In Situ NMR, Ex Situ XRD and SEM Study of the Hydrothermal Crystallization of Nanoporous Aluminum Trimesates MIL-96, MIL-100, and MIL-110

2012 ◽  
Vol 24 (13) ◽  
pp. 2462-2471 ◽  
Author(s):  
Mohamed Haouas ◽  
Christophe Volkringer ◽  
Thierry Loiseau ◽  
Gérard Férey ◽  
Francis Taulelle
Keyword(s):  
Ex Situ ◽  
Hydrothermal Crystallization ◽  
Sem Study ◽  
In Situ Nmr ◽  
Ex Situ Xrd

Growth, structure and properties of magnetron sputtered ultra-thin WTi films

2013 ◽  
Vol 1580 ◽  
Author(s):  
A. Le Priol ◽  
E. Le Bourhis ◽  
P.-O. Renault ◽  
L. Simonot ◽  
G. Abadias ◽  
...  
Keyword(s):  
Fiber Texture ◽  
Ex Situ ◽  
Structure And Properties ◽  
Working Pressure ◽  
Wafer Curvature ◽  
Size Dependent ◽  
Growth Structure ◽  
Refractory Metal Alloy ◽  
Ex Situ Xrd

ABSTRACTRefractory metal alloy WTi films were elaborated by magnetron sputtering from an alloyed target (W:Ti ∼ 70:30 at%). Film continuity threshold has been determined at 4.5 ± 0.2 nm using in situ surface differential reflectance (SDR) technique. Prior to film continuity, deposition of a continuous interfacial layer is suggested by both in situ and real-time SDR and wafer-curvature techniques. After continuity, WxTi1-x films (9.5 nm thick WTi films) have a body-centered structure with a {110} fiber texture. Composition (x) and microstructure can be tuned varying working pressure. A transition from compressive to tensile residual stresses was observed by ex situ XRD and wafer-curvature methods. Size dependent resistivity is obtained and slightly varies as a function of working pressure.

Controlled Solubilization of Toluene by Silicate−Catanionic Surfactant Mesophases as Studied by in Situ and ex Situ XRD

Langmuir ◽  
2002 ◽  
Vol 18 (4) ◽  
pp. 1380-1385 ◽  
Author(s):  
Anna Lind ◽  
Jenny Andersson ◽  
Stefan Karlsson ◽  
Patrik Ågren ◽  
Patrick Bussian ◽  
...  
Keyword(s):  
Ex Situ ◽  
Catanionic Surfactant ◽  
Ex Situ Xrd

scholarly journals Exploiting In-Situ NMR to Monitor the Formation of a Metal-Organic Framework

2020 ◽  
Author(s):  
Corey Jones ◽  
Colan Hughes ◽  
Hamish Yeung ◽  
Alison Paul ◽  
Kenneth D. M. Harris ◽  
...  
Keyword(s):  
Self Assembly ◽  
Metal Organic Framework ◽  
Quantitative Information ◽  
Ex Situ ◽  
Nmr Studies ◽  
In Situ Techniques ◽  
Nmr Study ◽  
Metal Organic ◽  
In Situ Nmr

The formation processes of metal-organic frameworks are becoming more widely researched using in-situ techniques, although there remains a scarcity of NMR studies in this field. In this work, the synthesis of framework MFM-500(Ni) has been investigated using an in‑situ NMR strategy that provides information on the time-evolution of the reaction and crystallization process. In our in‑situ NMR study of MFM-500(Ni) formation, liquid-phase 1H NMR data recorded as a function of time at 5 fixed temperatures afford qualitative information on the solution-phase processes and quantitative information on the kinetics of crystallization, allowing the activation energies for nucleation and growth to be determined. Ex-situ SAXS studies provide complementary nanoscale information on the rapid self-assembly prior to MOF crystallization and in-situ powder X-ray diffraction confirms that the only crystalline phase present during the reaction is phase-pure MFM-500(Ni).

scholarly journals Exploiting In-Situ NMR to Monitor the Formation of a Metal-Organic Framework

2020 ◽  
Author(s):  
Corey Jones ◽  
Colan Hughes ◽  
Hamish Yeung ◽  
Alison Paul ◽  
Kenneth D. M. Harris ◽  
...  
Keyword(s):  
Self Assembly ◽  
Metal Organic Framework ◽  
Quantitative Information ◽  
Ex Situ ◽  
Nmr Studies ◽  
In Situ Techniques ◽  
Nmr Study ◽  
Metal Organic ◽  
In Situ Nmr

The formation processes of metal-organic frameworks are becoming more widely researched using in-situ techniques, although there remains a scarcity of NMR studies in this field. In this work, the synthesis of framework MFM-500(Ni) has been investigated using an in‑situ NMR strategy that provides information on the time-evolution of the reaction and crystallization process. In our in‑situ NMR study of MFM-500(Ni) formation, liquid-phase 1H NMR data recorded as a function of time at 5 fixed temperatures afford qualitative information on the solution-phase processes and quantitative information on the kinetics of crystallization, allowing the activation energies for nucleation and growth to be determined. Ex-situ SAXS studies provide complementary nanoscale information on the rapid self-assembly prior to MOF crystallization and in-situ powder X-ray diffraction confirms that the only crystalline phase present during the reaction is phase-pure MFM-500(Ni).

An in situ and ex situ TEM study of the formation of thin cobalt silicide films by molecular beam epitaxy on the silicon (100) surface

1988 ◽  
Vol 46 ◽  
pp. 884-885
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove ◽  
R. T. Tung
Keyword(s):  
Molecular Beam Epitaxy ◽  
Molecular Beam ◽  
Defect Density ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Metal Base ◽  
In Situ Experiments ◽  
Potential Applications

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.

The use of transmission and analytical electron microscopy in studying reactions and phase transformations in thin film

1993 ◽  
Vol 51 ◽  
pp. 842-843
Author(s):  
K. Barmak
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Phase Transformations ◽  
Analytical Electron Microscopy ◽  
Ex Situ ◽  
Multilayer Thin Films ◽  
Absolute Concentration ◽  
Analytical Electron ◽  
Deposition Step

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.

Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

1989 ◽  
Vol 47 ◽  
pp. 462-463
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Diffraction ◽  
High Vacuum ◽  
High Energy ◽  
Energy Electron ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Transmission Electron

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.

Atomic Layer Deposition of LiF and Lithium Ion Conducting (AlF3)(LiF)x Alloys Using Trimethylaluminum, Lithium Hexamethyldisilazide and Hydrogen Fluoride

2017 ◽  
Author(s):  
Younghee Lee ◽  
Daniela M. Piper ◽  
Andrew S. Cavanagh ◽  
Matthias J. Young ◽  
Se-Hee Lee ◽  
...  
Keyword(s):  
Lithium Ion ◽  
Atomic Layer ◽  
Mass Gain ◽  
Alloy Film ◽  
Ex Situ ◽  
X Ray ◽  
Layer Deposition ◽  
Ion Conducting ◽  
Good Agreement

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH<sub>3</sub>)<sub>3</sub> as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF<sub>3</sub> and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF<sub>3</sub>)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film was measured as σ = 7.5 × 10<sup>-6</sup> S/cm.</div>

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