Advanced grazing-incidence techniques for modern soft-matter materials analysis

The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities forin situandin operandoGISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

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In situ investigation of annealing effect on lamellar stacking structure of polyethylene thin films by synchrotron grazing-incidence small-angle and wide-angle X-ray scattering

Journal of Applied Crystallography ◽

10.1107/s002188980700578x ◽

2007 ◽

Vol 40 (s1) ◽

pp. s642-s644 ◽

Cited By ~ 15

Author(s):

Sono Sasaki ◽

Hiroyasu Masunaga ◽

Hiroo Tajiri ◽

Katsuaki Inoue ◽

Hiroshi Okuda ◽

...

Keyword(s):

Thin Films ◽

Small Angle ◽

Grazing Incidence ◽

Annealing Effect ◽

Wide Angle ◽

X Ray ◽

X Ray Scattering ◽

In Situ Investigation ◽

Stacking Structure

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Functional materials analysis usingin situandin operandoX-ray and neutron scattering

IUCrJ ◽

10.1107/s2052252514026062 ◽

2015 ◽

Vol 2 (2) ◽

pp. 292-304 ◽

Cited By ~ 16

Author(s):

Vanessa K. Peterson ◽

Christine M. Papadakis

Keyword(s):

Neutron Scattering ◽

State Of The Art ◽

Functional Materials ◽

Materials Analysis ◽

X Ray ◽

Materials Research ◽

Recent Developments ◽

In Operando ◽

Types Of Information

In situandin operandostudies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-artin situandin operandoX-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them.

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Elucidating the Failure Mechanisms of Perovskite Solar Cells in Humid Environments Using In Situ Grazing-Incidence Wide-Angle X-ray Scattering

ACS Energy Letters ◽

10.1021/acsenergylett.8b01300 ◽

2018 ◽

Vol 3 (9) ◽

pp. 2127-2133 ◽

Cited By ~ 7

Author(s):

Kyle M. Fransishyn ◽

Soumya Kundu ◽

Timothy L. Kelly

Keyword(s):

Solar Cells ◽

Failure Mechanisms ◽

Perovskite Solar Cells ◽

Grazing Incidence ◽

Wide Angle ◽

X Ray ◽

X Ray Scattering ◽

Ray Scattering

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In situ grazing-incidence wide-angle X-ray scattering for hybrid perovskite semiconductors

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s0108767319099434 ◽

2019 ◽

Vol 75 (a1) ◽

pp. a56-a56

Author(s):

Hsinhan Tsai ◽

Cunming Liu ◽

Aditya Mohite ◽

Xiaoyi Zhang ◽

Joseph Strzalka ◽

...

Keyword(s):

Grazing Incidence ◽

Wide Angle ◽

X Ray ◽

X Ray Scattering ◽

Hybrid Perovskite ◽

Ray Scattering

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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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Application of In Situ X-ray Absorption Spectroscopy to Study Dilute Chromium Ions in a Molten Chloride Salt

10.26434/chemrxiv.9959807 ◽

2019 ◽

Author(s):

Jisue Moon ◽

Carter Abney ◽

Dmitriy Dolzhnikov ◽

James M. Kurley ◽

Kevin A. Beyer ◽

...

Keyword(s):

Absorption Spectroscopy ◽

Local Structure ◽

Chloride Salt ◽

X Ray ◽

Molten Chloride ◽

Stable Species ◽

Higher Temperature ◽

Cr Concentration ◽

X Ray Absorption

The local structure of dilute CrCl3 in a molten MgCl2:KCl salt was investigated by in situ x-ray absorption spectroscopy (XAS) at temperatures from room temperature to 800oC. This constitutes the first experiment where dilute Cr speciation is explored in a molten chloride salt, ostensibly due to the compounding challenges arising from a low Cr concentration in a matrix of heavy absorbers at extreme temperatures. CrCl3 was confirmed to be the stable species between 200 and 500oC, while mobility of metal ions at higher temperature (>700oC) prevented confirmation of the local structure.

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Strain Relaxation and In-Situ Observation of Voiding in Passivated Aluminum Alloy Lines.

MRS Proceedings ◽

10.1557/proc-308-249 ◽

1993 ◽

Vol 308 ◽

Cited By ~ 3

Author(s):

Paul R. Besser ◽

Thomas N. Marieb ◽

John C. Bravman

Keyword(s):

Strain Relaxation ◽

Grazing Incidence ◽

Scanning Transmission Electron Microscope ◽

In Situ Observation ◽

X Ray ◽

Scanning Transmission ◽

Length Width ◽

Measured Strain ◽

Ray Geometry

ABSTRACTStrain relaxation in passivated Al-0.5% Cu lines was measured using X-ray diffraction coupled with in-situ observation of the formation and growth of stress induced voids. Samples of 1 μm thick Al-0.5% Cu lines passivated with Si3N4 were heated to 380ºC, then cooled and held at 150ºC. During the test, principal strains along the length, width, and height of the line were determined using a grazing incidence x-ray geometry. From these measurements the hydrostatic strain in the metal was calculated and strain relaxation was observed. The thermal cycle was duplicated in a high voltage scanning transmission electron microscope equipped with a backscattered electron detector. The 1.25 μm wide lines were seen to have initial stress voids. Upon heating these voids reduced in size until no longer observable. Once the samples were cooled to 150ºC, voids reappeared and grew. The measured strain relaxation is discussed in terms of void and θ-phase (Al2Cu) formation.

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