机械活化-湿化学合成LiMn2O4的组成、结构与表征

以MnO2和LiOH·H2O为原料,采用机械活化与湿化学集成的方法,在水溶液中直接合成了结晶态的尖晶石锂锰氧化物.当锂含量介于3.78%～4.35%之间时,所得锂锰氧化物为纳米级球形粉末,以尖晶石结构为主,含极少量的Mn3O4杂相;在300～800℃温度范围内热处理后,Mn3O4杂相消失,尖晶石结构更趋完善.所合成的含锂5.80%的高锂样品则以LiMnO2层状结构为主,含少量Mn3O4杂相,其SEM形貌为片状;在300～700℃下热处理8 h后,层状LiMnO2转变成尖晶石LiMn2O4,Mn3O4杂相峰明显减弱并随热处理温度的升高而消失;当温度升高至700～800℃时,开始出现缺锂的Li1-xMn2O4相.结果表明:该法制备锂锰氧化物可实现锂、锰、氧在原子级水平的均匀混合,所得产物的热稳定性能良好,其化学计量组成与结构易于调整和控制.     

Use of electron microscopy on microstructure characterization of high chromium cast irons

The physical metallurgy underlying the development of cast microstructures in abrasion resistant high chromium cast irons, and their structural modification by thermal treatments is relatively complex. Structural characterisation via electron microscopy therefore has a key role to play in furthering our understanding of the phase transformations that control the microstructures and hence the service performances of these irons as wear parts. This paper shows how both scanning and especially transmission electron microscopy can provide valuable information on the nature of eutectic and secondary carbides and on the matrix structures in these irons. Particular attention is given to current characterisation research on conventionally cast 30%Cr irons that are used for applications involving corrosive wear e.g. slurry pumps and on a semi-solid cast 27%Cr iron that has a potential for applications in industry.     

玻璃包覆纯铜微丝的制备与表征

采用熔融纺丝法制备了玻璃包覆纯铜微丝,对微丝进行了组织观察以及尺寸和缺陷表征,提出了不同冷却条件下的纯铜芯丝凝固过程模型,讨论了制备过程中存在的问题并提出了相应的解决方案.结果表明:在空气中自然冷却凝固的纯铜芯丝内部组织为细等轴晶,加冷却水快速冷却凝固制备的纯铜芯丝内部的晶粒沿着微丝长度方向呈竹节状整齐排列;当微丝外径为45μm、芯丝直径为25 μm时,外径尺寸波动在6%以内,芯丝直径误差小于4%;当原料质量存在问题或制备过程中拉丝速度、冷却速度等工艺参数匹配不合理时,易导致芯丝表面存在凹坑和凹槽等缺陷.     

Preparation and properties of nanosize MnZn ferrite from δ-FeOOH

Ferrous ion was transformed into feroxyhyte (δ-FeOOH) by oxidation. Then, manganese sulfate and zinc sulfate in some ratio were added to the feroxyhyte solution. The co-precipitation was boiling reflux conditions sometime under constant stirring. The nanosize MnZn ferrite powder was formed. The mechanism of preparation of the nanosize MnZn ferrite was discussed, and the formation of feroxyhyte which was playing a key role during the process was mentioned. The properties of powder was tested by means of X-ray diffraction, transmission electron microscopy and vibrating sample magnetometer. The results show that the samples of spherical particles about 20 nm, which have characteristics of ferrimagnetism, has larger saturation magnetization, but the remanent magnetization and coercivity are comparatively smaller. The spinel MnZn ferrite nanosize powder was successfully prepared from δ-FeOOH at low temperature, with low-carbon steel and peroxide as main material.     

尖晶石纳米催化剂应用于烯丙醇多相氧化制烯丙醛或烯丙酮

使用共沉淀法通过Ru对MeFe2O4的同晶取供制备了纳米级MnFe1.95Ru0.05O4催化剂。在通过过渡金属进一步改性该催化剂的过程中，发现MnFe1.95Ru0.05O4的催化剂性能优异于文献报道的其他多相醇氧化催化剂，XRD测试表明该催化剂仍保持尖晶石结构。该纳米催化剂能有效地将不同烯丙醇类氧化成烯丙醛类或烯丙酮类，与文献报道的其他多相氧化催化体系相比，该催化剂具有更高的活性转换数。借助于EXAFS等表征结果和1－辛醇与4－辛醇的竞争反应，判断出单核的Ru类反应的活性中心，EXAFS的表征同时表明由于Cu的添加而产生的Ru=0能加快反应速率。作者在此基础上提出反应机理，认为Ru在反应过程中形成醇化物，再经过β消除反应生成相应的醛或酮。     

纳米CaCO3的表面改性研究

本文研究了纳米CaCO3表面改性的影响因素，确定了最优改性剂和改性条件，并运用沉降实验、透射电镜（TEM）等表征手段对粉体的改性效果进行了分析。结果表明：以月桂酸钠为改性剂，用量为10％，pH值为7，改性时间为1h时，改性后的纳米CaCO3的亲油化度达到85．1％，能较好地分散于环己烷和二甲苯中。     

Lead recovery from aqueous environment by using porous carbon of citrus fruits waste: equilibrium,kinetics and thermodynamic studies

ABSTRACT

The mixture of citrus fruits (orange, grapefruit, mandarin, and lemon) wastes was utilized to obtain high surface area activated carbon (AC) by H₃PO₄ activation. The production conditions were optimized and the optimum conditions were determined. The optimal-activated carbon (CFWAC) was characterized by various physicochemical techniques. CFWAC was also used as a sorbent for Pb (II) ions from water. Batch experiments were performed to explore the adsorption capacity and mechanism. The Langmuir isotherm and pseudo-second-order kinetic model showed good fitness to the experimental data. The maximum Pb (II) adsorption capacity of CFWAC was found to be 163.93 mg/g.     

配合物Zn(Him)2(OAc)2的室温固相合成及表征

乙酸锌与咪唑 (Him)通过室温固相反应一步合成配合物Zn(Him) 2 (OAc) 2 ,反应不需溶剂 ,2 0min即可完成 ,产率达 96% ,并用元素分析、红外光谱、热重分析、X -射线粉末衍射和X -射线单晶衍射对产物进行了表征。     

二氨基乙腈及三胺的合成及表征

利用加成反应合成了两种新化合物二 ( 2 -腈基乙基 )氨基乙腈及三 ( 2 -腈基乙基 )胺 ,用红外光谱、1 H -NMR核磁共振谱、元素分析、ES -MS质谱及热重分析对其结构和热性质进行了表征。结果证实所制备的两种化合物即为目标化合物 ,这两种化合物热性质相似 ,在 30 0℃以下具有较好的热稳定性。     

纳米层状双金属氢氧化物的制备及结构表征

采用恒定pH 12±0.2,按n(Mg2+)∶n(Al3+)∶n(OH-)∶n(CO2-3)=6∶2∶16∶1配制溶液,采用一步反应液相法,制备纳米层状双金属氢氧化物(LDH)粉体.为了获得无团聚、分散均匀的纳米粉体,探讨了溶剂置换干燥、真空干燥、常压干燥对纳米LDH粉体形成团聚的影响;用X射线衍射仪、透射电镜、红外光谱仪和元素分析仪对样品的物相、形貌、粒径和组成进行了表征.结果表明,溶剂置换干燥能够有效防止纳米粉体形成硬团聚,样品分散性好,呈针状形态,长50 nm,宽5 nm.