Determination of the composition of Ultra‐thin Ni‐Si films on Si: constrained modeling of electron probe microanalysis and x‐ray reflectivity data

Phung, Tran M.; Jensen, Jacob Hjelmager; Johnson, David C.; Donovan, John J.; McBurnett, Brian

doi:10.1002/xrs.1102

Cited by 60 publications

(69 citation statements)

References 20 publications

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“…A thin film technique applying three different acceleration voltages (10,15, and 20 kV) described in details elsewhere [17] was utilized for precise compositional analysis.…”

Section: Methodsmentioning

confidence: 99%

Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]1.15)1(V1+Se2)n for n=1, 2, 3, 4, 5, and 6

Falmbigl

Putzky

Ditto

et al. 2015

Journal of Solid State Chemistry

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Cite this article as: M. Falmbigl, D. Putzky, J. Ditto and D.C. Johnson, Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]1.15)1(V1+xSe2)n for n=1, 2, 3, 4, 5, and 6, Journal of Solid State Chemistry, http://dx. AbstractA series of ferecrystalline compounds ([SnSe] 1.15 ) 1 (V 1+x Se 2 ) n with n = 1 -6 and a thin film V 1+x Se 2 were synthesized utilizing the modulated elemental reactant technique. The effect of interstitial V-atoms ranging from 0.13  x  0.42 in different compounds on structure and electrical properties of these intergrowth compounds is reported. The presence of the interstitial V-atoms for n > 1 was confirmed by Rietveld refinements as well as HAADF-STEM cross sections. The off-stoichiometry in the thin film V 1.13 Se 2 causes a suppression of the charge density wave, similar to the effect of non-stoichiometry observed for the bulk compound. The charge density wave of ([SnSe] 1.15 ) 1 (V 1+x Se 2 ) 1, however, is not affected by the non-stoichiometry due to its incorporation as volume inclusions or due to the quasi 2-dimensionality of the isolated VSe 2 layer. In the compounds ([SnSe] 1.15 ) 1 (V 1+x Se 2 ) n with n = 2 -6, the temperature dependence of the electrical resistivity approaches bulk-like behavior.

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“…A thin film technique applying three different acceleration voltages (10,15, and 20 kV) described in details elsewhere [17] was utilized for precise compositional analysis.…”

Section: Methodsmentioning

confidence: 99%

Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]1.15)1(V1+Se2)n for n=1, 2, 3, 4, 5, and 6

Falmbigl

Putzky

Ditto

et al. 2015

Journal of Solid State Chemistry

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“…* The Stratagem data analysis program was used to extract the film composition from the variation of the relative characteristic x-ray intensities as a function of accelerating voltage. 5,6 Pure metals and compounds were employed as microanalysis standards. Ten independent measurements at different positions on the samples were averaged to determine the final composition.…”

Section: Methodsmentioning

confidence: 99%

Synthesis and Electronic Properties of the Misfit Layer Compound [(PbSe)1.00]1[MoSe2]1

Heideman

Rostek

Anderson

et al. 2010

Journal of Elec Materi

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An ultralow-thermal-conductivity compound with the ideal formula [(PbSe) 1.00 ] 1 [MoSe 2 ] 1 has been successfully crystallized across a range of compositions. The lattice parameters varied from 1.246 nm to 1.275 nm, and the quality of the observed 00' diffraction patterns varied through the composition region where the structure crystallized. Measured resistivity values ranged over an order of magnitude, from 0.03 X m to 0.65 X m, and Seebeck coefficients ranged from À181 lV K À1 to 91 lV K À1 in the samples after the initial annealing to form the basic structure. Annealing of samples under a controlled atmosphere of selenium resulted in low conductivities and large negative Seebeck coefficients, suggesting an n-doped semiconductor. Scanning transmission electron microscopy cross-sections confirmed the interleaving of bilayers of PbSe with Se-Mo-Se trilayers. High-angle annular dark-field images revealed an interesting volume defect, where PbSe grew through a region where a layer of MoSe 2 would be expected in the perfect structure. Further studies are required to correlate the density of these defects with the observed electrical properties.

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“…Calibration of the deposition parameters is necessary to determine the amount of each element required for a Se-Sn-Se-V unit to self-assemble into a single (SnSe) 1.15 VSe 2 unit cell after annealing [19,20]. Composition of the films was analyzed by electron probe microanalysis (EPMA) using a thin film technique described by Phung [28]. Precursors were annealed under a nitrogen atmosphere ( < 1 ppm O 2 ) to self assemble the targeted compound.…”

Section: Methodsmentioning

confidence: 99%

Insights from STEM and NBED studies into the local structure and growth mechanism of misfit layered compounds prepared using modulated reactants

Häusler

Atkins

Falmbigl

et al. 2014

Zeitschrift Für Kristallographie - Crystalline Materials

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X-ray diffraction and transmission electron microscopy were used to probe the structure of the misfit compound [(SnSe) 1.15 ] 1 (VSe 2 ) 1 grown using an elementally modulated precursor. The specular X-ray diffraction pattern contained only 00l reflections, which yielded a c lattice parameter of 1.203(1) nm. Cross-section STEM revealed alternating layers of SnSe and VSe 2 , in agreement with the structure model refined from the X-ray diffraction pattern using Rietveld refinement. Plan-view transmission electron microscopy revealed the in-plane grain structure of the films, yielding grain sizes in agreement with previously reported in plane X-ray diffraction studies and the cross-section STEM images. The plan view images also contained Moiré fringes resulting from grains with different relative tilting on both sides of interfaces as well as Moiré fringes resulting from different relative rotations between domains. An energy-filtered nano-beam electron diffraction pattern obtained from at least one domain in the [(SnSe) 1.15 ] 1 (VSe 2 ) 1 sample investigated in cross section contained a series of resolvable supercell reflections along the c axis that indicated that the supercell c-axis lattice parameter was a multiple of three times that determined using X-ray diffraction. Energy filtered NBED of plan-view samples showed diffraction patterns from select regions with 12-fold symmetry, indicating that the arrangement of the layers is not rotationally random from layer to layer. This suggests that during the self-assembly of the amorphous modulated elemental precursor, the SnSe and VSe 2 constituent layers must nucleate off the adjacent interfaces of the growing crystal, yielding layers that are locally rotationally aligned with growing crystal. Different processing conditions during the precursor to crystal selfassembly might enable the domain size and/or the extent of order to be controlled.

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Determination of the composition of Ultra‐thin Ni‐Si films on Si: constrained modeling of electron probe microanalysis and x‐ray reflectivity data

Cited by 60 publications

References 20 publications

Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]1.15)1(V1+Se2)n for n=1, 2, 3, 4, 5, and 6

Influence of interstitial V on structure and properties of ferecrystalline ([SnSe]1.15)1(V1+Se2)n for n=1, 2, 3, 4, 5, and 6

Synthesis and Electronic Properties of the Misfit Layer Compound [(PbSe)1.00]1[MoSe2]1

Insights from STEM and NBED studies into the local structure and growth mechanism of misfit layered compounds prepared using modulated reactants

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