Synthesis and characterisation of In(OH)3 and In2O3 nanoparticles by sol-gel and solvothermal methods

Indium hydroxide nanostructures were synthesised by sol-gel and hydrothermal processes from indium acetate and sodium hydroxide as precursors and polyvinyl alcohol, polyvinyl pyrrolidone or polydimethylsiloxane as stabilisers. Calcination of the In(OH)₃ nanostructures at 500°C in air yielded In₂O₃ nanoparticles. The morphology, crystallinity and thermal behaviour of the obtained products of each method were investigated by X-ray diffraction, scanning electron microscopy and thermal gravimetry analysis and differential thermal analysis.     

溶胶-凝胶燃烧法制备La_2O_3和La(OH)_3纳米晶的研究

采用燃烧法合成纳米La(OH)3材料,分别以硝酸镧和柠檬酸为镧源和络合剂,以氨水调节pH值为2～4、柠檬酸与硝酸镧的物质的量比为1～1.2∶1之间,加热凝胶至自蔓延燃烧后并在700～750℃煅烧1～2 h,得到膨松粉末状产物,即La2O3纳米晶。利用X射线衍射和透射电镜等测试方法对凝胶热分解过程及最终形成的La2O3纳米晶颗粒进行分析和表征。结果表明:用该方法得到的纳米La2O3产物的平均粒径在30～100 nm之间可控;纳米La2O3在空气中是不稳定的,在自然吸潮情况下和空气中的H2O发生反应生成La(OH)3,控制湿度即可得到纯La(OH)3纳米晶。     

阴离子（NO3－／Cl －／SO2－4）对 Ni（OH）2晶型及其结构稳定性的影响

采用超声波辅助沉淀法分别在单元掺杂、二元掺杂和不掺杂三种情况下制备了三种不同镍源的纳米氢氧化镍,研究三种阴离子（NO3－,Cl－,SO2－4）对产物晶相结构及稳定性的影响。结果表明：未掺杂时,半径较大的SO2－4离子有利于α‐Ni（OH）2的形成;在单掺杂Co（Ni2＋∶Co2＋＝1∶0．20）时,NO3－离子不仅有利于α‐Ni（OH）2的形成,而且可以使α‐Ni（OH）2在碱液中保持较高的稳定性;当复合掺杂Co／Cu（Ni2＋∶Co2＋∶Cu2＋＝1∶0．15∶0．05）时,三种镍源制得的样品均为纯α‐Ni（OH）2结构,但以Ni（NO3）2为镍源的α‐Ni（OH）2在碱液中结构稳定性较高,NiCl2次之,NiSO4较差。可见,α‐Ni（OH）2结构及稳定性既与掺杂情况有关,也与阴离子密切相关。     

水相沉淀法制备纳米片状钼铜矿（Cu3（MoO4）2（OH）2）（英文）

以硝酸铜、钼酸钠及氢氧化钠为原料,采用简单的水相沉淀法,在60℃下合成出钼铜矿(Cu3(MoO4)2(OH)2).通过X射线衍射、扫描电镜、透射电镜、热重与差热分析、红外光谱及荧光光谱等测试手段对材料的微观结构、形貌、热稳定性及谱学特性进行表征分析.结果显示,制备的产物为结晶性良好的、至少一维是纳米的片状结构材料,属于单斜型(晶胞参数a=0.53863 nm,b=1.40006 nm,c=0.56003 nm),其元素摩尔含量比约为3:2:10,与推测的分子式完全吻合.热重与差热分析数据表明Cu3(MoO4)2(OH)2纳米晶具有很好的热稳定性且起始分解温度为320℃.通过软件测得的d(021)面与d(ī21)面的晶间面距分别为0.435 nm与0.358 nm,与理论值基本相符.经测量,Cu3(MoO4)2(OH)2纳米晶具有强的荧光性质,在激发波长369 nm的作用下在530 nm表现为强发射峰.此外,还探讨了Cu3(MoO4)2(OH)2纳米晶的形成机理.     

燃烧合成Co（Ti）-Al2O3金属陶瓷的组织与性能

利用低放热Al-TiO2反应体系部分取代高放热Al-CoO反应体系,并加入适量的稀释剂Al2O3吸收反应热量,通过热爆燃烧合成结合致密化工艺制备了铁磁性Co(Ti)-Al2O3金属陶瓷。研究表明,Co(Ti)-Al2O3金属陶瓷中随着Al-TiO2体系的增加,燃烧反应温度降低,金属相尺寸减小,分布更均匀,同时在金属相与基体之间形成过渡区域,提高了界面结合。Co(Ti)-Al2O3复合材料的饱和磁化强度随着金属Co含量增加而增加,最高可达到37.2849Am2/kg,而矫顽力在3997.6～5615.4A/m范围内变化,介于软磁体和硬磁体之间。     

Facile synthesis and capacitive characteristics of Co(OH)2 nanoflakes via a solid-reaction route at room temperature

Flake-like β-Co(OH)₂ with dimension around 20-50 nm was conveniently synthesized via a simple, low cost and practical room-temperature solid-state reaction with the assistance of polyethylene glycol (PEG) 400 and its electrochemical properties were evaluated using cyclic voltammetry (CV) and galvanostatic charge-discharge technology. A high specific capacitance of 658.4 F g^− 1 at 5 mA was observed for the β-Co(OH)₂ nanoflakes, compared to 302.7 F g^− 1 for the block-like β-Co(OH)₂ obtained without the PEG-400, showing the morphological function of nanoflakes for improving the capacitive performance. Furthermore, the β-Co(OH)₂ nanoflakes can offer a good specific capacitance retention of ca. 80% after 1000 cycles, suggesting its potential application in supercapacitors.     

NiaSi2O5（OH）4 Multi-Walled Nanotubes with Tunable Magnetic Properties and Their Application as Anode Materials for Lithium Batteries

Highly crystalline and thermally stable pure multi-walled Ni₃Si₂O₅(OH)₄ nanotubes with a layered structure have been synthesized in water at a relatively low temperature of 200–210 °C using a facile and simple method. The nickel ions between the layers could be reduced in situ to form size-tunable Ni nanocrystals, which endowed these nanotubes with tunable magnetic properties. Additionally, when used as the anode material in a lithium ion battery, the layered structure of the Ni₃Si₂O₅(OH)₄ nanotubes provided favorable transport kinetics for lithium ions and the discharge capacity reached 226.7 mA·h·g⁻¹ after 21 cycles at a rate of 20 mA·g⁻¹. Furthermore, after the nanotubes were calcined (600 °C, 4 h) or reduced (180 °C, 10 h), the corresponding discharge capacities increased to 277.2 mA·h·g⁻¹ and 308.5 mA·h·g⁻¹, respectively.      

Pb(Fe2/3W1/3)O3的制备及其介电性能研究

本文采用半化学法,即硝酸铁代替传统氧化物混合法中的三氧化二铁与PbO和WO3浆料混合,经850℃,2h预烧,一步合成了钙钛矿单相的Pb(Fe2/3W1/3)O3(PFW)预烧粉体;再经870℃和2h烧结,得到了纯钙钛矿相的PFW陶瓷,其理论密度大于98%,在1kHz时的最大介电常数εmax为8000,高于二次合成法和传统氧化物法制备的PFW陶瓷,表明半化学法对制备PFW陶瓷是可行的.     

Hydrothermal synthesis of Zn3(OH)2V2O7·nH2O nanosheets and its application in lithium ion battery

Well crystallized zinc vanadium oxide hydroxide hydrate (Zn₃(OH)₂V₂O₇·nH₂O) nanosheets have been successfully synthesized by a simple hydrothermal method. The products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and Raman spectrum. The composition of Zn₃(OH)₂V₂O₇·nH₂O has been studied by thermal analysis (TG, DTA). The results indicate that there are two water molecules in Zn₃(OH)₂V₂O₇·nH₂O molecular formula. Electrochemical properties of Zn₃(OH)₂V₂O₇·nH₂O nanosheets as negative electrode of lithium ion battery were studied by conventional charge/discharge test, which shows steady platform near 1.4 V, suggesting it as an ideal candidate of negative material for lithium ion battery.     

Characterisation of binary (Fe3O4/SiO2) biocompatible nanocomposites as magnetic fluid

This article describes coating of magnetite nanoparticles (NPs) with amorphous silica shells. Controlled co-precipitation technique under N₂ gas was used to prevent undesirable critical oxidation of Fe²⁺. The synthesised Fe₃O₄ NPs were first coated with trisodium citrate to achieve solution stability and then covered by SiO₂ layer using Stober method. For uncoated Fe₃O₄ NPs, the results showed an octahedral geometry with saturation magnetisation range of 82–96?emu/g and coercivity of 85–120?Oe for particles between 35 and 96?nm, respectively. The best value of specific surface area (41?m²/g) for Fe₃O₄ alone was obtained at 0.9?M NaOH at 750?rpm and it increased to about 81?m²/g for Fe₃O₄/SiO₂ combination. The total thickness and the structure of core–shell was measured and studied by transmission electron microscopy. The average particles size was about 50?nm, indicating the presence of about 15?nm SiO₂ layer. Finally, the stable magnetic fluid contained well-dispersed magnetite-silica nanocomposites which showed monodispersity and fast magnetic response.     

化学表面处理对微型化的氮氧化硅驻极体层电荷储存性能的影响

研究了化学表面处理对微型化的氮氧化硅膜电荷稳定性的影响,考察了表面处理对脱阱面电荷横向扩散的抑止作用。借助对微型化前后的样品在高温和高湿环境中的表面电位衰减测量的对比,研究了不同试剂的表面处理对微型化样品的电荷储存及其动态特性的影响。     

Synthesis of Nanotubular Mg3Si2O5(OH)4-Ni3Si2O5(OH)4 Silicates at Elevated Temperatures and Pressures

Mg₃Si₂O₅(OH)₄-Ni₃Si₂O₅(OH)₄ nanotubes with the chrysotile structure and MgO : NiO molar ratios of 1 : 2 and 2 : 1 are synthesized by hydrothermal reactions at temperatures from 250 to 450°C and pressures from 30 to 100 MPa. The reaction path and kinetics, as well as the dimensions and morphology of the resulting nanotubes, are shown to depend on the nature of the starting reagents, chemical composition of the reaction system, and hydrothermal synthesis conditions. At higher nickel concentrations in the hydrous silicates, nanotube formation requires higher temperatures, longer hydrothermal treatment times, and higher NaOH concentrations in the reaction system.__________Translated from Neorganicheskie Materialy, Vol. 41, No. 7, 2005, pp. 849–855.Original Russian Text Copyright © 2005 by Korytkova, Maslov, Pivovarova, Polegotchenkova, Povinich, Gusarov.     

Synthesis and characterization of the open-framework cobalt borophosphate: (C4N2H12)Co[B2P3O12(OH)]

A high yield hydrothermal synthesis of the open-framework cobalt borophosphate (C₄N₂H₁₂)Co[B₂P₃O₁₂(OH)], has been developed. The compound was characterized by single crystal X-ray diffraction methods, thermogravimetric analysis, vibrational (IR and Raman) spectroscopy and magnetic measurements. In the structure Co(II)O₆ octahedra, BO₄ and PO₄ tetrahedra form nine-member rings which in turn are linked to form CoBPO layers parallel to the bc plane. The layers are joined together by another set of PO₄ tetrahedra and the (piperazinium)²⁺ cations occupy the channels running along [1 0 0]. The structure is compared with that of (C₂N₂H₁₀)Co[B₂P₃O₁₂(OH)].     

Synthesis of BaTiO3 nanoparticle/poly(2-hydroxyethyl methacrylate) hybrid nanofibers via electrospinning

BaTiO₃ nanoparticle/poly(2-hydroxyethyl methacrylate) (PHEMA) hybrid nanofibers were fabricated from an in situ synthesized BaTiO₃ nanoparticle/polymer hybrid by electrospinning. The bulk hybrid for nanofibers was synthesized through the in situ hydrolysis of Ba–Ti alkoxide modified with 2-vinyloxyethanol and subsequent copolymerization with HEMA monomer. IR and ¹³C NMR spectra showed the formation of polymer matrix. The molecular weights of BaTiO₃ nanoparticle/PHEMA hybrid for spinning were 1.3 × 10⁵ for 20 equiv. PHEMA and 5.7 × 10⁵ for 30 equiv. PHEMA. The crystallite size of BaTiO₃ particles in the hybrid was 4.5 nm according to the Scherrer equation. The diameter of BaTiO₃ nanoparticle/PHEMA hybrid nanofibers ranged from 500 nm to 1 μm. A field stress–strain curve was observed for the BaTiO₃ nanoparticle/PHEMA hybrid nanofiber.     

Synthesis of Cu3(PO4)2 · H2O based solid solutions through Co or Ni substitution for Cu

New substitutional solid solutions have been synthesized: (Cu_{1 ? x} Co_x)₃(PO₄)₂ · H₂O (0 < x ≤ 0.20), (Cu_{1 ? x} Ni_x)₃(PO₄)₂ · H₂O (0 < x ≤ 0.12), and (Cu_{1 ? y} Co_y)₃(PO₄)₂ · H₂O (0.55 ≤ y ≤ 0.65). The first two solid solutions are isostructural with Cu₃(PO₄)₂ · H₂O (monoclinic symmetry, sp. gr. C2/c); the third solid solution also has a monoclinic structure, which is a Cu₃(PO₄)₂ · H₂O related superstructure. The lattice parameter b of (Cu_{1 ? y} Co_y)₃(PO₄)₂ · H₂O (0.55 ≤ y ≤ 0.65) is almost twice that of (Cu_{1 ? x} Co_x)₃(PO₄)₂ · H₂O (0 < x ≤ 0.20), while their a and c parameters differ little. The solid solutions have been characterized by chemical analysis, x-ray diffraction, IR spectroscopy, and thermal analysis.