Preparation and characterization of yttria-stabilized zirconia nanotubes

Yttria-stabilized zirconia (YSZ) nanotubes were synthesized by the sol–gel method using porous anodic alumina oxide (AAO) as the templates. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersion X-ray (EDX) spectrum and selected area electron diffraction (SAED) techniques were used to characterize the morphology and crystalline structure of the prepared YSZ nanotubes. The length and the diameter of the YSZ nanotubes are 50 μm and 200 nm, respectively, which are in good agreement with the dimensions of the template pores, while the wall thickness of the nanotubes depends on the impregnation time. XRD and SAED measurements indicate that the obtained YSZ nanotubes after sintering at 1073 K possess a polycrystalline structure and a cubic crystal phase. Brunauer–Emmett–Teller (BET) measurement shows that the YSZ nanotubes have a surface specific area of around 40.5 m² g⁻¹ that is higher than that corresponding to the YSZ nanopowders.     

Preparation and characterization of nanocrystalline chromium boride

Nanocrystalline chromium boride (CrB) powders were successfully synthesized at 600 °C through a solid-state reaction. The synthesis was carried out in an autoclave by using CrCl₃, Mg and MgB₂ as the reactants. The X-ray powder diffraction pattern indicates the formation of orthorhombic CrB. Transmission electron microscopy image shows that typical CrB crystallites are composed of floss-like particles with less than 10 nm in diameter and about 50–100 nm in length. Thermogravimetric analysis revealed that the oxidation resistance for nanocrystalline CrB is much lower than that of bulk CrB.     

Preparation and characterization of zirconia and mixed zirconia/titania in ionic liquids

Zirconia and mixed zirconia/titania were synthesized in two different ionic liquids, namely, 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl) amide ([BMP]TFSA) and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide ([EMIm]TFSA) using sol–gel methods. The synthesized oxides were characterized by means of X-ray diffraction, scanning electron microscopy with energy dispersive X-ray (SEM-EDX)), thermogravimetric and differential thermal analyses (TGA–DTA). The results show that the as-synthesized ZrO₂ powders obtained either in [BMP]TFSA or in [EMIm]TFSA show amorphous behaviour, and calcination at 500 °C yields t-ZrO₂ which is subject to further phase transformation to m-ZrO₂ at 1000 °C. The type of the ionic liquid influences the morphology of the synthesized zirconia as the sample obtained from [BMP]TFSA showed a porous morphology with very fine particles in the nanometer regime, whereas micro-rods were obtained from [EMIm]TFSA. ZrO₂-TiO₂ nanorods with an average diameter of about 100 nm were synthesized in [EMIm]TFSA. The presence of zirconia in the mixed oxides stabilizes the anatase phase and elevates the temperature at which the phase transformation to rutile occurs.     

Preparation of nanosized yttria-stabilized zirconia powders and their characterization

Yttria-stabilized zirconia (YSZ) powders have been prepared by basic hydrolysis of a solution containing zirconium isopropoxide and yttrium nitrate. Crystallization of cubic YSZ occurs near 450 °C yielding ceramic powders with high specific areas, the values of which are dependent on the ammonia and water contents of the hydrolysis solution. Sintering at 1420 °C yields ceramics with nearly theoretical density and homogeneous grain size distribution.     

用于制备优质单壁碳纳米管管束的MgO负载Fe3O4纳米粒子的合成

采用沉淀方法制备了直径分布狭窄的均匀Fe3O4纳米颗粒.Fe3O4纳粒形体几近一致,平均粒径为10.33 nm±2.99 nm(平均粒径±标准偏差).在超声作用下将MgO纳米颗粒分散在一定量Fe3O4纳米颗粒的水溶液中获得MgO负载Fe3O4的纳米颗粒.以甲烷为碳源,Fe3O4/MgO为催化剂,经化学气相沉积,在Fe3O4纳粒上制得了大量直径近乎均匀的单壁碳纳米管(SWCNTs)束.TEM显示:SWCNTs的平均直径1.22rm.热重分析显示:样品在400℃～600℃温度区间失重量约19％.拉曼光谱显示:SWCNTs的ID/IG的强度比为0.03,表明采用Fe3O4/MgO催化剂可制得高石墨化程度的单壁碳纳米管.     

交联PS微球负载纳米Ni颗粒的制备及表征

采用种子聚合法制备出交联聚苯乙烯(PS)微球,经预处理在微球表面引入官能团,采用化学镀法在微球表面负载纳米级Ni颗粒,利用FI-IR、SEM、XRD等测试手段对其进行表征,结果表明:PS微球粒径均匀,平均粒径约为4.3μm,表面光滑;微球负载的纳米Ni颗粒分散性良好、平均晶粒度为9.41nm.利用负载微球对高氯酸铵(AP)进行催化实验,表明负载微球可使AP高温分解峰降低94.2℃左右.研究表明:采用PS微球负载可提高纳米Ni颗粒的分散性,进而提高了Ni颗粒的催化性能.     

TiO_2/HZSM-5的制备及光催化性能的表征

以钛酸四丁酯为钛源,采用溶胶-凝胶法在HZSM-5分子筛表面合成TiO2前驱体,程序升温处理制得TiO2/HZSM-5负载型光催化剂。采用X射线衍射、扫描电镜、傅里叶变换红外光谱、X射线光电子能谱对光催化剂晶相结构、表面形貌及化学组成进行了表征。结果表明,HZSM-5可提高TiO2分散性能,降低TiO2晶粒的尺寸。TiO2/HZSM-5中的Ti都以TiO2形式存在,没有Ti—O—Si键生成。甲基橙溶液的光催化降解结果表明,负载后提高了TiO2对甲基橙溶液的光催化降解活性。TiO2的质量分数为30%,400℃下煅烧2h时的催化剂光催化性能最好。     

Preparation and characterization of sol-gel derived yttria doped zirconia coatings on AISI 316L

A stable 4 mol% yttria-stabilized zirconia (YSZ) sol has been synthesized for coating stainless steel AISI 316L for biomedical applications. The sol was prepared by controlled hydrolysis of zirconium n-butoxide using acetylacetone and nitric acid as chelating agent and catalyst, respectively. X-ray diffractograms of calcined YSZ xerogel indicated a tetragonal structure at temperature as low as 400 °C. Stainless steel was dip-coated in transparent yellow YSZ sol followed by heat treatment between 400 and 600 °C for 2 h in air. A homogeneous and crack-free YSZ film was, thus, obtained on the stainless steel surface. Adhesion strength, measured by scratch test in progressive loading sequence on coated AISI 316L, showed 27 ± 3 N critical load. Corrosion performance of the surface coating was evaluated through open-circuit potential (OCP) measurement, impedance, polarization and chronoamperometry in Ringer's solution at 37 °C. The coating enhanced the pitting potential of the substrate. The metal ions released from AISI 316L was effectively controlled by the coating.     

Preparation and characterization of nanocrystallite size cuprous oxide

Uniform spheres of nanocrystallite size cuprous oxide particles have been prepared by a simple polyol process using cupric nitrate as a precursor in ethylene glycol. As synthesized compound was dried at 333 K in a vacuum oven and characterized by XRD, FT-IR and SEM techniques. The crystallite size of the cuprous oxide calculated from Scherer's formula was found to be ∼11 nm.     

Preparation and characterization of single-crystalline gallium oxide nanobelts

Single-crystalline β-Ga₂O₃ nanobelts were synthesized by a simple physical evaporation method in argon atmosphere with the starting materials of Ga. The β-Ga₂O₃ nanobelts have a width of 50-100 nm and width-to-thickness ratios of 5-10, and length of up to a few millimeters, which may have potential applications in nanosize sensors or optoelectronic nanodevices.     

国内外纳米ZnO研究和制备概况

概述了纳米ZnO的应用前景及国内外的研究现状,对纳米ZnO各种制备方法的基本原理、影响因素、产物粒径大小等进行了详细的分析讨论,同时提出了每种工艺的优缺点,并提出了研究方向。对其表征方法进行了介绍。     

硅藻土-莫来石陶瓷负载SiO2膜的制备与表征

将液晶模板技术与溶胶 -凝胶法相结合 ,制备了硅藻土 -莫来石陶瓷 (K -M )负载型SiO2 膜 .表征实验结果表明 :SiO2 膜层与TiO2 过渡膜层间通过Si—O—Ti键的价联方式形成了紧密、稳定的化合型复合膜 ;SiO2 膜孔径集中在 4～ 5nm ,孔分布较为均匀 ;K -M负载SiO2 膜管对气体具有较强的渗透能力 ,并有较好的气体分离作用 .根据实验结果探讨了模板剂的性质及用量对SiO2 膜孔结构的决定性作用 .     

Preparation and characterization of transition metal-modified lacunary Keggin 11-tungstophosphates supported on carbon

Transition metal-modified lacunary Keggin heteropolycompounds [PW₁₁O₃₉M]⁵⁻, with M = Ni²⁺, Co²⁺, Cu²⁺, or Zn²⁺, were synthesized and characterized. These heteropolycompounds were used to prepare the carbon-supported catalysts. Both the heteropolycompounds and the carbon-supported catalysts showed FT-IR spectra with the characteristic bands of these compounds and provided an indirect measure of the interaction strength between M and the oxygen of the central tetrahedron group of the Keggin structure. The anion decomposition of the modified compounds takes place at equal or lower temperature than that of the bulk and supported parent lacunary [PW₁₁O₃₉]⁷⁻ anion. The species present on the support surface may be highly dispersed as a non-crystalline form, as a result of the interaction with the support surface groups. The activity of the synthesized catalysts in isopropanol dehydration, reflecting their acidity, increases as the reduction temperature of the decomposition products of the heteropolycompounds decreases. It may be assumed that the generation of acid sites is a result of the interaction of hydrogen, donated by isopropanol during its decomposition, with the M cation, leading to M reduction and protons.     

负载型TiO2-聚丙烯疏水复合膜的制备与表征

采用热致相分离 (TIPS)技术制备浸涂型和反应型硅藻土 -聚丙烯疏水复合膜 ,用SEM、氮吸附、红外光谱和气体渗透性能测试装置等方法表征不同的制膜方法、浸膜液浓度及冷却方式等因素对膜形态、结构和气体渗透性能的影响 .结果表明 :浸涂型聚丙烯膜球形颗粒和孔径尺寸均小于反应型聚丙烯膜 ;TiO2 -聚丙烯膜与硅藻土陶瓷支承体是通过Si—O—Ti—O—C键的价联方式形成键联型复合膜层 ;在膜内 ,气体渗透由Knudsen扩散控制 ,H2 O与N2 的分离因子分别为 2 .4 6和 2 .2 2 .     

Electrochemical characterization of oxide formed on chromium containing mild steel alloys in LiOH medium

Flow accelerated corrosion leads to wall thinning of outlet-feeder pipes in the primary heat transport system of pressurized heavy water reactors and can even necessitate enmasse feeder replacement. Replacement of carbon steel 106-grade-B (CS) with chromium containing carbon steel reduces the risk of this failure. This paper discusses the role of small additions of chromium in modifying the properties of the oxide film. CS and chromium containing mild steels viz., A333, 2.25Cr–1Mo and modified 9Cr–1Mo alloy were exposed to primary heat transport (PHT) system chemistry conditions. The oxide films formed were characterized by electrochemical and surface characterization techniques. Mott–Schottky analysis showed donor type of defects. The densities of defects in the oxides of chromium containing alloys were 3–15 times less than that in CS. In presence of ∼200 ppb of dissolved oxygen, the oxides formed were hematite with two orders of magnitude smaller concentration of defects as compared to that formed under reducing conditions. These results suggest that the presence of chromium lowers the defect density of the oxide film and thus ensures a reduced corrosion rate.     

钒掺杂二氧化钛薄膜制备与材料特性分析

以钛酸四丁酯和乙酰丙酮钒（Ⅲ）为主要原料,采用溶胶-凝胶法制备了钒掺杂二氧化钛薄膜,利用XRD、紫外-可见吸收光谱、FT-IR及XPS等表征手段,将其与未掺杂二氧化钛薄膜进行了材料特性对比研究。结果表明两种薄膜均为锐钛矿结构,引入钒后二氧化钛的禁带宽度由3.28eV减小至3.15eV,吸收带边红移至可见光范围;XPS分析证实制备的钒掺杂二氧化钛薄膜中钒以四价和五价两种氧化价态存在,可能在二氧化钛禁带中引入较深的杂质能级而引起价带顶向禁带拓展,从而产生引起禁带宽度变窄效应,扩展了二氧化钛带边光吸收。理论分析还表明,钒掺杂引起的深能级杂质在二氧化钛晶界处易于形成有效的陷阱俘获光生空穴,从而抑制光生载流子的复合,尤其适于用作光催化材料。     

Preparation and characterization of thermosensitive PNIPAA-coated iron oxide nanoparticles

A new and facile approach was established to fabricate thermoresponsive poly(N-isopropylacrylamide) (PNIPAA) coated iron oxide nanoparticles in a non-aqueous medium. The morphology and structure of the nanoparticle-doped composite were analyzed by?means of transmission electron microscopy (TEM), x-ray powder diffraction (XRD), and Fourier transformation infrared spectrometry (FTIR). The thermosensitivity of the composite was also investigated. Results indicated that the oil-soluble iron oxide nanoparticles encapsulated with PNIPAA, composed of an inorganic iron oxide core and biocompatible PNIPAA shell, were dispersed well in water and had a sphere-like shape. The PNIPAA-coated iron oxide nanoparticles with such a kind of core-shell structure showed excellent thermosensitivity. Namely, the aqueous suspension of PNIPAA-coated iron oxide nanoparticles dramatically changed from transparent to opaque as the temperature increased from room temperature to 38?°C, showing potential as optical transmittance switch materials and their significance in the fields of protein adsorption and purification controlled release, and drug?delivery.     

TEM characterization of metal and metal oxide particles supported by multi-wall carbon nanotubes

Composites of Sn–Pd particles and multi-walled carbon nanotubes (MWNTs), and of Ni–Co particles and MWNTs were investigated by transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD). The Sn–Pd particle composites were prepared by impregnation deposition, and the Ni–Co particle composites were prepared by electroless deposition on MWNTs synthesized by a chemical vapor deposition method using thermal catalytic decomposition of hydrocarbon. The morphologies and the microstructure of the deposited particles were investigated upon annealing the composites with and without hydrogen. Both the crystalline particle structure and the particle morphology are observed to be different for the samples annealed with and without hydrogen.     

Tungstophosphoric acid supported onto hydrous zirconia: Physicochemical characterization and esterification of 1ℴ and 2ℴ alcohol

The Keggin type heteropolyacid, 12-tungstophosphoric acid (PW), was supported onto hydrous zirconia (Z) by impregnation method and designated as ZH₃. The ZH₃ was calcinated at 300°C and 500°C and designated as ZH₃₃ and ZH₃₅, respectively. The resulting materials were characterized by FTIR, diffuse reflectance spectroscopy (DRS), XRD, surface area measurement (BET method) and particle size distribution. The surface morphology was studied by scanning electron microscopy. The acidity of all materials was evaluated by carrying out chemisorption of ammonia and esterification of 1ℴ alcohol (n-butanol) with different acids like formic acid, acetic acid and propionic acid and 2ℴ alcohol (cyclohexanol, iso-butanol) with acetic acid. Above studies show the high dispersion of HPA in a non-crystalline form on the support as well as uniform distribution of particles of ZH₃ which contains 30% 12-tungstophosphoric acid. It also shows that when ZH₃ was calcinated at 500°C, it possesses highest acidity for both chemisorption of NH₃ as well as esterification reactions.