X-Ray Dynamical Diffraction in Powder Samples with Time-Dependent Particle Size Distributions

MRS Advances ◽  
2019 ◽  
Vol 5 (29-30) ◽  
pp. 1585-1591 ◽  
Author(s):  
Adriana Valério ◽  
Sérgio L. Morelhão ◽  
Alex J. Freitas Cabral ◽  
Márcio M. Soares ◽  
Cláudio M. R. Remédios
Keyword(s):  
Particle Size ◽  
Single Phase ◽  
Diffraction Peak ◽  
Time Dependent ◽  
Peak Width ◽  
Dynamical Diffraction ◽  
X Ray ◽  
Integrated Intensity ◽  
Diffraction Effects

ABSTRACTIn situ X-ray diffraction is one of the most useful tools for studying a variety of processes, among which crystallization of nanoparticles where phase purity and size control are desired. Growth kinetics of a single phase can be completely resolved by proper analysis of the diffraction peaks as a function of time. The peak width provides a parameter for monitoring the time evolution of the particle size distribution (PSD), while the peak area (integrated intensity) is directly related to the whole diffracting volume of crystallized material in the sample. However, to precisely describe the growth kinetics in terms of nucleation and coarsening, the correlation between PSD parameters and diffraction peak widths has to be established in each particular study. Corrections in integrated intensity values for physical phenomena such as variation in atomic thermal vibrations and dynamical diffraction effects have also to be considered in certain cases. In this work, a general correlation between PSD median value and diffraction peak width is deduced, and a systematic procedure to resolve time-dependent lognormal PSDs from in situ XRD experiments is described in details. A procedure to correct the integrated intensities for dynamical diffraction effects is proposed. As a practical demonstration, this analytical procedure has been applied to the single-phase crystallization process of bismuth ferrite nanoparticles.

scholarly journals X-Ray Dynamical Diffraction in Powder Samples with Time-Dependent Particle Size Distributions - ADDENDUM

MRS Advances ◽  
2020 ◽  
Vol 5 (29-30) ◽  
pp. 1623-1623
Author(s):  
Adriana Valério ◽  
Sérgio L. Morelhão ◽  
Alex J. Freitas Cabral ◽  
Márcio M. Soares ◽  
Cláudio M. R. Remédios
Keyword(s):  
Particle Size ◽  
Time Dependent ◽  
Size Distributions ◽  
Particle Size Distributions ◽  
Dynamical Diffraction ◽  
X Ray ◽  
Powder Samples

scholarly journals The Change of X‐ray Diffraction Peak Width During in situ Conventional Sintering of Nanoscale Powders

2016 ◽  
Vol 99 (3) ◽  
pp. 765-768 ◽  
Author(s):  
Jean‐Marie Lebrun ◽  
Shikhar K. Jha ◽  
Kiran S. Naik ◽  
Kevin C. Seymour ◽  
Waltraud M. Kriven ◽  
...  
Keyword(s):  
Diffraction Peak ◽  
Peak Width ◽  
X Ray Diffraction ◽  
X Ray ◽  
Conventional Sintering ◽  
Diffraction Peak Width

scholarly journals X-Ray Tomography Study on Porosity and Particle Size Distribution in In Situ Al-4.5Cu-5TiB2 Semisolid Rolled Composites

JOM ◽  
2019 ◽  
Vol 71 (11) ◽  
pp. 4050-4058 ◽  
Author(s):  
Swapnil Morankar ◽  
Monalisa Mandal ◽  
Nadia Kourra ◽  
Mark A. Williams ◽  
Rahul Mitra ◽  
...  
Keyword(s):  
Particle Size ◽  
Particle Size Distribution ◽  
Size Distribution ◽  
X Ray

scholarly journals Real-time synthesis and detection of plasmonic metal (Au, Ag) nanoparticles under monochromatic X-ray nano-tomography

2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Amardeep Bharti ◽  
Keun Hwa Chae ◽  
Navdeep Goyal
Keyword(s):  
Particle Size ◽  
Real Time ◽  
Reduction Process ◽  
Localized Surface Plasmon ◽  
Plasmonic Nanostructures ◽  
X Rays ◽  
X Ray ◽  
The Real ◽  
Size And Shape

AbstractPlasmonic nanostructures are of immense interest of research due to its widespread applications in microelectronics, photonics, and biotechnology, because of its size and shape-dependent localized surface plasmon resonance response. The great efforts have been constructed by physicists, chemists, and material scientists to deliver optimized reaction protocol to tailor the size and shape of nanostructures. Real-time characterization emerges out as a versatile tool in perspective to the optimization of synthesis parameters. Moreover, in the past decades, radiation-induced reduction of metallic-salt to nanoparticles dominates over the conventional direct chemical reduction process which overcomes the production of secondary products and yields ultra-high quality and pure nanostructures. Here we show, the real-time/in-situ synthesis and detection of plasmonic (Au andAg) nanoparticles using single synchrotron monochromatic 6.7 keV X-rays based Nano-Tomography beamline. The real-time X-ray nano-tomography of plasmonic nanostructures has been first-time successfully achieved at such a low-energy that would be leading to the possibility of these experiments at laboratory-based sources. In-situ optical imaging confirms the radiolysis of water molecule resulting in the production of $$e_{aq}^-,\,OH^\bullet ,$$ e aq - , O H ∙ , and $$O_2^-$$ O 2 - under X-ray irradiation. The obtained particle-size and size-distribution by X-ray tomography are in good agreement to TEM results. The effect of different chemical environment media on the particle-size has also been studied. This work provides the protocol to precisely control the size of nanostructures and to synthesize the ultrahigh-purity grade monodisperse nanoparticles that would definitely enhance the phase-contrast in cancer bio-imaging and plasmonic photovoltaic application.

Experimental Evaluation of Peak Height Approximation for X-Ray Diffracted Integrated Intensity Method

1980 ◽  
Vol 24 ◽  
pp. 277-282
Author(s):  
Charles P. Gazzara
Keyword(s):  
Mathematical Description ◽  
Experimental Evaluation ◽  
Polycrystalline Material ◽  
Peak Height ◽  
Diffraction Peak ◽  
Characteristic Peak ◽  
Practical Solution ◽  
X Ray ◽  
Integrated Intensity ◽  
Overlapping Peaks

The mathematical description of an X-ray peak, diffracted from a powder or polycrystalline material, using physically meaningful parameters has been of interest for many years. With the popularity of computers, this need to characterize a diffraction peak has intensified.A key problem which persists is how to describe the instrumental diffracted profile and therefore the observed diffracted characteristic peak with subsequent combinations of Kα doublets and mixed overlapping peaks. Many attempts have been made at finding a “true“ function to fit the observed diffracted peak; however, a practical solution has yet to be found.

scholarly journals Preparation of Nanoparticles Including Antisolvent Drugs by the Combination of Roll Milling and High-pressure Homogenization

2018 ◽  
Vol 14 (2) ◽  
pp. 143-147 ◽  
Author(s):  
Seitaro Kamiya ◽  
Maya Yamada ◽  
Miki Washino ◽  
Kenichiro Nakashima
Keyword(s):  
Particle Size ◽  
High Pressure ◽  
Organic Solvent ◽  
Organic Solvents ◽  
Peak Shift ◽  
Diffraction Peak ◽  
High Pressure Homogenization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wet Process

Description: Design methods of nanoparticle formulations are divided into break-down methods and build-up methods. The former is further divided into dry and wet processes. For drug nanoparticle preparations, the wet process is generally employed, and organic solvents are used in most formulations. Method: In this study, we investigate the preparation of nifedipine (IB) and griseofulvin (GF) nanoparticles without using organic solvent. Both IB and GF nanoparticles, with a mean particle size of approximately 50 nm, were prepared without organic solvent by employing a combination of roll milling and high-pressure homogenization. Result: The X-ray diffraction peak of the IB and GF samples prepared by roll milling was present at a position (2θ) identical to that of IB and GF crystals, indicating that no peak shift was induced by interaction with phospholipids. Conclusion: These findings demonstrate that most IB and GF nanoparticles exist as crystals in phospholipids.

Nondestructive Imaging of Materials Microstructures Using X-Ray Tomographic Microscopy

1990 ◽  
Vol 217 ◽  
Author(s):  
J.H. Kinney ◽  
M.C. Nichols ◽  
U. Bonse ◽  
S.R. Stock ◽  
T.M. Breunig ◽  
...  
Keyword(s):  
High Resolution ◽  
Three Dimensional ◽  
Time Dependent ◽  
Materials Processing ◽  
Dependent Data ◽  
Inspection Method ◽  
Dimensional Inspection ◽  
X Ray ◽  
Nondestructive Imaging

ABSTRACTA technique for nondestructively imaging microstructures of materials in situ, especially a technique capable of delineating the time evolution of chemical changes or damage, will greatly benefit studies of materials processing and failure. X-ray tomographic microscopy (XTM) is a high resolution, three-dimensional inspection method which is capable of imaging composite materials microstructures with a resolution of a few micrometers. Because XTM is nondestructive, it will be possible to examine materials under load or during processing, and obtain three-dimensional images of fiber positions, microcracks, and pores. This will allow direct imaging of microstructural evolution, and will provide time-dependent data for comparison to fracture mechanics and processing models.

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