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53
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2, in the presence of one equivalent oleic acid. After 48 h, the solvent is either evaporated to dryness, leading to sample 1; or the solution is concentrated and poured into a large volume of cold pentane to ensure precipitation of the particles (sample 2). Cobalt content in each sample was determined by chemical microanalysis at the CNRS center, Vernaison, France
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2, in the presence of one equivalent oleic acid. After 48 h, the solvent is either evaporated to dryness, leading to sample 1; or the solution is concentrated and poured into a large volume of cold pentane to ensure precipitation of the particles (sample 2). Cobalt content in each sample was determined by chemical microanalysis at the CNRS center, Vernaison, France.
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Transmission electron microscopy (TEM) was used to determine both particle size, size distribution and interparticle distances. Low-resolution TEM measurements were performed on a JEOL 200 CX (200 kV) at the TEMSCAN facility, Université Paul-Sabatier, Toulouse. More than 200 particles were measured to draw each size or distance histogram
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Transmission electron microscopy (TEM) was used to determine both particle size, size distribution and interparticle distances. Low-resolution TEM measurements were performed on a JEOL 200 CX (200 kV) at the TEMSCAN facility, Université Paul-Sabatier, Toulouse. More than 200 particles were measured to draw each size or distance histogram.
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5) in anisole was heated at reflux for 3 h in the presence of one equivalent (versus the total metal content) of HDA. During this time the initial orange solution turns black. The reaction is conducted under argon to avoid any surface oxidation of the particles. After evaporation of the crude solution to dryness, the solid material has been characterised without further purification step. The nickel and iron contents were determined by chemical microanalysis. Ni: 6.85% Fe: 5.67%. (i.e. metal content 12.52%)
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5) in anisole was heated at reflux for 3 h in the presence of one equivalent (versus the total metal content) of HDA. During this time the initial orange solution turns black. The reaction is conducted under argon to avoid any surface oxidation of the particles. After evaporation of the crude solution to dryness, the solid material has been characterised without further purification step. The nickel and iron contents were determined by chemical microanalysis. Ni: 6.85% Fe: 5.67%. (i.e. metal content 12.52%).
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WAXS structural characterisations by WAXS were performed in the solid state. The fine powder was introduced in a thin walled Lindemann capillary of 1 mm diameter subsequently sealed under argon. Measurements of the X-ray intensity scattered by the samples irradiated with graphite-monochromatised molybdenum Kα radiation (0.071069 nm) were performed using a dedicated two-axis diffractometer. Fluorescence from iron and nickel was removed at the measurement step by filtering. Time for data collection was typically 20 h for a set of 457 measurements collected at room temperature in the range 0° < θ < 65° for equidistant s values [s = 4π(sinθ/λ)]
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WAXS structural characterisations by WAXS were performed in the solid state. The fine powder was introduced in a thin walled Lindemann capillary of 1 mm diameter subsequently sealed under argon. Measurements of the X-ray intensity scattered by the samples irradiated with graphite-monochromatised molybdenum Kα radiation (0.071069 nm) were performed using a dedicated two-axis diffractometer. Fluorescence from iron and nickel was removed at the measurement step by filtering. Time for data collection was typically 20 h for a set of 457 measurements collected at room temperature in the range 0° < θ < 65° for equidistant s values [s = 4π(sinθ/λ)].
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59
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To be published
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To be published.
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0000678732
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FCC packing of nanoparticles, resulting from layer by layer growth on a compact 2D assembly of particles, has already been reported. In this case the interparticle spacings were identical in 2D and 3D assemblies
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FCC packing of nanoparticles, resulting from layer by layer growth on a compact 2D assembly of particles, has already been reported. In this case the interparticle spacings were identical in 2D and 3D assemblies A. Korgel S. Fullam S. Connolly D. Fitzmaurice J. Phys. Chem. B 1998 102 8379.
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J. Phys. Chem. B
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, pp. 8379
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Korgel, A.1
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Connolly, S.3
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62
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F. Dassenoy K. Philippot T. Ould Ely C. Amiens P. Lecante E. Snoeck A. Mosset M.-J. Casanove B. Chaudret New J. Chem. 1998 22 703.
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New J. Chem.
, vol.22
, pp. 703
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Dassenoy, F.1
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Lecante, P.5
Snoeck, E.6
Mosset, A.7
Casanove, M.-J.8
Chaudret, B.9
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65
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−1. Typical counting times for the 0.6 m detector position were 2.5 min. Background counts, recorded with an empty sample tube, were very low and showed no specific features. The 2D-diffraction patterns were radially integrated using the software package FIT2D (A. P. Hammersley, ESRF Internal Report, ESRF97HA02T, 1997, “FIT2D: An Introduction and Overview”) to display the intensity profile as a function of the scattering angle or vector
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−1. Typical counting times for the 0.6 m detector position were 2.5 min. Background counts, recorded with an empty sample tube, were very low and showed no specific features. The 2D-diffraction patterns were radially integrated using the software package FIT2D (A. P. Hammersley, ESRF Internal Report, ESRF97HA02T, 1997, “FIT2D: An Introduction and Overview”) to display the intensity profile as a function of the scattering angle or vector.
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Magnetisation measurements were performed on a SQUID magnetometer (MPMS Quantum Design). The temperature was varied between 2 and 300 K according to a classical zero field cooling/field cooling (ZFC/FC) procedure in the presence of a very weak applied magnetic field (10 Oe) and the hysteresis cycles were obtained at different temperatures in a magnetic field varying from + 50 to −50 kOe. The samples were prepared in gelatine capsules in a glove box to avoid any oxidation of the materials
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Magnetisation measurements were performed on a SQUID magnetometer (MPMS Quantum Design). The temperature was varied between 2 and 300 K according to a classical zero field cooling/field cooling (ZFC/FC) procedure in the presence of a very weak applied magnetic field (10 Oe) and the hysteresis cycles were obtained at different temperatures in a magnetic field varying from + 50 to −50 kOe. The samples were prepared in gelatine capsules in a glove box to avoid any oxidation of the materials.
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J. L. Dormann F. D’Orazio F. Lucarri E. Tronc P. Prené D. Fiorani D. Cherkaoui R. Noguès Phys. Rev. B 1996 53 14 291.
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, vol.53
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Dormann, J.L.1
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Fiorani, D.6
Cherkaoui, D.7
Noguès, R.8
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