Ex situ and in situ Raman microscopic investigation of the differences between stoichiometric LiMO2 and high-energy xLi2MnO3·(1–x)LiMO2 (M = Ni, Co, Mn)

2014 ◽  
Vol 130 ◽  
pp. 206-212 ◽  
Author(s):  
Patrick Lanz ◽  
Claire Villevieille ◽  
Petr Novák
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.


2000 ◽  
Vol 14 (25n27) ◽  
pp. 2688-2693 ◽  
Author(s):  
E. GIANNINI ◽  
E. BELLINGERI ◽  
F. MARTI ◽  
M. DHALLÉ ◽  
V. HONKIMÄKI ◽  
...  

In-situ and ex-situ high energy (80÷88 keV) X-Ray diffraction from a synchrotron radiation source were performed on multifilamentary Bi, Pb(2223)/Ag tapes using a transmission scattering geometry. Several thermo-mechanical procedures were compared, focusing mainly on the texture development of both Bi, Pb(2212) and Bi, Pb(2223) phases. The effect of the periodic pressing on the texture and on the critical current is elucidated. The texture development of the Bi, Pb(2212) phase prior to its transformation into Bi, Pb(2223) was directly observed in-situ at high temperature by using a dedicated high-energy X-ray compatible furnace and a high resolution Image Plate detector. A sharp increase of the Bi, Pb(2212) grain orientation along the [00l] direction was found to occur only above 750°C. Normal state transport measurements are in full agreement with the formation mechanism and with the texture development observed. A comparison of the results with the ones provided by in-situ neutron diffraction and standard low-energy XRD in a reflection geometry is presented.


1991 ◽  
Vol 222 ◽  
Author(s):  
B. W. Liang ◽  
H. Q. Hou ◽  
C. W. Tu

ABSTRACTA simple kinetic model has been developed to explain the agreement between in situ and ex situ determination of phosphorus composition in GaAs1−xPx (x < 0.4) epilayers grown on GaAs (001) by gas-source molecular-beam epitaxy (GSMBE). The in situ determination is by monitoring the intensity oscillations of reflection high-energy-electron diffraction during group-V-limited growth, and the ex situ determination is by x-ray rocking curve measurement of GaAs1−xPx/GaAs strained-layer superlattices grown under group-III-limited growth condition.


2019 ◽  
Vol 627 ◽  
pp. A122 ◽  
Author(s):  
B. Augé ◽  
E. Dartois ◽  
J. Duprat ◽  
C. Engrand ◽  
G. Slodzian ◽  
...  

Context. Micrometeorites represent, at timescales shorter than a few million years, the dominant source of extraterrestrial matter at the surface of the Earth. Analyses of ultracarbonaceous micrometeorites recovered from Antarctica, known as UCAMMs reveal an exceptionally N-rich organic matter associated with spatially extended high D enrichments. Experiments show that this specific organic matter might have been formed in the outer solar system by energetic irradiation of N-rich icy surfaces. Aims. We experimentally investigate the hydrogen isotopic fractionation resulting from irradiation of normal and D-rich N2-CH4 ices by high energy ions, simulating the exposition to Galactic cosmic rays of icy bodies surfaces orbiting at large heliocentric distances. Methods. Films of N2-CH4 ices and a N2-CH4/CD4/N2-CH4 “sandwich” ice were exposed to 129Xe13+ ion beams at 92 and 88 MeV. The chemical evolution of the samples was monitored using in situ Fourier transform infrared spectroscopy. After irradiation, targets were annealed to room temperature. The solid residues of the whole process left after ice sublimation were characterized in situ by infrared spectroscopy, and the hydrogen isotopic composition measured ex situ by imaging secondary ion mass spectrometry at the sub-micron scale (NanoSIMS). Results. Irradiation leads to the formation of new molecules and radicals. After annealing, the resulting poly-HCN-like macro-molecular residue exhibits an infrared spectrum close to that of UCAMMs. The residue resulting from irradiation of N2-CH4 ices does not exhibit a significant deuterium enrichment comparable to that found in extraterrestrial organic matter. The residue formed by irradiation of D-rich ices shows the formation of isotopic heterogeneities with localised hotspots and an extended contribution likely due to the diffusion of the radiolytic products from the D-rich layer. Conclusions. These results show that high-energy cosmic ray irradiation does not induce the large hydrogen isotopic fractionation observed at small spatial scale in interplanetary organics. By contrast, large D/H ratio heterogeneities at the sub-micron spatial scale in extraterrestrial organic matter can result from isotopically heterogeneous ices mixtures (i.e. condensed with different D/H ratios), which were transformed into refractory organic matter upon irradiation.


1993 ◽  
Vol 313 ◽  
Author(s):  
I. Hashim ◽  
H.A. Atwater ◽  
Thomas J. Watson

ABSTRACTWe have investigated structural and magnetic properties of epitaxial Ni80Fe20 films grown on relaxed epitaxial Cu/Si (001) films. The crystallographic texture of these films was analyzed in situ by reflection high energy electron diffraction (RHEED), and ex situ by x-ray diffraction and cross-sectional transmission electron Microscopy (XTEM). In particular, RHEED intensities were recorded during epitaxial growth, and intensity profiles across Bragg rods were used to calculate the surface lattice constant, and hence, find the critical epitaxial thickness for which Ni80Fe20 grows pseudomorphically on Cu (100). XTEM analysis indicated that the epitaxial films had atomically-abrupt interfaces which was not the case for polycrystalline Cu and Ni80Fe20 film interfaces. The Magnetic properties of these epitaxial films were Measured in situ using Magneto-optic Kerr effect magnetometry and were compared with those of polycrystalline films grown on SiO2/Si. Large Hc (∼ 35 Oe) was observed for epitaxial Ni80Fe20 films less than 3.0 nm thick whereas for increasing thickness, Hc decreased approximately monotonically to a few Oersteds. Correlations were made between magnetic properties of these epitaxial films, the strain in the film and the interface roughness obtained from XTEM analysis.


1993 ◽  
Vol 312 ◽  
Author(s):  
A. H. Bensaoula ◽  
A. Freundlich ◽  
A. Bensaoula ◽  
V. Rossignol

AbstractPhosphorus exposed GaAs (100) surfaces during a Chemical Beam Epitaxy growth process are studied using in-situ Reflection High Energy Electron Diffraction and ex-situ High Resolution X-ray Diffraction. It is shown that the phosphorus exposure of a GaAs (100) surface in the 500 – 580 °C temperature range results in the formation of one GaP monolayer.


1991 ◽  
Vol 220 ◽  
Author(s):  
Q. F. Xiao ◽  
J. R. Jimenez ◽  
L. J. Schowalter ◽  
L. Luo ◽  
T. E. Mitchell ◽  
...  

ABSTRACTEpitaxial Si layers have been grown under a variety of growth conditions on CoSi2 (001) by molecular beam epitaxy (MBE). The structural properties of the Si overgrowth were studied by in-situ Reflection High Energy Electron Diffraction (RHEED), as well as ex-situ MeV4He+ ion channeling and High Resolution Transmission Electron Microscopy (HRTEM). Strong influences of the CoSi2 surface reconstruction on the Si overgrowth have been observed. RHEED studies show islanding growth of Si on the CoSi2 (001) (3/√2 × √2)R45 reconstructed surface, but smooth growth of Si on the CoSi2 (001) {√2 × √2)R45 reconstructed surface, under the same growth conditions. The growth of Si on thin layers of CoSi2 (2nm-6nm) with (√2 × √2)R45 reconstructed surface at 460°C results in high crystalline quality for the Si top layer, as indicated by good channeling minimum yield (Xmin < 6%), but cross-sectional TEM shows that the CoSi2 layers are discontinuous. We also report preliminary results on Si grown on a 2 × 2 reconstructed CoSi2 (001) surface.


Author(s):  
Felix Schmeiser ◽  
Erwin Krohmer ◽  
Christian Wagner ◽  
Norbert Schell ◽  
Eckart Uhlmann ◽  
...  

AbstractLaser powder bed fusion is an additive manufacturing process that employs highly focused laser radiation for selective melting of a metal powder bed. This process entails a complex heat flow and thermal management that results in characteristic, often highly textured microstructures, which lead to mechanical anisotropy. In this study, high-energy X-ray diffraction experiments were carried out to illuminate the formation and evolution of microstructural features during LPBF. The nickel-base alloy Inconel 625 was used for in situ experiments using a custom LPBF system designed for these investigations. The diffraction patterns yielded results regarding texture, lattice defects, recrystallization, and chemical segregation. A combination of high laser power and scanning speed results in a strong preferred crystallographic orientation, while low laser power and scanning speed showed no clear texture. The observation of a constant gauge volume revealed solid-state texture changes without remelting. They were related to in situ recrystallization processes caused by the repeated laser scanning. After recrystallization, the formation and growth of segregations were deduced from an increasing diffraction peak asymmetry and confirmed by ex situ scanning transmission electron microscopy. Graphical Abstract


2020 ◽  
Author(s):  
Miao Wang ◽  
Zhenpeng Yao ◽  
Qianqian Li ◽  
Yongfeng Hu ◽  
Jing Zhang ◽  
...  

<p>Wadsley-Roth (W-R) structured oxides featured with wide channels represent one of the most promising material families showing compelling rate performance for lithium ion batteries. But the structural origin for the fast kinetics of W-R structures is not well understood. Herein, we report an in-depth study on the fast and extensive intercalation chemistry of phosphorus stabilized W-R phase PNb<sub>9</sub>O<sub>25 </sub>and its application in high energy and fast-charging devices. We explore the intercalation geometry of PNb<sub>9</sub>O<sub>25</sub> and identify two geometrical types of stable insertion sites with the total amount (2.22 per Nb ion) much higher than conventional intercalation-type electrodes. We reveal the ion transportation kinetics that the Li ions initially diffuse along the open type III channels and then penetrate to type-α edge sites with low kinetic barriers. Through <i>in-situ</i> TEM and <i>ex-situ</i> XRD investigations, we confirm that the whole intercalation/deintercalation process proceeds <i>via</i> a solid-solution behavior with continuous lithium (de)occupying/(re)ordering on the identified insertion sites exhibiting nearly “zero-stress” characteristics. Therefore, the oxide framework of PNb<sub>9</sub>O<sub>25</sub> keeps almost intact with all the fast diffusion channels and insertion cavities well-maintained upon cycling, which accomplishes the unconventional electrochemical performance of<sub> </sub>W-R structured electrodes.</p>


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