In situ SAXS/XRD on mesoscopically ordered surfactant-silica mesophases; What can we learn?

2004 ◽  
Vol 847 ◽  
Author(s):  
Mika Lindén ◽  
Cilaine V. Teixeira ◽  
Heinz Amenitsch ◽  
Viveka Alfredsson ◽  
Freddy Kleitz
Keyword(s):  
Structural Evolution ◽  
Careful Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Synthesis ◽  
Composite Formation ◽  
Alkaline Conditions ◽  
Quantitative Results ◽  
Diffraction Patterns

ABSTRACTIn situ investigations have proven to be a very useful means of understanding the different processes involved in the formation of mesoporous materials. In this communication, we demonstrate the potential of in situ small angle x-ray scattering, SAXS and x-ray diffraction, XRD, measurements for giving both qualitative and quantitative results on the structural evolution during the early stages of the surfactant-silicate composite formation. The examples given are based on results obtained for 2D hexagonal structures, synthesized both under acidic and alkaline conditions. Careful analysis of both the scattering and diffraction patterns allows the different stages of the formation to be described in some detail. Thus, new synthesis approaches can be foreseen that allow the structure of the final hybrid mesophase to be rationally controlled.

STRUCTURAL EVOLUTION OF EXCEPTIONALLY IRON-DEFICIENT HEMATITE NANOCRYSTALS AS OBSERVED BY IN SITU SYNCHROTRON X-RAY DIFFRACTION

2019 ◽  
Author(s):  
Si Athena Chen ◽  
◽  
Peter Heaney ◽  
Jeffrey E. Post ◽  
Peter J. Eng ◽  
...  
Keyword(s):  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Iron Deficient

Structural evolution of NASICON-type Li1+xAlxGe2−x(PO4)3 using in situ synchrotron X-ray powder diffraction

2016 ◽  
Vol 4 (20) ◽  
pp. 7718-7726 ◽  
Author(s):  
Dorsasadat Safanama ◽  
Neeraj Sharma ◽  
Rayavarapu Prasada Rao ◽  
Helen E. A. Brand ◽  
Stefan Adams
Keyword(s):  
Solid Electrolyte ◽  
Diffraction Study ◽  
Powder Diffraction ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nasicon Type ◽  
Precursor Glass

In situ synchrotron X-ray diffraction study of the synthesis of solid-electrolyte Li1+xAlxGe2−x(PO4)3 (LAGP) from the precursor glass reveals that an initially crystallized dopant poor phase transforms into the Al-doped LAGP at 800 °C.

scholarly journals Elucidating the Structural Evolution of a Highy Porous Responsive Metal-Organic Framework (DUT-49(M)) upon Guests Desorption by Time-Resolved In-Situ Powder X-Ray Diffraction

2020 ◽  
Author(s):  
Bikash Garai ◽  
Volodymyr Bon ◽  
Francesco Walenszus ◽  
Azat Khadiev ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Adsorption Isotherms ◽  
Metal Organic Framework ◽  
Structural Evolution ◽  
Structural Transformations ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Metal Organic ◽  
Subcritical Fluid

Variation in the metal centres of M-M paddle-wheel SBU results in the formation of isostructural DUT-49(M) frameworks. However, the porosity of the framework was found to be different for each of the structures. While a high and moderate porosity was obtained for DUT-49(Cu) and DUT-49(Ni), respectively, other members of the series [DUT-49(M); M= Mn, Fe, Co, Zn, Cd] show very low porosity and shapes of the adsorption isotherms which is not expected for op phases of these MOFs. Investigation on those MOFs revealed that those frameworks undergo structural collapse during the solvent removal at the activation step. Thus, herein, we aimed to study the detailed structural transformations that are possibly occurring during the removal of the subcritical fluid from the framework.

In situ characterization of strain-induced crystallization of natural rubber by synchrotron radiation wide-angle X-ray diffraction: construction of a crystal network at low temperatures

Soft Matter ◽  
2019 ◽  
Vol 15 (4) ◽  
pp. 734-743 ◽  
Author(s):  
Pinzhang Chen ◽  
Jingyun Zhao ◽  
Yuanfei Lin ◽  
Jiarui Chang ◽  
Lingpu Meng ◽  
...  
Keyword(s):  
Low Temperatures ◽  
Structural Evolution ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
X Ray ◽  
Crystal Network ◽  
Strain Induced Crystallization ◽  
Induced Crystallization

The structural evolution of NR during stretching at −40 °C and in the strain–temperature space.

In situ coupling of atomic force microscopy and sub-micrometer focused X-ray techniques

2014 ◽  
Vol 1712 ◽  
Author(s):  
Thomas W. Cornelius ◽  
Zhe Ren ◽  
Francesca Mastropietro ◽  
Simon Langlais ◽  
Anton Davydok ◽  
...  
Keyword(s):  
Mechanical Response ◽  
Elemental Distribution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cu Nanowires ◽  
Force Microscopy ◽  
Indentation Tests ◽  
Scanning Force ◽  
Diffraction Patterns

ABSTRACTA scanning force microscope for in situ nanofocused X-ray studies (SFINX) has been developed which can be installed on diffractometers at synchrotron beamlines allowing for the combination with various techniques such as coherent X-ray diffraction and fluorescence. The capabilities of this device are demonstrated on Cu nanowires and on Au islands grown on sapphire (0001). The sample topography, crystallinity, and elemental distribution of the same area are investigated by recording simultaneously an AFM image, a scanning X-ray diffraction map, and a fluorescence map. Additionally, the mechanical response of Au islands is studied by in situ indentation tests employing the AFM-tip and recording 2D X-ray diffraction patterns during mechanical loading.

Effects of Glass Elements on the Structural Evolution ofin situGrown Ferroelectric Perovskite Crystals in Sol-gel Derived Glass-ceramics

1997 ◽  
Vol 12 (4) ◽  
pp. 1131-1140 ◽  
Author(s):  
Kui Yao ◽  
Weiguang Zhu ◽  
Liangying Zhang ◽  
Xi Yao
Keyword(s):  
Crystallization Process ◽  
Sol Gel ◽  
Glass Ceramics ◽  
Structural Evolution ◽  
Dielectric Measurements ◽  
X Ray Diffraction ◽  
Process Change ◽  
X Ray ◽  
Ferroelectric Perovskite

Several ABO3perovskite ferroelectric crystals, PbTiO3, Pb(Zr, Ti)O3, and BaTiO3have beenin situgrown from amorphous gels with glass elements, and the structural evolution has been systematically investigated using x-ray diffraction (XRD), infrared spectra (IR), differential thermal analysis (DTA), thermogravimetric analysis (TGA), and dielectric measurements. It is found that in the Si-contained glass-ceramic systems, Si and B glass elements are incorporated into the crystalline structures, resulting in the variation of the crystallization process, change of lattice constant, and dielectric properties. Some metastable phases expressed by a general formula AxByGzOw(A = Pb and Ba; B = Zr and Ti; G for glass elements, especially for Si) have been observed and discussed.

Development of an in situ synchrotron X-ray total scattering setup under pressurized hydrogen gas

2018 ◽  
Vol 51 (3) ◽  
pp. 796-801 ◽  
Author(s):  
Kouji Sakaki ◽  
Hyunjeong Kim ◽  
Akihiko Machida ◽  
Tetsu Watanuki ◽  
Yoshinori Katayama ◽  
...  
Keyword(s):  
Pair Distribution Function ◽  
Hydrogen Gas ◽  
Ex Situ ◽  
Sample Holder ◽  
Hydrogen Storage Materials ◽  
X Ray Diffraction ◽  
Total Scattering ◽  
X Ray ◽  
Diffraction Patterns

This article describes the development of an in situ gas-loading sample holder for synchrotron X-ray total scattering experiments, particularly for hydrogen storage materials, designed to collect diffraction and pair distribution function (PDF) data under pressurized hydrogen gas. A polyimide capillary with a diameter and thickness of 1.4 and 0.06 mm, respectively, connected with commercially available Swagelok fittings was used as an in situ sample holder. Leakage tests confirmed that this sample holder allows 3 MPa of hydrogen gas pressure and 393 K to be achieved without leakage. Using the developed in situ sample holder, significant background and Bragg peaks from the sample holder were not observed in the X-ray diffraction patterns and their signal-to-noise ratios were sufficiently good. The PDF patterns showed sharp peaks in the r range up to 100 Å. The results of Rietveld and PDF refinements of Ni are consistent with those obtained using a polyimide capillary (1.0 mm diameter and 0.04 mm thickness) that has been used for ex situ experiments. In addition, in situ synchrotron X-ray total scattering experiments under pressurized hydrogen gas up to 1 MPa were successfully demonstrated for LaNi4.6Cu.

scholarly journals A Flow-Through Reaction Cell for Studying Minerals Leaching by In-Situ Synchrotron Powder X-ray Diffraction

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 990
Author(s):  
Fatemeh Nikkhou ◽  
Fang Xia ◽  
Xizhi Yao ◽  
Idowu A. Adegoke ◽  
Qinfen Gu ◽  
...  
Keyword(s):  
Flow Rate ◽  
Pressure Leaching ◽  
X Ray Diffraction ◽  
Reaction Cell ◽  
Time Resolved ◽  
X Ray ◽  
Ore Minerals ◽  
Flow Through ◽  
Diffraction Patterns

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.

Investigation of Structural Evolution of Li1.1V3O8 by In Situ X-ray Diffraction and Density Functional Theory Calculations

2017 ◽  
Vol 29 (5) ◽  
pp. 2364-2373 ◽  
Author(s):  
Qing Zhang ◽  
Alexander B. Brady ◽  
Christopher J. Pelliccione ◽  
David C. Bock ◽  
Andrea M. Bruck ◽  
...  
Keyword(s):  
Density Functional Theory ◽  
Density Functional ◽  
Structural Evolution ◽  
Density Functional Theory Calculations ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray

scholarly journals In-situhigh-pressure powder X-ray diffraction study of α-zirconium phosphate

2014 ◽  
Vol 70 (3) ◽  
pp. 510-516
Author(s):  
Jennifer E. Readman ◽  
Alistair Lennie ◽  
Joseph A. Hriljac
Keyword(s):  
High Pressure ◽  
Synchrotron Radiation ◽  
Zirconium Phosphate ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
X Ray ◽  
Additional Water ◽  
Diffraction Patterns ◽  
Layered Phosphate

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied usingin-situhigh-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus,K0= 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr—O—P.

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