Quick X-ray reflectivity using monochromatic synchrotron radiation for time-resolved applications

A new technique for the parallel collection of X-ray reflectivity (XRR) data, compatible with monochromatic synchrotron radiation and flat substrates, is described and applied to thein situobservation of thin-film growth. The method employs a polycapillary X-ray optic to produce a converging fan of radiation, incident onto a sample surface, and an area detector to simultaneously collect the XRR signal over an angular range matching that of the incident fan. Factors determining the range and instrumental resolution of the technique in reciprocal space, in addition to the signal-to-background ratio, are described in detail. This particular implementation records ∼5° in 2θ and resolves Kiessig fringes from samples with layer thicknesses ranging from 3 to 76 nm. The value of this approach is illustrated by showingin situXRR data obtained with 100 ms time resolution during the growth of epitaxial La0.7Sr0.3MnO3on SrTiO3by pulsed laser deposition at the Cornell High Energy Synchrotron Source (CHESS). Compared with prior methods for parallel XRR data collection, this is the first method that is both sample-independent and compatible with the highly collimated, monochromatic radiation typical of third-generation synchrotron sources. Further, this technique can be readily adapted for use with laboratory-based sources.

Download Full-text

Microstructure Evolution during Thermal Processing : Insight from In-Situ Time-Resolved Synchrotron Radiation Experiments

Materials Science Forum ◽

10.4028/www.scientific.net/msf.550.607 ◽

2007 ◽

Vol 550 ◽

pp. 607-612

Author(s):

J. Bednarčík ◽

R. Nicula ◽

Karel Saksl ◽

M. Stir ◽

E. Burkel

Keyword(s):

Synchrotron Radiation ◽

Thermal Processing ◽

Applied Pressure ◽

High Energy ◽

Coarse Grained ◽

Microstructure Development ◽

Time Resolved ◽

Nanostructured Alloys ◽

X Ray

The magnetic, mechanical or chemical properties of nanocrystalline materials strongly differ from the ones of their coarse-grained counterparts. Moreover, significant changes of the phase diagrams were already evidenced for nanostructured alloys. Thermal processing with or without applied pressure controls the microstructure development at the nanometer scale and thus essentially decides upon the final nanomaterial behaviour and properties. A common route for the synthesis of metallic nanomaterials is the devitrification of amorphous precursors obtained via non-equilibrium processing, e.g. by rapid solidification or high-energy ball-milling. Time-resolved in-situ X-ray diffraction experiments may nowadays be performed at high-brilliance synchrotron radiation sources for a variety of temperature-pressure conditions. The temperature-time evolution of the grain-size distribution and microstrain can be monitored in detail at specimen-relevant scales. Together with local information from electron microscopy and chemical analysis, in-situ X-ray experiments offer a complete set of tools for engineering of the microstructure in nanomaterials. The effect of individual processing steps can be distinguished clearly and further tuned. An example is provided, concerning the high-temperature microstructure development in Co-rich soft magnetic nanostructured alloys.

Download Full-text

X-ray reflectivity with a twist: Quantitative time-resolved X-ray reflectivity using monochromatic synchrotron radiation

Applied Physics Letters ◽

10.1063/1.5085063 ◽

2019 ◽

Vol 114 (8) ◽

pp. 081904 ◽

Cited By ~ 1

Author(s):

Howie Joress ◽

Shane Q. Arlington ◽

Timothy P. Weihs ◽

Joel D. Brock ◽

Arthur R. Woll

Keyword(s):

Synchrotron Radiation ◽

Time Resolved ◽

X Ray ◽

Monochromatic Synchrotron

Download Full-text

A large-solid-angle X-ray Raman scattering spectrometer at ID20 of the European Synchrotron Radiation Facility

Journal of Synchrotron Radiation ◽

10.1107/s1600577516020579 ◽

2017 ◽

Vol 24 (2) ◽

pp. 521-530 ◽

Cited By ~ 46

Author(s):

S. Huotari ◽

Ch. J. Sahle ◽

Ch. Henriquet ◽

A. Al-Zein ◽

K. Martel ◽

...

Keyword(s):

Synchrotron Radiation ◽

Raman Scattering ◽

Solid Angle ◽

European Synchrotron Radiation Facility ◽

Electronic Excitations ◽

Raman Scattering Spectroscopy ◽

X Ray ◽

Area Detector ◽

Spectroscopic Tool

An end-station for X-ray Raman scattering spectroscopy at beamline ID20 of the European Synchrotron Radiation Facility is described. This end-station is dedicated to the study of shallow core electronic excitations using non-resonant inelastic X-ray scattering. The spectrometer has 72 spherically bent analyzer crystals arranged in six modular groups of 12 analyzer crystals each for a combined maximum flexibility and large solid angle of detection. Each of the six analyzer modules houses one pixelated area detector allowing for X-ray Raman scattering based imaging and efficient separation of the desired signal from the sample and spurious scattering from the often used complicated sample environments. This new end-station provides an unprecedented instrument for X-ray Raman scattering, which is a spectroscopic tool of great interest for the study of low-energy X-ray absorption spectra in materials under in situ conditions, such as in operando batteries and fuel cells, in situ catalytic reactions, and extreme pressure and temperature conditions.

Download Full-text

Time-Resolved X-Ray Studies During Pulsed-Laser Irradiation of Ge

MRS Proceedings ◽

10.1557/proc-35-119 ◽

1984 ◽

Vol 35 ◽

Author(s):

J.Z. Tischler ◽

B.C. Larson ◽

D.M. Mills

Keyword(s):

Melting Point ◽

Laser Irradiation ◽

Pulsed Laser ◽

Laser Pulses ◽

High Energy ◽

Measured Temperature ◽

Time Resolved ◽

Synchrotron Source ◽

X Ray ◽

Pulsed Laser Irradiation

ABSTRACTSynchrotron x-ray pulses from the Cornell High Energy Synchrotron Source (CHESS) have been used to carry out nanosecond resolution measurements of the temperature distrubutions in Ge during UV pulsed-laser irradiation. KrF (249 nm) laser pulses of 25 ns FWHM with an energy density of 0.6 J/cm2 were used. The temperatures were determined from x-ray Bragg profile measurements of thermal expansion induced strain on <111> oriented Ge. The data indicate the presence of a liquid-solid interface near the melting point, and large (1500-4500°C/pm) temperature gradients in the solid; these Ge results are analagous to previous ones for Si. The measured temperature distributions are compared with those obtained from heat flow calculations, and the overheating and undercooling of the interface relative to the equilibrium melting point are discussed.

Download Full-text

In Situ Stress Tensor Determination during Phase Transformation of a Metal Matrix Composite by High-Energy X-ray Diffraction

Materials ◽

10.3390/ma11081415 ◽

2018 ◽

Vol 11 (8) ◽

pp. 1415 ◽

Cited By ~ 4

Author(s):

Guillaume Geandier ◽

Lilian Vautrot ◽

Benoît Denand ◽

Sabine Denis

Keyword(s):

Phase Transformation ◽

Stress Tensor ◽

Metal Matrix Composite ◽

Matrix Composite ◽

Metal Matrix ◽

High Energy ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray

In situ high-energy X-ray diffraction using a synchrotron source performed on a steel metal matrix composite reinforced by TiC allows the evolutions of internal stresses during cooling to be followed thanks to the development of a new original experimental device (a transportable radiation furnace with controlled rotation of the specimen). Using the device on a high-energy beamline during in situ thermal treatment, we were able to extract the evolution of the stress tensor components in all phases: austenite, TiC, and even during the martensitic phase transformation of the matrix.

Download Full-text