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Selected-area Electron Diffraction (selected-area + electron_diffraction)
Selected AbstractsSurfactant-Assisted Synthesis and Characterization of Novel Chain-Like CoNi Alloy AssembliesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 25 2007Lu-Ping Zhu Abstract Novel chain-like CoNi alloy assemblies with a length of up to 6,7 ,m were successfully prepared by a surfactant-assisted hydrothermal synthetic route at 100 °C for 2 h. The individual submicrospheres built from smaller CoNi nanoparticles had a diameter of about 400,500 nm. These microspheres were then integrated to form the novel chain-like CoNi alloy assemblies. The effects of synthetic parameters such as surfactant and solvent on the formation and morphology of CoNi samples were investigated. The experimental results showed that N2H4·H2O and CTA+ play important roles in the formation of the novel chain-like CoNi alloy assemblies. Based on the structural information provided by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, selected-area electron diffraction and energy-dispersive X-ray analysis, a growth mechanism was tentatively proposed for the formation of chain-like CoNi alloy assemblies. Magnetic hysteresis measurement revealed that the chain-like CoNi alloy assemblies display ferromagnetic behavior with a saturation magnetization of 96.15 emu/g and a coercivity of 144.75 Oe at room temperature. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Synthesis, Mechanism, and Gas-Sensing Application of Surfactant Tailored Tungsten Oxide NanostructuresADVANCED FUNCTIONAL MATERIALS, Issue 11 2009Suman Pokhrel Abstract Widely applicable nonaqueous solution routes have been employed for the syntheses of crystalline nanostructured tungsten oxide particles from a tungsten hexachloride precursor. Here, a systematic study on the crystallization and assembly behavior of tungsten oxide products made by using the bioligand deferoxamine mesylate (DFOM) (product I), the two chelating ligands hexadecyltrimethylammoniumbromide (CTAB) (II) and poly(alkylene oxide) block copolymer (Pluronic P123) (III) is presented. The mechanistic pathways for the material synthesis are also discussed in detail. The tungsten oxide nanomaterials and reaction solutions are characterized by Fourier transform IR, 1H, and 13C NMR spectroscopies, powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM, and selected-area electron diffraction. The indexing of the line pattern suggests WO3 is in its monoclinic structure with a,=,0.7297,nm, b,=,0.7539,nm, c,=,0.7688,nm, and ,-i;,=,90.91,°. The nanoparticles formed have various architectures, such as chromosomal shapes (product I) and slates (II), which are quite different from the mesoporous one (III) that has internal pores or mesopores ranging from 5 to 15,nm. The nanoparticles obtained from all the synthetic procedures are in the range of 40,60,nm. The investigation of the gas-sensing properties of these materials indicate that all the sensors have good baseline stability and the sensors fabricated from material III present very different response kinetics and different CO detection properties. The possibility of adjusting the morphology and by that tuning the gas-sensing properties makes the preparation strategies used interesting candidates for fabricating gas-sensing materials. [source] A Spring-Like Behavior of Chiral Block Copolymer with Helical Nanostructure Driven by CrystallizationADVANCED FUNCTIONAL MATERIALS, Issue 3 2009Yeo-Wan Chiang Abstract The crystallization of helical nanostructure resulting from the self-assembly of a chiral diblock copolymer, poly(styrene)- b -poly(L -lactide) (PS-PLLA), is studied. Various crystalline PS-PLLA nanostructures are obtained by controlling the crystallization temperature of PLLA (Tc,PLLA), at which crystalline helices and crystalline cylinders occur while Tc,PLLA,<,Tg,PS (the glass transition temperature of PS) and Tc,PLLA,,,Tg,PS, respectively. As evidenced by selected-area electron diffraction and two-dimensional X-ray diffraction results, the PLLA crystallites under confinement reveal a unique anisotropic character regardless of the crystallization temperature. On the basis of observed uniaxial scattering results the PLLA crystallites grown within the microdomains are identified as crystals with preferential growth directions either along the [100] or along the [110]-axes of the PLLA crystalline unit cell, at which the molecular chains and the growth direction are normal and parallel to the central axes of helices, respectively. The formation of this exclusive crystalline growth is attributed to the spatial confinement effect for crystallization. While Tc,PLLA,<,Tg,PS, owing to the directed crystallization by helical confinement, the preferential crystalline growth leads to the crystallization following a helical track with growth direction parallel to the central axes of helices through a twisting mechanism. Consequently, winding crystals with specific crystallographic orientation within the helical microdomains can be found. By contrast, while Tc,PLLA,,,Tg,PS, the preferential growth may modulate the curvature of microdomains by shifting the molecular chains to access the fast path for crystalline growth due to the increase in chain mobility. As a result, a spring-like behavior of the helical nanostructure can be driven by crystallization so as to dictate the transformation of helices, resulting in crystalline cylinders that might be applicable to the design of switchable large-strain actuators. [source] Formation of Highly Crystallized ,-PbO Thin Films by Cathodic Electrodeposition of Pb and Its Rapid Oxidation in Air,ADVANCED FUNCTIONAL MATERIALS, Issue 2 2005S. Sawatani Abstract The process of electrodeposition of ,-PbO thin films from aqueous solutions of PbII salts has been studied in detail. Contrary to the mechanism assumed in previous studies, thin films of crystalline ,-PbO are obtained after cathodic electrolysis in aqueous solutions of various soluble salts of PbII (Pb(NO3)2, Pb(ClO4)2, and Pb(CH3COO)2), and in both the presence and the absence of O2, thus indicating no contribution of OH, generation by electroreduction of NO3, and/or O2 to the formation of ,-PbO. A gradual color change is noted: a freshly electrodeposited gray film turns yellow as it dries in air. Drying of the films under controlled atmosphere (Ar or O2), combined with scanning electron microscopy (SEM) observation and X-ray diffraction (XRD) measurement, has revealed that freshly deposited films are of metallic Pb, which are oxidized and converted into ,-PbO. Such a reaction is operative only when a freshly electrodeposited activated wet Pb film is in contact with gaseous O2. Despite the rapid conversion of a solid material, the resultant ,-PbO thin films are highly crystallized and possess highly ordered internal nanostructure. Elongated nanoparticles (30,nm,×,100,nm) are assembled in a regular alignment to compose a large platelet (greater than 10,,m in size) with single-crystalline character, as revealed by transmission electron microscopy (TEM) observation and selected-area electron diffraction (SAED) measurement. [source] Crystalline Transition from H2Ti3O7 Nanotubes to Anatase Nanocrystallines Under Low-Temperature Hydrothermal ConditionsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 11 2006Ning Wang In this paper, we first reported the crystalline transition from H2Ti3O7 nanotubes to anatase TiO2 nanocrystallines under low-temperature hydrothermal conditions (,140°C). A newly proposed mechanism for the crystalline transition from H2Ti3O7 nanotubes to anatase TiO2 nanocrystallines under low-temperature conditions is discussed in detail, which is supported by X-ray diffraction, high-resolution transmission electronic microscope, selected-area electron diffraction, and crystal structure models. [source] Octahedral tilt twinning and compositional modulation in NaLaMgWO6ACTA CRYSTALLOGRAPHICA SECTION B, Issue 6 2009Graham King A combination of selected-area electron diffraction (SAED), neutron powder diffraction (NPD) and high-resolution transmission electron microscopy (HRTEM) reveals a complex superstructure in the ordered perovskite NaLaMgWO6. Through indexing of SAED patterns the unit-cell dimensions are found to be 46.8 × 7.8 × 7.9,Å, which corresponds to a 12ap× 2ap× 2ap superstructure of the simple perovskite unit cell. HRTEM images reveal the formation of an unmistakable stripe contrast that repeats with the same periodicity. Doubling of the b and c axes is brought about by a combination of layered ordering of Na and La, rock-salt ordering of Mg and W, and octahedral tilting. The a axis repeat distance results from a one-dimensional twinning of the octahedral tilts in combination with a compositional modulation. Modeling of the NPD pattern shows that the underlying tilt system is a,a,c0 with tilt angles of ,,8° about the a and b axes. The octahedral tilt-twin boundaries run perpendicular to the a axis and are separated by 6ap. Simulated HRTEM images show that octahedral tilt twinning alone cannot explain the stripes seen in the HRTEM images, rather a compositional modulation involving the A -site cations is necessary to explain the experimental images. [source] Electron diffraction of ABX3 perovskites with both layered ordering of A cations and tilting of BX6 octahedraACTA CRYSTALLOGRAPHICA SECTION B, Issue 4 2009Kyosuke Kishida It is shown that 21 ABX3 perovskites with tilted BX6 octahedra and layered ordering of A cations can be generated on the basis of group,subgroup relations. These structures (with 16 different space groups) are classified into ten diffraction types in terms of the conditions for superstructure reflections caused by the ordering of A cations, tilting of BX6 octahedra and structural absences. SAED (selected-area electron diffraction) allows the distinction of seven of the 21 different perovskites, while additional symmetry analysis by CBED (convergent-beam electron diffraction) is needed for the remaining 14 structures. The space groups of lithium lanthanum titanate pseudomorphs (with discrete chemical compositions) are successfully deduced by electron diffraction experiments. [source] | |||||||||||||