Temperature driven morphological changes of hydrothermally prepared copper oxide nanoparticles

The size and shape of nanocrystals have a strong effect on the optical, electrical and catalytic properties. Therefore, controlling the size, shape and structure of nanocrystals is technically important. The controlled synthesis of CuO nanostructures was achieved using a hydrothermal process by simply controlling the precipitation reaction temperature between copper nitrate trihydrate and sodium hydroxide. The Scanning Electron Microscopy (SEM), EDS, XRD, and FTIR analysis revealed that the synthesized product at 200 °C is of pure copper oxide particles. From Scherrer formula, the prepared CuO particles varied approximately 3–7 nm in size simply by varying the reaction temperature. The synthesized particles exhibited a regular flake like morphology and had a uniform size distribution. The morphology and size depend on the reaction conditions. Copyright © 2008 John Wiley & Sons, Ltd.     

Synthesis and Crystal Structure of Mercury(II) Metal Crown Ether with N‐Heterocyclic Carbene Linkage

The mercury(II) metal crown ether ( 2a ) was obtained in high yield by reaction of the carbene precursor 1,2‐bis[N‐(1‐naphthylmethylene)imidazoliumethoxy]benzene dihexafluorophosphate ( 1 ) and Hg(OAc)₂. Addition of NaI to the acetone solution of 2a resulted in precipitation of pale yellow solid 2b . The structures of 2a and 2b were determined by single‐crystal X‐ray diffractometry. Both molecules display a helical conformation with a torsional cycle. The mercury atom in complex 2a is tricoordinated by two intramolecular carbene carbon atoms and an acetate oxygen atom. The mercury atom in complex 2b is tetracoordinated by two intramolecular carbene carbon atoms and two cis‐iodine atoms.     

光色效应(Fe,Mn)\:LiNbO3晶体非挥发性全息存储中自衍射效应的实验研究

在双掺杂 (Fe ,Mn)…LiNbO3 晶体光色效应非挥发性全息存储实验中 ,观测到光束耦合作用导致的自增强和自衰减效应。根据这种自衍射效应 ,归纳了四种记录和光固定实验组合方案。实验结果表明 ,在记录和光固定过程中利用自增强效应得到的最高衍射效率为利用自衰减效应得到的衍射效率的两倍左右 ,说明在实际应用中必须考虑和利用自增强效应。     

Triacetylcellulose on silica compared with non-dilute triacetylcellulose I as a high-performance liquid chromatographic sorbent

Summary Triacetylcellulose coated on silica is a novel HPLC sorbent introduced for the separation of enantiomers. A comparison of enantioselectivities α, and resolutions R₅ of this material with known pure triacetylcellulose I shows considerable differences. From X-ray wideangle diffraction it is suggested that the novel sorbent also consists of the triacetylcellulose modification I, but its degree of crystallinity is probably lower than that of the non-dilute sorbent. The advantages of the two stationary phases are discussed. Liquid Chromatography on Triacetylcellulose, Part 13. For Part 12, see ref. [1].     

Quantitative surface analysis performed with an imaging photoelectron spectrometer

The paper gives an outline of the basic principle of our imaging technique for XPS. The advantage of the concept is its excellent applicability to quantitative pixel information. This idea is verified by two examples which are representative for routine problems in XPS. These are quantitative surface analysis and determination of overlayer thicknesses. A lateral resolution of at least 0.2 mm is achieved and thus a pixel size of 0.2 mm × 0.2 mm can be quantified automatically by means of numerical algorithms without need of reference samples.Dedicated to Professor Günther Tölg on the occasion of his 60th birthday     

Formation of niobium oxynitrides by rapid thermal processing (RTP)

The potential of rapid thermal processing (RTP) for the preparation of thin films of niobium oxynitrides was investigated. The 200 and 500 nm niobium films were deposited via sputtering on oxidized silicon(1 0 0)- and on sapphire(1 −1 0 2)-substrates. At first, oxidation of niobium films in molecular oxygen and then nitridation in ammonia using an RTP-system was performed. The films were characterized before and after the oxidation and nitridation processes by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and secondary ion mass spectrometry (SIMS). The influence of the two different substrates, amorphous SiO₂ and single crystalline sapphire on the reactivity of the niobium films was studied in dependence of temperature, time of reaction and film thickness. The existence of niobium oxynitride formation was verified for some of the films. In some of the experiments, crack formation in the films or even delamination of the Nb-films from the substrates was observed.     

Novel structurally characterized o-semiquinonato PCP-pincer nickel complexes

Structural study of dialkyl (PCP)-pincer o-semiquinonato nickel complexes indicated sloped relative positions of bi- and tri-dentate ligands. It became bright confirmation of propositions made on the base of their EPR spectra followed by molecular modelling.     

Crystalline structure of sequential poly(ester amide)s derived from glycolic acid, 1,6‐hexanediamine,and even aliphatic dicarboxylic acids

Basic structural data of two sequential poly(ester amide)s derived from glycolic acid, 1,6‐hexanediamine, and adipic acid or dodecanodioic acid have been determined by means of X‐ray and electron diffraction patterns from fibers and single crystals. Chain‐folded lamellar crystals were obtained by isothermal crystallization from diol or glycerine solutions, and the crystalline habit was investigated by real space electron microscopy. Polyethylene decoration techniques were applied to evaluate the regularity of the folding surfaces. Spherulites prepared from evaporation of formic acid solutions were also studied. The two sequential poly(ester amide)s crystallized according to triclinic and monoclinic unit cells, in which the a crystallographic parameter was close to the typical distance between hydrogen‐bonded chains. Projections viewed down the chain axis revealed differences in the packing mode since oblique and rectangular cells were found for the adipic acid and dodecanodioic acid derivatives, respectively. Both structures can be envisaged as a stacking of hydrogen‐bonded sheets although clear differences concerning the shift between consecutive sheets and the number of layers comprising the unit cell were found. The large unit cells that have been deduced seem to be a consequence of the different packing preferences of the diester and diamide moieties. Both polymers have a molecular conformation that deviates from the all‐trans conformation typical of aliphatic polyamides and polyesters with a large number of methylene groups. © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 194–206, 2009     

X‐ray photoelectron spectroscopic chemical state quantification of mixed nickel metal,oxide and hydroxide systems

Quantitative chemical state X‐ray photoelectron spectroscopic analysis of mixed nickel metal, oxide, hydroxide and oxyhydroxide systems is challenging due to the complexity of the Ni 2p peak shapes resulting from multiplet splitting, shake‐up and plasmon loss structures. Quantification of mixed nickel chemical states and the qualitative determination of low concentrations of Ni(III) species are demonstrated via an approach based on standard spectra from quality reference samples (Ni, NiO, Ni(OH)₂, NiOOH), subtraction of these spectra, and data analysis that integrates information from the Ni 2p spectrum and the O 1s spectra. Quantification of a commercial nickel powder and a thin nickel oxide film grown at 1‐Torr O₂ and 300 °C for 20 min is demonstrated. The effect of uncertain relative sensitivity factors (e.g. Ni 2.67 ± 0.54) is discussed, as is the depth of measurement for thin film analysis based on calculated inelastic mean free paths. Copyright © 2009 John Wiley & Sons, Ltd.