氧化钐包覆铁纳米复合粒子的合成及微波响应特性

以Fe和Sm2O3的微米粉体为原料，压制成块体靶材，在H2＋Ar混合气氛下蒸发，原位合成了Sm2O3包覆Fe纳米复合粒子，对其成分、结构和微波频段的电磁响应特性进行了分析。结果表明，Fe／Sm2O3复合纳米粒子具有清晰的“核／壳”结构，并通过“定量氧辅助-气-液-固”机制对其形成过程进行了探讨。电磁性能分析结果显示，由介电性稀土氧化物和铁磁性‘金属构成的“核／壳”纳米结构具有微波吸收特性，其损耗机制主要以介电型损耗为主。本文采用的物理气相方法有利于多组元的纳米结构复合，实现了稀土氧化物包覆异质金属纳米胶囊合成，为金属／稀土氧化物纳米复合材料的合成与应用提供，了试验依据。     

制备纳米铁酸锌的一种新方法

利用滚压振动磨在干法室温条件下和化学共沉淀法分别制备了纳米锌和纳米Fe3O4颗粒,再通过锌和Fe3O4水解反应制备纳米ZnFe2O4颗粒;用XRD、TEM以及Mssbauer谱仪等对其进行了表征。结果表明:制得的纳米锌、纳米Fe3O4和纳米ZnFe2O4的颗粒平均粒径分别为40,20,40 nm;当水解反应温度为300℃时,ZnFe2O4颗粒尺寸比较均匀,但明显出现Fe2O3;由Mssbauer谱可知出现了三个六条亚谱。     

油胺修饰镍纳米粒子在锂基脂中的摩擦学性能*

为提高镍纳米粒子作为润滑脂添加剂的减摩和抗磨能力,采用油胺对其进行修饰以减少团聚,通过SEM、FT-IR和XRD对OA-Ni的微观形态和结构进行了表征,利用四球摩擦试验机和TE77往复摩擦试验机考察表面修饰的镍纳米粒子(OA-Ni)对锂基润滑脂摩擦学性能的影响,并探讨其在润滑脂中的减摩抗磨机制。结果表明:制备的油胺修饰镍纳米粒子呈不规则的圆片状,粒径约为100 nm,在润滑脂中有良好的分散性;经油胺表面改性的镍纳米粒子能有效改善锂基脂的摩擦学性能,抗磨和减摩性能分别提升了36.6%和15%。磨损表面分析结果表明,在摩擦过程中油胺修饰的镍纳米粒子在摩擦表面形成了主要成分为Fe2O3、 Fe3O4、NiO、Ni2O3等金属氧化物的摩擦化学膜,提高了锂基脂的摩擦学性能。     

Fe_3O_4/MnO_2磁性复合颗粒的制备及表征

以纳米Fe3O4颗粒为核,分别采用液相沉积法和溶胶一凝胶法两种方法将MnO2包覆在其上制备了Fe3O4/MnO2磁性复合颗粒,并借助XRD、TEM、FTIR和VSM等手段分别对纳米Fe3O4颗粒和两种复合颗粒进行表征.结果表明:采用液相沉积法进行包覆可生成以多个纳米Fe3O4颗粒为核、粒径约为200 nm的近球形Fe3O4/MnO2磁性复合颗粒,其饱和磁化强度为24.4 kA·m-1;采用溶胶-凝胶法进行包覆则生成以单个纳米Fe3O4颗粒为核、粒径约为50 nm的磁性复合颗粒,包覆层为絮状MnO2,其饱和磁化强度为16.5 kA·m-1.     

硅油基纳米Fe_3O_4磁性液体的制备

采用化学共沉淀法,成功制备了纳米Fe3O4微粒,主要研究了Fe2+与Fe3+不同物质的量比对Fe3O4微粒、粒径及磁化强度的影响,采用不同表面活性剂制备了硅油基纳米Fe3O4磁性液体。结果表明:Fe2+与Fe3+物质的量比对Fe3O4微粒性能影响显著,对微粒尺寸影响不大,均为纳米级,当Fe2+与Fe3+物质的量比为0.6时,其饱和磁化强度达到最大,为52.1 A.m2.kg-1;在无水乙醇中,聚乙烯吡咯烷酮(PVP)的分散效果虽优于油酸,但与硅油相溶性差、增粘作用明显的缺点限制了PVP的使用;而油酸由于亲油性好,更适合作为制备硅油基Fe3O4磁性液体的表面活性剂。     

高速电弧喷涂FeAlCrNi-Cr3C2涂层的组织与相结构研究

采用粉芯丝材高速电弧喷涂技术制备了FeAlCrNi-Cr3C2涂层,并研究了涂层的组织和相结构.结果表明涂层具有致密的层状结构,扁平颗粒小,氧化物膜细小,硬质点相分布均匀,孔隙率低;在涂层中存在着多种结构复杂的组织和化合物相,包括单立方结构基体相FeAl、Fe3Al、AlNi,AlNi;硬质相Cr3C2、Fe3C及AlFe3C0.5;氧化物相FeO·Al2O3、Cr2O3、少量六方结构的α-Al2O3和面心立方结构的γ-Al2O3以及面心立方结构的FeO·Cr2O3;某些区域还存在面心立方结构的γ-(Fe,Ni).     

热挤压润滑油用纳米润滑添加剂润滑性能的研究

采用化学沉淀法分别制备了经表面修饰的纳米Fe3O4和纳米CuO粒子,在透射电镜下研究了纳米粒子的粒径大小、形貌及其分散性;在四球摩擦试验机上,研究了纳米Fe3O4和纳米CuO粒子对润滑油承载能力的影响,同时在CSS-2220型万能试验机上,对比研究了添加纳米Fe3O4和纳米CuO粒子的润滑油在LY12热挤压成形过程中的润滑性能.试验结果表明:所制备的纳米Fe3O4和纳米CuO粒子均呈球形、平均粒径分别为10和20 nm,在润滑油中均具有良好的分散性;纳米Fe3O4和纳米CuO粒子均可以提高润滑油的最大无卡咬载荷,其中纳米Fe3O4粒子的性能优于纳米CuO粒子;添加纳米Fe3O4和纳米CuO粒子的润滑油均可降低挤压变形功,挤压件表面SEM形貌结果表明,纳米粒子的存在有效地隔离了挤压件与模具表面的直接接触,减少了挤压件表面犁沟数量,降低了热挤压变形功.     

纳米Fe3O4磁流体的制备及其影响因素研究

通过液相共沉淀法制备了Fe3O4水基磁流体,选择油酸作为表面活性剂,获得油酸包覆的Fe3O4纳米粉,将其分散于有机溶剂中,制备了纳米Fe3O4有机基磁流体。采用X-Ray衍射分析仪和粒径分布仪分析了生成物的结构和粒径分布;用FT-IR和高分辨透射电镜表征了生成物的成分和形貌。结果表明:制得的立方晶体纳米Fe3O4平均粒径为16.3 nm,FT-IR图谱中1 593、1 736和2 926 cm-1等处的吸收峰很强烈,这充分说明该纳米粒子被油酸很好地包覆;选择油酸作为表面活性剂,起到表面改性和萃取出纳米粒子的作用;制得的油酸包覆纳米Fe3O4粒子能够稳定分散于有机溶剂中。     

高速电弧喷涂FeAlCrNi-Cr3C2涂层的组织与相结构研究

采用粉芯丝材高速电弧喷涂技术制备了FeAlCrNi-Cr3C2涂层,并研究了涂层的组织和相结构.结果表明:涂层具有致密的层状结构,扁平颗粒小,氧化物膜细小,硬质点相分布均匀,孔隙率低;在涂层中存在着多种结构复杂的组织和化合物相,包括单立方结构基体相FeAl、Fe3Al、AlNi,AlNi;硬质相Cr3C2、Fe3C及AlFe3C0.5;氧化物相FeO·Al2O3、Cr2O3、少量六方结构的α-Al2O3和面心立方结构的γ-Al2O3以及面心立方结构的FeO·Cr2O3;某些区域还存在面心立方结构的γ-(Fe,Ni).     

室温气敏型Fe2O3纳米膜的制备及表征

针对传统Fe2O3气敏元件工作温度高、响应时间长等缺点,采用分析纯FeCl3·6H2O和乙醇为主要原料,以AI2O3陶瓷片为基底,利用溶胶凝胶法制备了Fe2O3纳米膜及气敏元件.利用XRD(X射线衍射)、AFM(原子力显微镜)对纳米膜的结构及形貌进行了表征,结合Fe2O3纳米膜的形成机理,主要讨论了镀膜次数对薄膜结构、性能的影响;研究了薄膜元件的阻温特性及室温气敏性能.结果表明:镀膜20次后,Fe2O3颗粒粒径约为20～30 mn,镀膜30次后,纳米膜平整、均匀、无裂纹;室温下薄膜元件便对H2CH4有一定的气敏效应,响应时间小于3s,灵敏度随气体浓度变化呈线性关系.     

Electron energy-loss near-edge structures of 3d transition metal oxides recorded at high-energy resolution

Near-edge fine structures of the metal L(2,3) and O K-edges in transition metal-oxides have been studied with a transmission electron microscope equipped with a monochromator and a high-resolution imaging filter. This system enables the recording of EELS spectra with an energy resolution of 0.1eV thus providing new near-edge fine structure details which could not be observed previously by EELS in conventional TEM instruments. EELS-spectra from well-defined oxides like titanium oxide (TiO(2)), vanadium oxide (V(2)O(5)), chromium oxide (Cr(2)O(3)), iron oxide (Fe(2)O(3)), cobalt oxide (CoO) and nickel oxide (NiO) have been measured with the new system. These spectra are compared with EELS data obtained from a conventional microscope and the main spectral features are interpreted. Additionally, the use of monochromised TEMs is discussed in view of the natural line widths of K and L(2,3) edges.     

尼龙66粉末与纳米Fe3O4粒子作润滑油添加剂的摩擦学匹配性研究

利用化学共沉淀法制备了油酸修饰的粒径大小为8nm左右的Fe3O4纳米粒子，并将其与尼龙66粉末混合作润滑油添加剂进行摩擦学试验。试验结果表明在添加纳米Fe3O4粒子的润滑油中再添加适量的尼龙66粉未，润滑油的摩擦学性能得到改善，在保持润滑油润滑性能不变的情况下，磨损量明显降低。可见，纳米Fe3O4粒子与尼龙66粉末表现出了良好的摩擦学协同性能。     

基于SnO2-CuO掺杂的CO2气体敏感特性研究

以氧化物半导体SnO2为基体材料加入40％的活性CuO材料,制备出了对CO2具有敏感性的气体敏感材料,其检测浓度范围为0 ～5％.实验结果表明,在SnO2 - CuO敏感材料的基础上掺杂适量CeO2、Ag2O、Bi2O3等氧化物,不仅提高了其对CO2气体的灵敏度,而且可以提高其稳定性,从而改善了其对CO2的敏感特性.在试验结果的基础上,分析并讨论了该系列材料对CO2气体的敏感机制.基于这种敏感材料的CO2气体传感器具有结构简单、容易制备、使用方便和价格低廉等优点.     

常温甲烷气敏元件的研制

采用掺有Pd活性SnO_2-InO_3-TiO_2敏感材料,再掺入MgO等金属氢化物,制成复合基体材料,采用直热式气敏元件制造工艺,经表面修饰改性,研制成功常温CH_4气敏元件,给出了常温下的气敏特性,并探讨其机理。     

High temperature faraday balance for in situ measurement of magnetization in transition metal oxides

We report the design of a Faraday balance that can be used to measure the magnetization of transition metal oxides at high temperatures and under controlled atmosphere. The instrument is sufficiently sensitive and stable to quantify the magnetic force on diamagnetic and paramagnetic samples at temperatures up to 1000 degrees C and in oxygen partial pressures as low as 100 ppm. We demonstrate the performance of the instrument by presenting preliminary magnetic measurements of lanthanum strontium cobalt oxide (La1-xSr(x)CoO3-delta) and aluminum oxide (Al2O3).     

INFLUENCE OF RARE EARTH DOPING ON MECHANICAL PROPERTY AND MICRO-STRUCTURE OF CHROMIA OXIDE FILM

The isothermal oxidizing kinetics of Co-40Cr alloy and its yttrium ion-implanted samples are studied at 1 000 ℃ in air by thermal-gravity analysis （TGA）. Scanning electronic microscopy （SEM） is used to examine the Cr2O3 oxide film＇s morphology after oxidation. Acoustic emission （AE） method is used in situ for monitoring the cracking and spalling of oxide films formed on both samples during oxidizing and subsequent air-cooling stages. Theoretical model is proposed relating to the film fracture process and is used for analyzing the acoustic emission spectrum both on time domain and on AE-event number domain. It is found that yttrium implantation remarkably reduces the isothermal oxidizing rate of Co-40Cr and improves the anti-cracking and anti-spalling properties of Cr2O3 oxide film. The reasons for the improvement are mainly that the implanted yttrium reduced the grain size of Cr2O3 oxide, increased the high temperature plasticity of oxide film, and remarkably reduced the number and size of Cr2O3/Co-40Cr inteffacial defects.     

TEM study of the structural dependence of the epitaxial passive oxide films on crystal facets in polyhedral nanoparticles of chromium

Nanocubes and partially truncated rhombic dodecahedral nanoparticles of Cr have been studied by electron diffraction, high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy. It is found that the nanoparticles of Cr are enclosed by the epitaxial passive oxide films. The oxide films on 100% truncated nanocubes of Cr with only one kind of facets, (100) facets, are face-centered cubic (fcc) structured Cr(2)O(3) with a lattice constant of 0.407nm. There are two kinds of oxide films in partially truncated nanoparticles of Cr with two kinds of crystallographic facets, (100) and (110). The same fcc Cr(2)O(3) is found on the (100) facets while the rhombohedral [Formula: see text] -Cr(2)O(3) is found on the (110) facets. This is similar to the two kinds of oxides, fcc and rhombohedral Fe(2)O(3), which have also been observed in polyhedral nanoparticles of Fe. These passive Cr(2)O(3), found in nanoparticles of Cr which have remained unchanged in water for four years, may have important implications for protective oxide films involving Cr.     

Nanotribology of Si oxide layers on Si by atomic force microscopy

Atomic force microscopy (AFM) has been used for tribological studies of Si surfaces covered by oxide layers of various kinds: chemical oxides prepared by the SC1 (NH4OH/H2O2/H2O) and the SC2 (HCl/H2O2/H2O) treatments and a thermal oxide. In the case of the SC1 chemical oxide, the oxide layer was scratched and the underlying Si substrate was ploughed by the Si3N4 AFM tip. On the other hand, no wear of the sample was noted on the other surfaces: the AFM often produced elevated patterns in the shape of the scanned area, which were no longer visible after HF etching. By annealing the SC1-treated surface in N2 gas at above 200 degrees C for 30 min, the oxide layer could not be scratched any more. By soaking the thermal oxide in KOH, the oxide layer was then scratched. It is concluded that the presence of OH bases is the necessary condition for the nano-scratching of the oxide layers.     

金属氧化物在润滑脂中的极压抗磨性能研究

采用四球机考察了氧化铋、氧化铜、氧化铅以及二氧化锡等金属氧化物在锂基润滑脂中的极压抗磨性能.结果表明,4种金属氧化物对润滑脂的抗磨性能有着不同的影响,氧化铜、氧化铅有利于提高润滑脂的抗磨性能,尤其2% CuO具有良好的抗磨性能,氧化铋和二氧化锡对润滑脂的抗磨性能没有明显改善;4种氧化物在润滑脂中都有良好的极压性能,其中氧化铋和氧化铅表现得更加突出.因此,4种氧化物作为固体润滑剂,能够改善润滑脂的摩擦学性能.