microscopy. A possible mechanism of the formation of the 3-D microstructures of β-Co(OH)2 was proposed.     

Fe(OH)2悬浮液在EDTA作用下氧气氧化生成δ-FeOOH的机理研究

At room temperature and in the presence of trace EDTA, the formation of δ-FeOOH was studied by the rapid oxidation of Fe(OH)2 suspension with O2. The structural and morphological changes were characterized by various techniques such as XRD, FTIR and TEM. γ-FeOOH and δ-FeOOH formed simutaneously in the early period of oxidation. But as the rate of mass transfer was in equilibrium, trace γ-FeOOH vanished gradually. Accordingly, pure phase δ-FeOOH was obtained. At the same time, critical amount ratio K of EDTA to Fe^2 was verified. The experiments show that the reactivity, rate of the oxidizing agent and pH of the initial medium were important factors for the formation of pure phase δ-FeOOH. Under the auxiliary effect of EDTA, the reactivity of O2 was nearly improved to that of H2O2. And the process of the oxidation that Fe(OH)2 suspension was oxidized by O2 under that condition was discussed.     

Preparation of Nanocrystalline MoS2 Hollow Spheres

NanocrystaUine MoS2 with hollow spherical morphology has been prepared by the hydrothermal method. The products are characterized by means of X-ray powder diffraction,transmission electron microscopy and high-resolution transmission electron microscopy. The experimental results give the evidence that the sample is consists of hollow spheres 400～600nm in diameter, and there is much whisker on the surface of MoS2 hollow sphere.     

Controlled synthesis of single-crystalline Mg(OH)2 nanotubes and nanorods via a solvothermal process

The synthesis of Mg(OH)₂ one-dimensional (1D) nanostructures was systematically investigated in different solvents at various temperatures with Mg₁₀OH₁₈Cl₂·5H₂O nanowires as source materials. The results showed that the characters of the products, such as crystal size, shape, and structure, were strongly influenced by the solvent and temperature during the solvothermal process. 1D nanotubes of Mg(OH)₂, with 80-300 nm outer diameter, 30-80 nm wall thickness, and several tens of micrometers in length were obtained by choosing bidentate ligand solvents such as ethylenediamine and 1,6-diaminohexane as the reaction solvent. But when using monodentate ligand pyridine as the reaction solvent, the obtained samples showed nanorods morphology. The Mg(OH)₂ thus produced was analyzed by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), high-resolution electron microscopy (HRTEM), and selected-area electron diffraction (SAED). The possible growth mechanism of the 1D nanostructure Mg(OH)₂ was discussed.     

Facile Synthesis of Leaf-like Cu(OH)2 and Its Conversion into CuO with Nanopores

Leaf-like Cu(OH)₂ single crystals were synthesized via the controlled emulsion interface method using Span80 (sorbitan monooleate) as the stabilizer of the emulsion system. CuO products with nanopores could be simply obtained by the dehydration of Cu(OH)₂, while maintaining the strip-shaped architecture. The phase structures and morphologies were measured by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectra, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Experimental results showed that Cu(OH)₂ microleaves were single crystals and the growth direction seemed to be in [111] crystal plane of the orthorhombic Cu(OH)₂. The formation of the nanopores should be attributed to the water loss of the transformation from Cu(OH)₂ to CuO. The formation process of Cu(OH)₂ was investigated by taking TEM images at different stages of the reaction. The formed nanoparticles began to rearrange to form nanorods and microleaves possibly via edge-by-edge and side-by-side oriented-attachments because of the formation of larger crystals greatly reducing the interfacial energy. Besides, CuO microarchitectures exhibit blue shifts in UV-Vis spectra and possess larger band gaps compared with those of bulk crystals.     

Sacrificial template growth of CdS nanotubes from Cd(OH)2 nanowires

A diffusion-controlled process was proposed for the preparation of inorganic nanotubes from nanowires. The preformed Cd(OH)₂ nanowires were used as the sacrificial templates to generate CdS nanotubes with different wall thickness. The axle-sleeve transition state found in-between the precursor and the formation of products proves the diffusion-controlled mechanism. CdS nanotubes can be prepared via this method at different temperature and with various sulfide sources. X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) results showed that all obtained CdS nanotubes consist conglomerated crystallites, and the crystallinity can be altered by changing the temperature of the growth process. The wall thickness of the produced CdS nanotubes can be controlled by changing the concentration of the sulfide source and stopping the reaction at different stages.     

矿化剂对水热法改性氢氧化镁晶体的影响

近几年来,氢氧化镁作为一种无机阻燃剂由于其具有制备条件相对温和,生产工艺简单且产品与自然环境友好等特点,在研究及生产活动方面备受关注且得到了长足的发展[1～4].目前采用氢氧化钠法进行反应一水热制备高分散阻燃级氢氧化镁的工艺路线已经比较成熟[5～8].然而,不利的是,氢氧化钠偏高的价格导致了产品的制造成本较高.而采用石灰法制备氢氧化镁阻燃剂具有价格低廉的特点,引起了人们的关注.     

3D nanostructured Ni(OH)2 microspheres as an efficient immobilization matrix of Ru(bpy)3 for high-performance electrochemiluminescence sensor

The electrochemistry and electrochemiluminescence (ECL) of novel three-dimensional nanostructured Ru(bpy)₃²⁺/Ni(OH)₂ microspheres were investigated for the first time. The negatively charged porous Ni(OH)₂ microspheres composed of Ni(OH)₂ nanowires were specifically designed to interact with Ru(bpy)₃²⁺. The large surface area and porous structure of Ni(OH)₂ microspheres enhance loading of Ru(bpy)₃²⁺ and mass transport of the model analyte, tripropylamine (TPA). Excellent ECL performance of the presented sensor was achieved including good stability and wide linear range from 7.7 × 10⁻¹⁰ to 3.8 × 10⁻³ M with the detection limit of 2.6 × 10⁻¹⁰ M to TPA.     

La(OH)3和 La2O2CO3纳 米 棒 的 合 成 及 其 催 化 Claisen-Schmidt缩合反应性能简

通过调节溶液的pH值,在水热条件下合成出长径比为2-45的La（OH）₃纳米棒. 对水热合成过程中间体的结构演变分析,发现高碱度有利于小尺寸晶核的形成,La（OH）₃晶体结构的各向异性导致这些晶种沿着C轴方向生长,进而形成纳米棒结构. 将La（OH）₃纳米棒前驱体于773 K焙烧可以得到长径比为2-20的La₂O₂CO₃纳米棒. 随着长径比的增加,La₂O₂CO₃纳米棒暴露的（110）晶面逐渐增加,La³⁺-O^2-碱性位的数目也从0.08增加到0.24 mmol/g. 因此,在Claisen-Schmidt缩合反应中,La₂O₂CO₃纳米棒催化剂上的反应速率随着长径比的增加而逐渐增大.     

Crystal structure and characterization of Rb2Ca[B4O5(OH)4]2·8H2O

Dirubidium calcium tetraborate octahydrate, Rb₂Ca[B₄O₅(OH)₄]₂·8H₂O, was prepared by reaction of Rb-borate aqueous solution with CaCl₂ and it's structure has been determined by single-crystal X-ray diffraction data. It crystallizes in the orthorhombic system, space group P2₁2₁2₁ with unit cell parameters, Z=4, The structure contains alternate layers of [B₄O₅(OH)₄]²⁻ polyanions separated by water molecules and Rb, Ca cations. The isolated [B₄O₅(OH)₄]²⁻ is constructed from two BO₃(OH) tetrahedron groups and two BO₂(OH) triangular groups joined at common oxygen atoms. The two BO₃(OH) tetrahedron groups are further linked by means of an oxygen bridge across the ring. The Ca²⁺ ion displays seven coordination, while the two non-equivalent Rb⁺ ions display nine and seven coordination, respectively. Infrared and Raman (4000-400 cm⁻¹) spectra of Rb₂Ca[B₄O₅(OH)₄]₂·8H₂O were recorded at room temperature and analyzed. Fundamental vibrational modes were identified and band assignments were made. The dehydration of this hydrated mixed borate occurs in one step and leads to an amorphous phase which undergoes a crystallization.     

氧化锌表面包覆Sn_6O_4(OH)_4的制备及其在锌镍电池中的应用

采用水热-共沉淀法在氧化锌表面包覆锡化合物,利用扫描电子显微镜(SEM)、X射线衍射(XRD)和能谱分析(EDS)对制备的包覆ZnO材料进行表征。结果表明:XRD表明附着在氧化锌表面的是Sn_6O_4(OH)_4,且结晶度较好;SEM测试显示在p H=12条件下,Sn_6O_4(OH)_4能够很好地附着在氧化锌颗粒表面;EDS显示组成物中的元素包含Zn、Sn、O三种元素。利用循环伏安曲线(CV)、电化学阻抗谱(EIS)、倍率充放电技术对包覆ZnO材料进行了电化学性能的测试,结果表明:包覆Sn_6O_4(OH)_4的ZnO可以提高锌负极的耐蚀性能,增大电荷转移电阻(Rct);锌电极覆Sn_6O_4(OH)_4量为3%时充放电效率最佳,在0.2C充放循环40次后充放电循环保持率仍有70%。     

La(OH)3负载锌铝水滑石的制备及其应用在锌镍二次电池中的性能

采用共沉淀法将氢氧化镧(La(OH)₃)负载在锌铝水滑石(Zn-Al LDHs)的表面,扫描电镜(SEM)、X射线衍射(XRD)表明La(OH)₃成功负载在锌铝水滑石表面,并且负载后的锌铝水滑石仍然为六边形片状晶体,且粒径均匀、分散性好。La(OH)₃质量其具有较好的可逆性、更大的正腐蚀电位及较小的电池内阻。5%La(OH)₃@Zn-Al LDHs在经过80次循环后,其循环保持率为94.84%。     

FeO(OH)-TiO2/CoPi复合光阳极的制备及其光电催化氧化水性能

采用溶胶-凝胶法制备了TiO₂ 纳米晶, 并通过浸渍技术在其表面引入了FeO(OH). 采用紫外-可见(UV-Vis)吸收光谱确定了引入FeO(OH)的最佳Fe³⁺浓度. 通过电化学法在FeO(OH)-TiO₂光阳极上沉积了催化水分解制备氧气的钴基催化剂(CoPi), 得到了FeO(OH)-TiO₂/CoPi 复合光阳极. 利用透射电镜(TEM), 高分辨透射电镜(HRTEM), X射线衍射(XRD), 扫描电镜(SEM)对TiO₂纳米晶, FeO(OH)-TiO₂以及FeO(OH)-TiO₂/CoPi复合光阳极进行了表征, 采用电化学和光电化学技术研究了中性条件下FeO(OH)-TiO₂/CoPi 复合光阳极的光电催化分解水性能. 结果表明, TiO₂纳米晶为梭形的锐钛矿, 其表面修饰的FeO(OH)为针铁矿型, 且当前驱体溶液中Fe³⁺与TiO₂的质量比为0.05%时得到的FeO(OH)-TiO₂具有最佳的光吸收效果. 形成FeO(OH)-TiO₂/CoPi复合光阳极后, 在光照条件下CoPi 电催化分解水制备氧气的过电位显著降低. TiO₂表面FeO(OH)的引入增加了光阳极对可见光的吸收能力, 同时光阳极表面沉积的CoPi有效地利用了FeO(OH)-TiO₂产生的光生空穴, 将水氧化形成氧气, 从而在光照条件下显著提高了CoPi催化氧化水的效率.