[Liu, Chang; Li, Feng; Ma, Lai-Peng; Cheng, Hui-Ming] Chinese Acad Sci, Inst Met Res, Shenyang Natl Lab Mat Sci, Shenyang 110016, Peoples R China.;Cheng, HM (reprint author), Chinese Acad Sci, Inst Met Res, Shenyang Natl Lab Mat Sci, 72 Wenhua Rd, Shenyang 110016, Peoples R China;cheng@imr.ac.cn

Advanced Materials for Energy Storage

The advantages in using nanoscale materials for electrochemical energy storage are generally attributed to short diffusion path lengths for both electronic and lithium ion transport. Here, we consider another contribution, namely the charge storage from faradaic processes occurring at the surface, referred to as pseudocapacitive effect. This paper describes the synthesis and pseudocapacitive characteristics of block copolymer templated anatase TiO2 thin films synthesized using either sol−gel reagents or preformed nanocrystals as building blocks. Both materials are highly crystalline and have large surface areas; however, the structure of the porosity is not identical. The different titania systems are characterized by a combination of small- and wide-angle X-ray diffraction/scattering, combined with SEM imaging and physisorption measurements. Following our previously reported approach, we are able to use the voltammetric sweep rate dependence to determine quantitatively the capacitive contribution to the ...

Templated Nanocrystal-Based Porous TiO2 Films for Next-Generation Electrochemical Capacitors

Chirality at the molecular level is found in diverse biological structures, such as polysaccharides, proteins and DNA, and is responsible for many of their unique properties. Introducing chirality into porous inorganic solids may produce new types of materials that could be useful for chiral separation, stereospecific catalysis, chiral recognition (sensing) and photonic materials. Template synthesis of inorganic solids using the self-assembly of lyotropic liquid crystals offers access to materials with well-defined porous structures, but only recently has chirality been introduced into hexagonal mesostructures through the use of a chiral surfactant. Efforts to impart chirality at a larger length scale using self-assembly are almost unknown. Here we describe the development of a photonic mesoporous inorganic solid that is a cast of a chiral nematic liquid crystal formed from nanocrystalline cellulose. These materials may be obtained as free-standing films with high surface area. The peak reflected wavelength of the films can be varied across the entire visible spectrum and into the near-infrared through simple changes in the synthetic conditions. To the best of our knowledge these are the first materials to combine mesoporosity with long-range chiral ordering that produces photonic properties. Our findings could lead to the development of new materials for applications in, for example, tuneable reflective filters and sensors. In addition, this type of material could be used as a hard template to generate other new materials with chiral nematic structures.

Free-standing mesoporous silica films with tunable chiral nematic structures

Nanoparticles in cellular drug delivery.

This review presents an extensive discussion on the major advances in the field of periodically organized mesoporous thin films (POMTFs) obtained via surfactant templated growth of inorganic or hybrid polymers. A large variety of templating agents can be coupled with inorganic polymerization reactions for the design of periodically organized nanostructured hybrid phases that yield POMTFs. The tuning of the interface between the template and the polymerizing phase and the control over chemical and processing conditions are the key parameters in producing tailor-made POMTFs with a high degree of reproducibility. This dynamic coupling between chemical and processing conditions dictates extensive use of complementary ex situ measurements with in situ characterization techniques that follow, in real time, film formation from the molecular precursor solutions to the final stabilized POMTF. Among modern analytical tools, 2D-GISAXS, ellipsoporosimetry, HRTEM, X-ray reflectometry, WAXS, time-resolved infrared spec...

Design, Synthesis, and Properties of Inorganic and Hybrid Thin Films Having Periodically Organized Nanoporosity†

Surfactant templating is a method that has successfully been used to produce nanoporous inorganic structures from a wide range of oxide-based material. Co-assembly of inorganic precursor molecules with amphiphilic organic molecules is followed first by inorganic condensation to produce rigid amorphous frameworks and then, by template removal, to produce mesoporous solids. A range of periodic surfactant/semiconductor and surfactant/metal composites have also been produced by similar methods, but for virtually all the non-oxide semiconducting phases, the surfactant unfortunately cannot be removed to generate porous materials. Here we show that it is possible to use surfactant-driven self-organization of soluble Zintl clusters to produce periodic, nanoporous versions of classic semiconductors such as amorphous Ge or Ge/Si alloys. Specifically, we use derivatives of the anionic Ge9(4-) cluster, a compound whose use in the synthesis of nanoscale materials is established. Moreover, because of the small size, high surface area, and flexible chemistry of these materials, we can tune optical properties in these nanoporous semiconductors through quantum confinement, by adsorption of surface species, or by altering the elemental composition of the inorganic framework. Because the semiconductor surface is exposed and accessible in these materials, they have the potential to interact with a range of species in ways that could eventually lead to new types of sensors or other novel nanostructured devices.

Hexagonal nanoporous germanium through surfactant-driven self-assembly of Zintl clusters.

In this paper, we explore the relationship between the nanoscale structure and electrochemical performance of nanoscale scrolls of vanadium oxides (vanadium oxide nanorolls). The vanadium oxide nanorolls, which are synthesized through a ligand-assisted templating method, exhibit different morphologies and properties depending upon the synthetic conditions. Under highly reducing conditions, nearly perfect scrolls can be produced which have essentially no cracks in the walls (well-ordered nanorolls). If the materials are produced under less reducing conditions, nanorolls with many cracks in the oxide walls can be generated (defect-rich nanorolls). Both types of samples were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoemission spectroscopy (XPS) to characterize their local structure, local redox state, and nanoscale structure. After ion-exchange to replace the templating ammonium ions with Na+, the ability of these materials to electrochemically intercalate lithium reversibly was investigated. In sweep voltammetry experiments, the well-ordered nanorolls showed responses similar to those seen in crystalline orthorhombic V2O5. In contrast, the defect-rich vanadium oxide nanorolls behaved electrochemically more like sol–gel-prepared vanadium oxide materials. Moreover, the specific capacity of the well-ordered nanorolls was about 240 mA h g–1 while that of the defect rich nanorolls was found to be as much as 340 mA h g–1 under these same conditions. Disorders on both the atomic and nanometer length scales are believed to contribute to this difference.

The Relationship Between Nanoscale Structure and Electrochemical Properties of Vanadium Oxide Nanorolls

Ambient-temperature chloroaluminate molten salts, mixtures of aluminum trichloride (AlCl3) and 1-ethyl-3-methylimidazolium chloride (ImCl), have been used as solvents to excise and isolate centered hexanuclear zirconium halide clusters from their solid-state precursors. Cluster compounds synthesized via high-temperature reactions, KZr6CCl15 and Li2Zr6MnCl15, were dissolved into basic molten salts at 100−110 °C. The C-centered cluster compound, Im4Zr6CCl18, was isolated in 70% yield, and the Mn-centered cluster compound, Im5Zr6MnCl18·C7H8·2CH3CN, was isolated in 54% yield. Im5Zr6BCl18 is efficiently oxidized by ferrocenium tetrafluoroborate, and one-electron-oxidized B-centered cluster, [(Zr6B)Cl18]4-, was isolated in 90% yield as the salt Im4Zr6BCl18.

Chloroaluminate ionic liquids as reagents for isolating soluble hexanuclear zirconium halide cluster compounds.

Ambient temperature AlCl(3)-1-ethyl-3-methylimidazolium chloride (ImCl) molten salts, both basic (40/60 mol % AlCl(3)/ImCl) and acidic (60/40 mol % AlCl(3)/ImCl), were used in an electrochemical investigation of centered hexanuclear zirconium halide clusters In the basic molten salt, these [(Zr(6)ZCl(12))Cl(6)](n-) (Z = Be, B, C, Mn, Fe) centered clusters exhibit the following electrochemical reactions on a glassy carbon electrode (potentials vs Al/Al(3+)): [(Zr(6)BeCl(12))Cl(6)](n)()(-) + e(-) right harpoon over left harpoon [(Zr(6)BeCl(12))Cl(6)](()(n)()(+1))(-), E(1/2) = -0613 V (n = 4), E(1/2) = -1085 V (n = 5); [(Zr(6)BCl(12))Cl(6)](n)()(-) + e(-) right harpoon over left harpoon [(Zr(6)BCl(12))Cl(6)](()(n)()(+1))(-), E(1/2) = -0365 V (n = 4), E(1/2) = 0072 V (n = 3); [(Zr(6)CCl(12))Cl(6)](n)()(-) + e(-) right harpoon over left harpoon [(Zr(6)CCl(12))Cl(6)](()(n)()(+1))(-), E(1/2) = 0230 V (n = 3); [(Zr(6)MnCl(12))Cl(6)](4)(-) + e(-) right harpoon over left harpoon [(Zr(6)MnCl(12))Cl(6)](5)(-), E(1/2) = -0432 V In the acidic melt, only electrochemical reactions [(Zr(6)BeCl(12))(AlCl(4))(6)](n)()(-) + e(-) right harpoon over left harpoon [(Zr(6)BeCl(12))(AlCl(4))(6)](()(n)()(+1))(-), E(1/2) = -0069 V (n = 5), E(1/2) = 0504 V (n = 4), and [(Zr(6)BCl(12))(AlCl(4))(6)](4)(-) + e(-) right harpoon over left harpoon [(Zr(6)BCl(12))(AlCl(4))(6)](5)(-), E(1/2) = 0700 V are clearly observed These data is consistent with less systematic observations of oxidation of these clusters in solution No unambiguous one-electron electrochemical reduction nor oxidation is observable for the Fe-centered cluster in the ionic liquids The half-wave potentials of the above reactions of the Be-, B-, C-, and Mn-centered clusters are controlled largely by clusters' charges This correlation of redox potentials allows a useful direct comparison with data for related hexanuclear niobium clusters in the literature

Electrochemistry of Centered Hexanuclear Zirconium Halide Clusters in Ambient-Temperature Chloroaluminate Molten Salts.

Chloroaluminate Ionic Liquids as Reagents for Isolating Soluble Hexanuclear Zirconium Halide Cluster Compounds.

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