纳米Cu-Ni复合氧化物的制备及表征

通过溶胶-凝胶法制备了纳米Cu-Ni复合氧化物,利用DTA、XRD、TEM等方法对样品结构和性质进行了表征,研究了前驱体焙烧温度、原料浓度、搅拌速度和表面活性剂对粉体晶形和粒度的影响.结果表明,焙烧温度为350℃时能制得CuO-NiO复合物,其尺度为纳米结构;原料液浓度越低,搅拌速度越小,纳米粉体越易团聚;聚乙二醇表面活性剂对纳米粉体有良好的分散作用,颗粒较均匀.     

Solid-State Properties of Fullerenes and Their Compounds

In this article, we present a resume of experimental activities performed at the Research Center Karlsruhe in the field of fullerene solid-state physics. Central issues are the rotational order-disorder phase transitions in pure fullerene crystals and the electronic properties of undoped and doped fullerenes. The major part deals with C₆₀ but selected results for solid C70 and C₈₄ are also given. The experimental methods comprise X-ray diffraction, inelastic neutron scattering, dilatometry, magnetometry and photo-electron spectroscopy.     

Solid-State Properties of Fullerenes and Their Compounds

Abstract

In this article, we present a resume of experimental activities performed at the Research Center Karlsruhe in the field of fullerene solid-state physics. Central issues are the rotational order-disorder phase transitions in pure fullerene crystals and the electronic properties of undoped and doped fullerenes. The major part deals with C₆₀ but selected results for solid C70 and C₈₄ are also given. The experimental methods comprise X-ray diffraction, inelastic neutron scattering, dilatometry, magnetometry and photo-electron spectroscopy.     

Ceramic Membranes for Filtration Applications — Preparation and Characterization

This article gives an overview about the preparation and characterization of asymmetric ceramic membranes that have been developed at our institute within the last years. Depending on the required pore size of the filter active layer for filtration applications ranging from microfiltration (MF) up to nanofiltration (NF) different preparation routes have to be applied.     

洋葱状富勒烯的制备与提纯

采用CVD法制备了洋葱状富勒烯(OLFs),研究了不同工艺条件对OLFs形成的影响,并通过硝酸回流法对得到的粗产品进行了提纯处理.研究结果表明,在相同的反应体系中,采用乙炔作碳源,氩气和氢气的混合气体作载气,制得的OLFs的纯度较高;硝酸处理可有效去除粗产品中碳纳米管、无定形炭和金属催化剂颗粒等杂质,使得OLFs的整体纯度得到提高.     

Synthesis and Spectral Characterization of Difunctional Fullerenes

The oxidation of C₆₀ with m-chloroperbenzoic acid gave C₆₀O₂ with a high positional selectivity, as the ¹³C NMR analysis suggested. Diadducts C₆₀CCI₂O, C₆₀CCl₂(anthracene), C₆₀CCl₂[(CH₂CH₂)₂N₂], and C₆₀CCI₂[Pt-(PPh₃)₂] were synthesized, isolated, and characterized by negative ion FAB mass spectroscopy.     

洋葱状富勒烯的制备及摩擦性能研究

通过水下电弧放电法制备出洋葱状富勒烯(OLFs).采用高分辨透射电镜(HRTEM)、X射线衍射(XRD)分析了OLFs的晶体结构和形貌,并通过热重(TGA)考察了OLFs的热稳定性.在MRS-10A型四球摩擦试验机上测试了OLFs作为长城牌SE级15W-40汽油机油添加剂的摩擦性能.结果表明,所制备的OLFs具有较高的石墨化程度,直径约25nm,外形呈球状并具有一定的空心结构;在空气中的热稳定性维持到600℃以上.在不同的质量分数和载荷下,OLFs作为润滑油添加剂在减摩性能上均优于碳纳米管(CNTs).     

高支化含无机粒子的巯基硅氧烷溶胶的制备及结构表征

用溶胶-凝胶法制备了一种新型的多功能巯基硅氧烷溶胶,其结构用1H-NM R,FT-IR和M S进行了表征,巯基硅氧烷溶胶的无机粒子粒径大小与分布用小角度光散射仪(SALS)进行了测定。这种新型巯基硅氧烷溶胶能够提高改性亚麻籽油体系自由基聚合速率。     

类水滑石的合成、表征及应用进展

较全面地综述了近年来类水滑石(HTlc)的最新研究进展,总结了类水滑石的多种合成方法,结合XRD、FT-IR、TG-DTA三种典型表征对HTlc的结构和性能进行进一步阐述,并重点归纳了HTlc在催化、吸附、环保及新型材料等多方面的应用概况,同时也展望了其未来发展趋势。     

PANI/CB[6]包合物的合成与表征

从合成甘脲、葫芦脲(CB[6])出发,进一步采用氧化聚合方法,在盐酸苯胺-CB[6]溶液中合成聚苯胺(PANI)与CB[6]的包合物PANI/CB[6]。通过红外光谱、紫外可见光谱和核磁共振(1H-NMR)对包合物进行了表征,结果表明,CB[6]包合在PANI链结构中的醌式结构部位。包合物的荧光光谱存在4个荧光峰,并且随着包合物浓度减小,吸收峰强度增强;包合物的热重分析(TG-DTA)曲线显示了失水、失去HCl分子、短链PANI分解和CB[6]与长链PANI共同分解的4步失重过程。     

Trifluoromethylated [60]Fullerenes: Synthesis and Characterization

Abstract

The high temperature reaction of C₆₀ with silver(I) trifluoroacetate followed by 500°C sublimation and HPLC purification has led to the characterization of the trifluoromethyl‐[60]fullerenes 1,4‐C₆₀(CF₃)₂, C _s‐C₆₀(CF₃)₄, C ₁‐C₆₀(CF₃)₄, and C ₁‐C₆₀(CF₃)₆ by EI‐MS and ¹⁹F NMR. The compounds C ₁‐C₆₀(CF₃)₄ and C ₁‐C₆₀(CF₃)₆ were obtained with 90+% compositional purity. A sample of C₆₀(CF₃)₂ also contained ca. 15–20% of a C _s‐symmetry isomer of C₆₀(CF₃)₄. The structural assignments are based on calculations at the AM1 and DFT levels of theory.     

煤基纳米洋葱状富勒烯制备及其结构表征

在射频等离子体条件下以煤为原料制备纳米洋葱状富勒烯(Nano-structured Onion—like Fullerenes:NSOFs).高分辨透射电镜(HRTEM)和X射线衍射(XRD)表征结果表明:以煤为原料可大量制备NSOFs,纯度较高,无碳纳米管伴随生成,外观呈准球状或多面体状,内中空,直径分布较均匀,石墨化程度很高,为低成本合成纯净的NSOFs提供了一条新途径.     

Hybrid Organic–Inorganic Materials—In Search of Synergic Activity

This review surveys the work developed in the field of functional hybrid materials, especially those containing conducting organic polymers (COPs), in combination with a variety of inorganic species, from molecular to extended phases, including clusters and nano‐sized inorganic particles. Depending on the dominating structural matrix, we distinguish and analyze organic–inorganic (OI) hybrids, nanocomposite materials, and inorganic–organic (IO) phases. These materials have been used in a wide variety of applications, including energy‐storage applications, electrocatalysis, the harnessing of electrochromic and photoelectrochromic properties, application in display devices, photovoltaics, and novel energy‐conversion systems, proton‐pump electrodes, sensors, or chemiresistive detectors, which work as artificial “noses”.     

Reaction of Fullerenes with Radicals Generated by Thermal Decomposition of Azo Compounds

Radicals generated thermally from azo compounds having cyano or ester function were added to C₆₀ to give poly-functionalized C₆₀ derivatives. Interestingly, their reactivities toward C₆₀ were found to be higher than those toward C₇₀.     

无机层状化合物的剥离技术及应用研究

从无机层状化合物构造出发,描述了不同电性无机层状化合物的结构和剥离方法.在此基础上着重介绍了层状锰氧化物的剥离过程,并利用剥离/重组技术成功合成了一系列纳米级锰氧化物功能材料,所合成的纳米级锰氧化物功能材料期待在选择性吸附剂、选择性催化剂及锂离子二次电池正极材料等方面得到广泛应用.     

Characterization and Liquid Chromatography-MS/MS Based Quantification of Hydroxylated Fullerenes

Highly water-soluble hydroxylated fullerene derivatives are being investigated for a wide range of commercial products as well as for potential cytotoxicity. However, no analytical methods are currently available for their quantification at sub-ppm concentrations in environmental matrixes. Here, we report on the development and comparison of liquid chromatography-ultraviolet/visible spectroscopy (LC-UV/vis) and liquid chromatography-mass spectrometry (LC-MS) based detection and quantification methods for commercial fullerols. We achieved good separation efficiency using an amide-type hydrophilic interaction liquid chromatography (HILIC) column (plate number >2000) under isocratic conditions with 90% acetonitrile as the mobile phase. The method detection limits (MDLs) ranged from 42.8 ng/mL (UV detection) to 0.19 pg/mL (using MS with multiple reaction monitoring, MRM). Other MS measurement modes achieved MDLs of 125 pg/mL (single quad scan, Q1) and 1.5 pg/mL (multiple ion monitoring, MI). Each detection method exhibited a good linear response over several orders of magnitude. Moreover, we tested the robustness of these methods in the presence of Suvanee River fulvic acids (SRFA) as an example of organic matter commonly found in environmental water samples. While SRFA significantly interfered with UV- and Q1-based quantifications, the interference was relatively low using MI or MRM (relative error in presence of SRFA: 8.6% and 2.5%, respectively). This first report of a robust MS-based quantification method for modified fullerenes dissolved in water suggests the feasibility of implementing MS techniques more broadly for identification and quantification of fullerols and other water-soluble fullerene derivatives in environmental samples.     

无机矿物填料表面纳米化修饰及性能表征

采用化学方法对无机矿物填料表面进行包覆改性，制备出具有表面纳米化结构的复合矿物颗粒，有效地改善了原有颗粒的表面形貌，提高了比表面积，通过搅拌磨湿法研磨，讨论了包覆颗粒与基体的结合方式，初步证明了包覆颗粒与基体的结合方式为化学吸附而非物理吸附，两者结合牢固，包覆层不易脱落，包覆矿物颗粒在聚丙烯（PP）中填充，其复合材料的力学性能有较大的改善。     

Heteropolyanions doped polyimine—Preparation and spectroscopic properties

It is demonstrated that aromatic polyimine obtained by the condensation of p-phenylenediamine and terephtalaldehyde can be chemically doped with heteropolyanions of Keggin-type. The spectroscopic studies show that polyimine undergoes protonation. The structural identity of the Keggin units are preserved upon incorporation into the polymer matrix.