In-situ X-ray and visual observation of foam morphology and behavior at the batch-melt interface during melting of simulated waste glass

ABSTRACTIn order to design a scheme to monitor the state of preservation of iron alloys that are found on historic shipwrecks sunk in fresh water, it was first necessary to identify the predominant form of corrosion found on the wrecks. This was done by visual observation, in situ surface pH measurements, and X-ray powder diffraction of the corrosion layers. Once the form of corrosion was identified as pitting corrosion, a monitoring scheme based on photographic recording of the rust-red tubercles was designed. This scheme is simple and nondestructive, both necessary characteristics for the monitoring of submerged historic resources.

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The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071107 ◽

1973 ◽

Vol 31 ◽

pp. 132-133 ◽

Cited By ~ 1

Author(s):

R. E. Herfert

Keyword(s):

Surface Characterization ◽

Analytical Techniques ◽

X Ray Diffraction ◽

Depth Of Penetration ◽

X Ray ◽

The Past ◽

Transmission Electron ◽

Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

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In Situ X-Ray Absorption Studies of the Electrochemical Reduction of Hydroxocobalamin

Journal de Physique IV (Proceedings) ◽

10.1051/jp4/1997116 ◽

1997 ◽

Vol 7 (C2) ◽

pp. C2-619-C2-620 ◽

Cited By ~ 1

Author(s):

M. Giorgett ◽

I. Ascone ◽

M. Berrettoni ◽

S. Zamponi ◽

R. Marassi

Keyword(s):

Electrochemical Reduction ◽

X Ray ◽

Absorption Studies ◽

X Ray Absorption

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In-situ investigation by X-ray diffraction and wafer curvature of phase formation and stress evolution during metal thin film – silicon reactions

Zeitschrift für Kristallographie Supplements ◽

10.1524/zksu.2007.2007.suppl_26.81 ◽

2007 ◽

Vol 2007 (suppl_26) ◽

pp. 81-89

Author(s):

O. Thomas

Keyword(s):

Thin Film ◽

Phase Formation ◽

Stress Evolution ◽

X Ray Diffraction ◽

X Ray ◽

Wafer Curvature ◽

Thin Film Silicon ◽

Metal Thin Film ◽

In Situ Investigation

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A Revised O2 Reduction Model in Li-O2 Batteries as Revealed by in Situ Small Angle X-Ray Scattering

10.26434/chemrxiv.11447775.v1 ◽

2019 ◽

Author(s):

Christian Prehal ◽

Aleksej Samojlov ◽

Manfred Nachtnebel ◽

Manfred Kriechbaum ◽

Heinz Amenitsch ◽

...

Keyword(s):

Small Angle ◽

Wide Angle ◽

Reduction Mechanism ◽

Reduction Model ◽

X Ray ◽

X Ray Scattering ◽

O2 Reduction ◽

Ray Scattering

Here we use in situ small and wide angle X-ray scattering to elucidate unexpected mechanistic insights of the O2 reduction mechanism in Li-O2 batteries.

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Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

10.26434/chemrxiv.11345063.v2 ◽

2020 ◽

Author(s):

Keishiro Yamashita ◽

Kazuki Komatsu ◽

Hiroyuki Kagi

Keyword(s):

Crystal Structure ◽

High Pressure ◽

Crystal Growth ◽

Single Crystal ◽

Room Temperature ◽

Growth Technique ◽

Salt Hydrate ◽

X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl2·7H2O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

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Monitoring Polymer-Assisted Mechanochemical Cocrystallisation Through in Situ X-Ray Powder Diffraction

10.26434/chemrxiv.11996589.v1 ◽

2020 ◽

Author(s):

Luzia S. Germann ◽

Sebastian T. Emmerling ◽

Manuel Wilke ◽

Robert E. Dinnebier ◽

Mariarosa Moneghini ◽

...

Keyword(s):

Molecular Weight ◽

Powder Diffraction ◽

Reaction Rate ◽

Polymer Additives ◽

Time Resolved ◽

X Ray

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the monitoring of polymer-assisted grinding reactions using in situ X-ray powder diffraction, revealing that reaction rate is almost double compared to neat grinding and independent of the molecular weight and amount of used polymer additives.

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

10.26434/chemrxiv.5459653 ◽

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 (AlF3)(LiF)x 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/(cm2 cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH3)3 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/(cm2 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 AlF3 and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF3)(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 (AlF3)(LiF)x 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 (AlF3)(LiF)x alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF3)(LiF)x alloy film was measured as σ = 7.5 × 10-6 S/cm.</div>

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In situ Time-Resolved Small-Angle X-ray Scattering Reveals the Formation Kinetics of Polyelectrolyte Complex Micelles

10.26434/chemrxiv.9876395.v1 ◽

2019 ◽

Author(s):

Hao Wu ◽

Jeffrey Ting ◽

Siqi Meng ◽

Matthew Tirrell

Keyword(s):

Small Angle ◽

Self Assembly ◽

Electrostatic Interactions ◽

Polyelectrolyte Complex ◽

Time Resolved ◽

X Ray ◽

X Ray Scattering ◽

Kinetics Of ◽

Ray Scattering

We have directly observed the in situ self-assembly kinetics of polyelectrolyte complex (PEC) micelles by synchrotron time-resolved small-angle X-ray scattering, equipped with a stopped-flow device that provides millisecond temporal resolution. This work has elucidated one general kinetic pathway for the process of PEC micelle formation, which provides useful physical insights for increasing our fundamental understanding of complexation and self-assembly dynamics driven by electrostatic interactions that occur on ultrafast timescales.

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