Self-Propagation Low Temperature Flameless Combustion Synthesis of Ni and Al Nanoparticles: Time-Resolved XRD Study

2014 ◽  
Vol 91 ◽  
pp. 1-6
Author(s):  
Yu.M. Mikhailov ◽  
V.V. Aleshin ◽  
A.M. Kolesnikova ◽  
D.Yu. Kovalev ◽  
V.I. Ponomarev

The combustion of cellulose nitrate (NC) in ballasted mixtures containing an organic binder and nickel hydroxycarbonate (NiOHCO3) or silver carbonate (Ag2CO3) as precursors has been found to produce Ni or Ag nanoparticles. Formation of Ni and Ag nanoparticles in the wave of flameless combustion of NC was monitored by the time-resolved X-Ray diffraction (TRXRD) method. During the formation of the Ag nanoparticles, the diffraction patterns exhibited only signals from decreasing amounts of the precursor and newly simultaneously formed 20-30 nm silver particles. It has been detected that in the systems with NiOHCO3the formation of the Ni 5-10 nm crystals proceeded via some 2-3 seconds diffraction-silent intermediate state of the whole system.

2014 ◽  
Vol 40 (1) ◽  
pp. 88-94 ◽  
Author(s):  
Yurii M. Mikhailov ◽  
Victor V. Aleshin ◽  
Alexandra M. Kolesnikova ◽  
Dmitrii Yu. Kovalev ◽  
Vasilii. I. Ponomarev

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 990
Author(s):  
Fatemeh Nikkhou ◽  
Fang Xia ◽  
Xizhi Yao ◽  
Idowu A. Adegoke ◽  
Qinfen Gu ◽  
...  

A flow-through reaction cell has been developed for studying minerals leaching by in-situ time-resolved powder X-ray diffraction, allowing for a better understanding of the leaching mechanisms and kinetics. The cell has the capability of independent control of temperature (up to 95 °C) and flow rate (>0.5 mL min−1) for atmospheric pressure leaching. It was successfully tested at the powder diffraction beamline at the Australian Synchrotron. Galena powder was leached in a citrate solution under flow-through condition at a flow rate of 0.5 mL min−1, while diffraction patterns were collected during the entire leaching process, showing rapid galena dissolution without the formation of secondary mineral phases. The flow-through cell can be used to study leaching processes of other ore minerals.


2014 ◽  
Vol 369 (1647) ◽  
pp. 20130325 ◽  
Author(s):  
John C. H. Spence ◽  
Nadia A. Zatsepin ◽  
Chufeng Li

The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested.


2001 ◽  
Vol 19 (1) ◽  
pp. 125-131 ◽  
Author(s):  
KENICHI KINOSHITA ◽  
HIDEKI HARANO ◽  
KOJI YOSHII ◽  
TAKERU OHKUBO ◽  
ATSUSHI FUKASAWA ◽  
...  

For ultrafast material analyses, we constructed the time-resolved X-ray diffraction system utilizing ultrashort X-rays from laser-produced plasma generated by the 12-TW–50-fs laser at the Nuclear Engineering Research Laboratory. Ultrafast transient changes in laser-irradiated GaAs crystals were observed as X-ray diffraction patterns. Experimental results were compared with numerical analyses.


Author(s):  
Carlo Knupp ◽  
Edward Morris ◽  
John M. Squire

Unlike electron microscopy, which can achieve very high resolutions, but to date can only be used to study static structures, time-resolved X-ray diffraction from contracting muscles can, in principle, be used to follow the molecular movements involved in force generation on a millisecond timescale albeit at moderate resolution. However, previous X-ray diffraction studies of resting muscles have come up with structures for the head arrangements in resting myosin filaments that are different from the apparently ubiquitous interacting heads motif (IHM) found by single particle analysis of electron micrographs of isolated myosin filaments from a variety of muscle types. This head organization is supposed to represent the super-relaxed state of the myosin filaments where ATP usage is minimized. Here we have tested whether the interacting heads motif structures will satisfactorily explain the observed low-angle X-ray diffraction patterns from resting vertebrate (bony fish) and invertebrate (insect flight) muscles. We find that the interacting heads motif does not, in fact, explain what is observed. Previous X-ray models fit the observations much better. We conclude that the X-ray diffraction evidence has been well interpreted in the past and that there is more than one ordered myosin head state in resting muscle. There is, therefore, no reason to question some of the previous X-ray diffraction results on myosin filaments; time-resolved X-ray diffraction should be a reliable way to follow crossbridge action in active muscle and may be one of the few ways to follow molecular changes in myosin heads on a millisecond timescale as force is actually produced.


1987 ◽  
Vol 01 (07n08) ◽  
pp. 289-293 ◽  
Author(s):  
WANG HUAQIN ◽  
ZHANG SHIYUAN ◽  
JIN TONGZHENG ◽  
HAN SHIYING ◽  
QIU DIRONG ◽  
...  

In this paper the differences in diffraction intensities from some crystal planes in the X-ray diffraction patterns of high Tc Y-Ba-Cu-O system superconductors prepared by different processing conditions and the difference among various structure cells in references are interpreted using computer fitting. The results suggest that there exists two structure cells in the single phase YBa2Cu3O7−x samples. Both structure cells have the same crystal symmetry and almost the same lattice parameters, a=3.821Å, b=3.892Å and c=11.676Å, but the different distortion degree of Cu2-O plane. According to EPR spectra measured on the same samples, it is considered that the improvement of superconductivity for the samples prepared by two-step annealing in flowing oxygen may be related to concentration of the structure cell with more serious distortion on the Cu2-O plane.


2015 ◽  
Vol 177 ◽  
pp. 237-247 ◽  
Author(s):  
Kerry Simmance ◽  
Wouter van Beek ◽  
Gopinathan Sankar

Time resolved high-resolution X-ray powder diffraction was utilized to obtain detailed changes in the crystal structure parameters during the hydrothermal crystallization process of the nanoporous aluminophosphate AlPO-5 (AFI) structure. This in situ study offered not only the influence of metal ions on the onset of crystallization and estimation of the activation energy of the process, but also allowed us to determine in detail the changes in lattice parameters during this process. More importantly the time-resolved study clearly showed the lattice expansion in the divalent metal ions substituted system right from the on-set of crystallization process, compared to the one without any dopant ions, which suggest that an amorphous or poorly crystalline network is formed prior to crystallization that contains the large divalent ions (compared to Al(iii), the substituting element), which is in agreement with the combined XAS/XRD study reported earlier. A mechanism based on this and the earlier study is suggested.


2004 ◽  
Vol 22 (3) ◽  
pp. 285-288 ◽  
Author(s):  
KAZUTAKA G. NAKAMURA ◽  
YOICHIRO HIRONAKA ◽  
HIDETAKA KAWANO ◽  
HIROAKI KISHIMURA ◽  
KEN-ICHI KONDO

Ultrashort pulsed hard X rays are generated by focusing an intense femtosecond laser beam onto metal targets. Kαemissions are obtained from a Cu target. Picosecond time-resolved X-ray diffraction is performed to investigate structural dynamics of laser-shocked semiconductors using the laser plasma X-ray pulses. Lattice deformation associated with shock-wave propagation is directly observed. Evolution of strain profiles inside the crystal is determined without disturbance from the time-resolved X-ray diffraction patterns.


2018 ◽  
Vol 3 (4) ◽  
pp. 36 ◽  
Author(s):  
Angelo Mullaliu ◽  
Paolo Conti ◽  
Giuliana Aquilanti ◽  
Jasper Plaisier ◽  
Lorenzo Stievano ◽  
...  

The reversible electrochemical lithiation of potassium iron hexacyanocobaltate (FeCo) was studied by operando X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) assisted by chemometric techniques. In this way, it was possible to follow the system dynamics and retrieve structural and electronic transformations along cycling at both Fe and Co sites. These analyses confirmed that FeCo features iron as the main electroactive site. Even though the release of potassium ions causes a local disorder around the iron site, the material exhibits an excellent structural stability during the alkali ion deinsertion/insertion processes. An independent but interrelated analysis approach offers a good strategy for data treatment and provides a time-resolved picture of the studied system.


Time-resolved crystallography is founded on the belief that a complete understanding of mechanism at the molecular level demands knowledge, not just of long-lived, readily observable structures, but also of short-lived intermediates in processes such as catalysis, ligand binding and release, and protein unfolding. Synchrotron X-ray sources enable X -ray diffraction patterns of high quality to be obtained from single crystals with exposure times that are often commensurate with the lifetime of the desired intermediates. The basic tools are therefore in place. How shall they be applied effectively? Can crystallography, long regarded as a static technique, in fact encompass dynamic processes? What pitfalls remain to be overcome? A time-resolved crystallographic experiment has five main components: the X -ray source; reaction initiation; reaction monitoring by optical or other techniques; X-ray data acquisition in real time; and data reduction and analysis. These are illustrated by our recent work on photoactive yellow protein, and on the acquisition and analysis of crystallographic data using 120 ps exposures.


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