Real time In Situ X-Ray Topographic Observation of Deformation of Single Crystals and Thin Films

1998 ◽  
Vol 524 ◽  
Author(s):  
Z. B. Zhao ◽  
J. Hershberger ◽  
A. Chiaramonti ◽  
Z. U. Rek ◽  
J. C. Bilello
Keyword(s):  
Real Time ◽  
X Ray ◽  
Mechanical Cycling ◽  
Experimental Apparatus ◽  
Tensile Data ◽  
Deformation Behaviors ◽  
Deformation Processes ◽  
Increasing Temperature ◽  
Increasing Load

ABSTRACTAn experimental apparatus, which is capable of performing real time in situ X-ray topographic observation of deformation process via synchrotron white beam topography, has been developed. This device enables both tensile data (load-displacement) and topographic images to be recorded simultaneously. It has been utilized to study the deformation behaviors of crystals of Mo and W.These specimens have been subject to mechanical cycling with increasing load, and their deformation processes have been observed in real time and in situ via x-ray topography. This leads to the observation of several phenomena, which would have been difficult to reveal by other experimental techniques. They include stress concentration, microyielding, reversible variation of contrasts and stress relaxation. In addition, the deformation behaviors of small angle grain boundaries have also been examined. Furthermore, the specimens can be heated through a heating device attached to the tensile stage, which allows high temperature topography to be performed in real time. The technique has been applied to the Ta films on Si (100) substrates. With increasing temperature, the topographic observations have revealed that the Ta films yield, fracture and then proceed to delaminate from their substrates.

Real Time Observation of Material Deformation Processes by Synchrotron White Beam X-ray Topography

1997 ◽  
Vol 502 ◽  
Author(s):  
Z. B. Zhao ◽  
J. Hershberger ◽  
Z. U. Rek ◽  
J. C. Bilello
Keyword(s):  
Single Crystals ◽  
Real Time ◽  
High Strength ◽  
X Ray ◽  
White Beam ◽  
Experimental Apparatus ◽  
Tensile Data ◽  
Deformation Processes ◽  
Time Observation ◽  
The Stability

ABSTRACTAn experimental apparatus which exploits synchrotron white beam X-ray diffraction topography has been developed to perform real time in situ observation of deformation processes of single crystals. The apparatus consists of a fully automated and remotely controlled mini-tensile device and a CCD based X-ray imaging detector with associated video system. Both tensile data and X-ray topographic images are recorded simultaneously. The materials under study include single crystals of Si, and single crystals or bicrystals of the refractory metals W and Mo. The deformation processes of these crystals have been studied by monitoring a selected transmission Laue spot while the specimen is mechanically cycled by loading and unloading. The X-ray images have been captured by a frame grabber and recorded via a VCR. Several phenomena have been observed, including bending contours, strain concentrations, reversible anelastic effect and microyielding. The observed stress relaxations are correlated to microstructural variations shown by X-ray topography. The stability of low angle grain boundaries in bicrystals; and the effect of high strength and toughness coatings on the deformation of single crystal substrates was investigated.

Kinetics of Ion-Exchange Reactions in Hybrid Organic–Inorganic Perovskite Thin Films Studied by In Situ Real-Time X-ray Scattering

2018 ◽  
Vol 9 (23) ◽  
pp. 6750-6754 ◽  
Author(s):  
Alessandro Greco ◽  
Alexander Hinderhofer ◽  
M. Ibrahim Dar ◽  
Neha Arora ◽  
Jan Hagenlocher ◽  
...  
Keyword(s):  
Thin Films ◽  
Ion Exchange ◽  
Real Time ◽  
Exchange Reactions ◽  
Inorganic Perovskite ◽  
X Ray ◽  
X Ray Scattering ◽  
Kinetics Of ◽  
Kinetics Of Ion Exchange

scholarly journals Tracking Metamorphic Dehydration Reactions in Real Time with Transmission Small- and Wide-Angle Synchrotron X-ray Scattering: the Case of Gypsum Dehydration

2020 ◽  
Vol 61 (6) ◽  
Author(s):  
C E Schrank ◽  
K Gioseffi ◽  
T Blach ◽  
O Gaede ◽  
A Hawley ◽  
...  
Keyword(s):  
Real Time ◽  
Wide Angle ◽  
Length Scales ◽  
X Ray ◽  
Rock Samples ◽  
X Ray Scattering ◽  
Dehydration Reactions ◽  
The Impact ◽  
Ray Scattering

Abstract We present a review of a unique non-destructive method for the real-time monitoring of phase transformations and nano-pore evolution in dehydrating rocks: transmission small- and wide-angle synchrotron X-ray scattering (SAXS/WAXS). It is shown how SAXS/WAXS can be applied to investigating rock samples dehydrated in a purpose-built loading cell that allows the coeval application of high temperature, axial confinement, and fluid pressure or flow to the specimen. Because synchrotron sources deliver extremely bright monochromatic X-rays across a wide energy spectrum, they enable the in situ examination of confined rock samples with thicknesses of ≤ 1 mm at a time resolution of order seconds. Hence, fast kinetics with reaction completion times of about hundreds of seconds can be tracked. With beam sizes of order tens to hundreds of micrometres, it is possible to monitor multiple interrogation points in a sample with a lateral extent of a few centimetres, thus resolving potential lateral spatial effects during dehydration and enlarging sample statistics significantly. Therefore, the SAXS/WAXS method offers the opportunity to acquire data on a striking range of length scales: for rock samples with thicknesses of ≤ 10-3 m and widths of 10-2 m, a lateral interrogation-point spacing of ≥ 10-5 m can be achieved. Within each irradiated interrogation-point volume, information concerning pores with sizes between 10-9 and 10-7 m and the crystal lattice on the scale of 10-10 m is acquired in real time. This article presents a summary of the physical principles underpinning transmission X-ray scattering with the aim of providing a guide for the design and interpretation of time-resolved SAXS/WAXS experiments. It is elucidated (1) when and how SAXS data can be used to analyse total porosity, internal surface area, and pore-size distributions in rocks on length scales from ∼1 to 300 nm; (2) how WAXS can be employed to track lattice transformations in situ; and (3) which limitations and complicating factors should be considered during experimental design, data analysis, and interpretation. To illustrate the key capabilities of the SAXS/WAXS method, we present a series of dehydration experiments on a well-studied natural gypsum rock: Volterra alabaster. Our results demonstrate that SAXS/WAXS is excellently suited for the in situ tracking of dehydration kinetics and the associated evolution of nano-pores. The phase transformation from gypsum to bassanite is correlated directly with nano-void growth on length scales between 1 and 11 nm for the first time. A comparison of the SAXS/WAXS kinetic results with literature data emphasises the need for future dehydration experiments on rock specimens because of the impact of rock fabric and the generally heterogeneous and transient nature of dehydration reactions in nature. It is anticipated that the SAXS/WAXS method combined with in situ loading cells will constitute an invaluable tool in the ongoing quest for understanding dehydration and other mineral replacement reactions in rocks quantitatively.

Carbonate-cancrinite: In-situ real-time thermal processes studied by means of energy-dispersive X-ray powder-diffractometry

1995 ◽  
Vol 10 (3) ◽  
pp. 173-177 ◽  
Author(s):  
P. Ballirano ◽  
A. Maras ◽  
R. Caminiti ◽  
C. Sadun
Keyword(s):  
Real Time ◽  
Room Temperature ◽  
Rietveld Analysis ◽  
Molecular Water ◽  
Heating Process ◽  
Thermal Processes ◽  
X Ray ◽  
Reversible Phase Transition ◽  
Reversible Phase

New powder X-ray data for cancrinite [ideally Na8Si6Al6O24 (CO3)2·2 H2O] are reported along with in-situ real-time thermal processes recorded using energy dispersive X-ray diffractometry (EDXD). A completely anhydrous phase is obtained after heating the sample up to 600 °C and quickly cooling it to room temperature, as shown by means of both Rietveld analysis and IR spectroscopy. The anhydrous phase does not show any tendency to re-acquire molecular water. During the heating process, at around 450 °C, a peak splitting is observed, possibly due to a reversible phase transition.

Dynamics of the nanocrystal structure and composition in growth solutions monitored by in situ lab-scale X-ray diffraction

Nanoscale ◽  
2021 ◽  
Author(s):  
Helena Fridman ◽  
Michael Volokh ◽  
Taleb Mokari
Keyword(s):  
Real Time ◽  
Growth Dynamics ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nanocrystal Growth ◽  
Novel Approach ◽  
Phase Size ◽  
Time Observation ◽  
Real Time Observation

Nanocrystal growth dynamics are investigated by a novel approach: real-time observation of nanocrystals in growth solutions using lab-scale in situ X-ray diffraction. The method reveals the evolution of crystal phase, size, shape, and composition.

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.

scholarly journals Mechanisms of mechanochemical salt formation by in situ real time X-ray powder diffraction

2016 ◽  
Vol 72 (a1) ◽  
pp. s394-s394
Author(s):  
Adam A. L. Michalchuk ◽  
Ivan A. Tumanov ◽  
Simon A. J. Kimber ◽  
Elena V. Boldyreva ◽  
Colin R. Pulham
Keyword(s):  
Real Time ◽  
Powder Diffraction ◽  
Salt Formation ◽  
X Ray

scholarly journals Inside Back Cover: Real-Time In Situ Powder X-ray Diffraction Monitoring of Mechanochemical Synthesis of Pharmaceutical Cocrystals (Angew. Chem. Int. Ed. 44/2013)

2013 ◽  
Vol 52 (44) ◽  
pp. 11665-11665
Author(s):  
Ivan Halasz ◽  
Andreas Puškarić ◽  
Simon A. J. Kimber ◽  
Patrick J. Beldon ◽  
Ana M. Belenguer ◽  
...  
Keyword(s):  
Real Time ◽  
Mechanochemical Synthesis ◽  
X Ray Diffraction ◽  
Pharmaceutical Cocrystals ◽  
X Ray ◽  
Back Cover

In situ and real-time monitoring of mechanochemical milling reactions using synchrotron X-ray diffraction

2013 ◽  
Vol 8 (9) ◽  
pp. 1718-1729 ◽  
Author(s):  
Ivan Halasz ◽  
Simon A J Kimber ◽  
Patrick J Beldon ◽  
Ana M Belenguer ◽  
Frank Adams ◽  
...  
Keyword(s):  
Real Time ◽  
X Ray Diffraction ◽  
Real Time Monitoring ◽  
X Ray ◽  
Mechanochemical Milling
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