Three-Dimensional X-Ray Structural Microscopy Using Polychromatic Microbeams

MRS Bulletin ◽  
2004 ◽  
Vol 29 (3) ◽  
pp. 170-176 ◽  
Author(s):  
Gene E. Ice ◽  
Bennett C. Larson
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
X Rays ◽  
Actual Structure ◽  
X Ray ◽  
Elastic And Plastic Deformation ◽  
Strain Tensors ◽  
Microprobe Technique

AbstractIn this article, the authors describe the principle and application of differential-aperture x-ray microscopy (DAXM). This recently developed scanning x-ray microprobe technique uses a confocal or traveling pinhole camera approach to determine the crystal structure, crystallographic orientation, and elastic and plastic strain tensors within bulk materials. The penetrating properties of x-rays make the technique applicable to optically opaque as well as transparent materials, and it is nondestructive; this provides for in situ, submicrometer-resolution characterization of local crystal structure and for measurements of microstructure evolution on mesoscopic length scales from tenths to hundreds of micrometers. Examples are presented that illustrate the use of DAXM to study grain and subgrain morphology, grain-boundary types and networks, and local intra- and intergranular elastic and plastic deformation. Information of this type now provides a direct link between the actual structure and evolution in materials and increasingly powerful computer simulations and multiscale modeling of materials microstructure and evolution.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

X-RAY DIFFRACTION FOR SURFACES AND BURIED INTERFACES

2000 ◽  
Vol 07 (04) ◽  
pp. 437-446 ◽  
Author(s):  
G. RENAUD
Keyword(s):  
Grazing Incidence ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Grain Sizes ◽  
Buried Interfaces ◽  
Surfaces And Interfaces ◽  
Coherent Interfaces

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.

scholarly journals Microstructural characterization of a Canadian oil sand

2012 ◽  
Vol 49 (10) ◽  
pp. 1212-1220 ◽  
Author(s):  
Dinh Hong Doan ◽  
Pierre Delage ◽  
Jean François Nauroy ◽  
Anh Minh Tang ◽  
Souhail Youssef
Keyword(s):  
Three Dimensional ◽  
Microstructural Characterization ◽  
Water Layer ◽  
3D Image ◽  
Oil Sand ◽  
X Ray ◽  
Mcmurray Formation ◽  
Gas Expansion

The microstructure of oil sand samples extracted at a depth of 75 m from the estuarine Middle McMurray Formation (Alberta, Canada) has been investigated using high resolution three-dimensional (3D) X-ray microtomography (µCT) and cryo scanning electron microscopy (CryoSEM). µCT images evidenced some dense areas composed of highly angular grains surrounded by fluids, which are separated by larger pores full of gas. In dense areas, 3D image analysis provided porosity values comparable with in situ log data and macroscopic laboratory determinations, showing that they are representative of intact states. µCT hence provided some information on the morphology of the cracks and disturbance created by gas expansion. The CryoSEM technique, in which the sample is freeze fractured within the SEM chamber prior to observation, provided pictures in which the (frozen) bitumen clearly appears between the sand grains. No evidence of the existence of a thin connate water layer between grains and the bitumen, frequently mentioned in the literature, has been obtained. Bitumen appears to strongly adhere to the grains, with some grains being completely coated. The curved shape of some bitumen menisci suggests a bitumen wet behaviour.

scholarly journals Development of a sticker sealed microfluidic device for in situ analytical measurements using synchrotron radiation

2021 ◽  
Author(s):  
ITAMAR NECKEL ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica Teixeira ◽  
Angelo Gobbi ◽  
...  
Keyword(s):  
Microfluidic Device ◽  
Green Energy ◽  
X Rays ◽  
Electrical Measurements ◽  
X Ray ◽  
Electrochemical Nucleation ◽  
Synchrotron Light

Abstract Shedding synchrotron light on microfluidic systems, exploring several contrasts in situ operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.

scholarly journals Characterization of the crystal structure, kinematics, stresses and rotations in angular granular quartz during compaction

2018 ◽  
Vol 51 (4) ◽  
pp. 1021-1034 ◽  
Author(s):  
Ryan C. Hurley ◽  
Eric B. Herbold ◽  
Darren C. Pagan
Keyword(s):  
Crystal Structure ◽  
Mechanical Response ◽  
Three Dimensional ◽  
Spherical Particles ◽  
X Ray ◽  
Porosity Evolution ◽  
Individual Grains ◽  
Particle Packings ◽  
Number Of Particles

Three-dimensional X-ray diffraction (3DXRD), a method for quantifying the position, orientation and elastic strain of large ensembles of single crystals, has recently emerged as an important tool for studying the mechanical response of granular materials during compaction. Applications have demonstrated the utility of 3DXRD and X-ray computed tomography (XRCT) for assessing strains, particle stresses and orientations, inter-particle contacts and forces, particle fracture mechanics, and porosity evolution in situ. Although past studies employing 3DXRD and XRCT have elucidated the mechanics of spherical particle packings and angular particle packings with a small number of particles, there has been limited effort to date in studying angular particle packings with a large number of particles and in comparing the mechanics of these packings with those composed of a large number of spherical particles. Therefore, the focus of the present paper is on the mechanics of several hundred angular particles during compaction using in situ 3DXRD to study the crystal structure, kinematics, stresses and rotations of angular quartz grains. Comparisons are also made between the compaction response of angular grains and that of spherical grains, and stress-induced twinning within individual grains is discussed.

In-Situ X-Ray Characterization of LiMn2O4: A Comparison of Structural and Electrochemical Behavior

1997 ◽  
Vol 496 ◽  
Author(s):  
Mark A. Rodriguez ◽  
David Ingersoll ◽  
Daniel H. Doughty
Keyword(s):  
Crystal Structure ◽  
Structural Changes ◽  
Phase Changes ◽  
X Ray ◽  
In Situ Xrd ◽  
Electrochemical Cycling ◽  
Kinetic Effects ◽  
Carbon Anodes

ABSTRACTLixMn2O4 materials are of considerable interest in battery research and development. The crystal structure of this material can significantly affect the electrochemical performance. The ability to monitor the changes of the crystal structure during use, that is during electrochemical cycling, would prove useful to verify these types of structural changes. We report in-situ XRD measurements of LiMn2O4 cathodes with the use of an electrochemical cell designed for in-situ X-ray analysis. Cells prepared using this cell design allow investigation of the changes in the LiMn2O4 structure during charge and discharge. We describe the variation in lattice parameters along the voltage plateaus and consider the structural changes in terms of the electrochemical results on each cell. Kinetic effects of LiMn2O4 phase changes are also addressed. Applications of the in-situ cell to other compounds such as LiCoO2 cathodes and carbon anodes are presented as well.

Dichloro(diphosphine)(2-pyridyl-ketone)ruthenium(II) complexes

2003 ◽  
Vol 81 (11) ◽  
pp. 1263-1269 ◽  
Author(s):  
Salete L Queiroz ◽  
Alzir A Batista ◽  
Marcio P de Araujo ◽  
Roberto C Bianchini ◽  
Glaucius Oliva ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Synthesis And Characterization ◽  
X Ray

Described are the synthesis and characterization of Ru(II) complexes of the type RuCl2L2(N-O), where L2 is either 1,4-bis(diphenylphosphino)butane (dppb) or (PPh3)2, and N-O represents chelated 2-benzoylpyridine (2-bzpy) or 2-acetylpyridine (2-acpy); the Ru presursors used were [RuCl2(dppb)]2(µ-dppb) or RuCl2(PPh3)3. The crystal structure of cis-RuCl2(dppb)(2-bzpy) is presented, and three other RuCl2L2(N-O) complexes with cis-chlorines are isolated and characterized spectroscopically; of the trans-dichloro species, RuCl2(PPh3)2(N-O) complexes are isolated, while the corresponding dppb species are characterized in situ. In all cases, thermodynamically stable cis-complexes are formed from initially formed trans-species.Key words: ruthenium, phosphines, 2-benzoylpyridine, 2-acetylpyridine, X-ray structures.

scholarly journals Development of a sticker sealed microfluidic device for in situ analytical measurements using synchrotron radiation

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Itamar T. Neckel ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica C. Teixeira ◽  
Angelo L. Gobbi ◽  
...  
Keyword(s):  
Microfluidic Device ◽  
Green Energy ◽  
X Rays ◽  
Electrical Measurements ◽  
X Ray ◽  
Electrochemical Nucleation ◽  
Synchrotron Light

AbstractShedding synchrotron light on microfluidic systems, exploring several contrasts in situ/operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.

Synthesis, crystal structure and characterization of a three-dimensional CdII coordination polymer constructed from 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalate

2018 ◽  
Vol 74 (2) ◽  
pp. 166-170 ◽  
Author(s):  
Li Meng ◽  
Miao-Li Zhu ◽  
Li-Ping Lu
Keyword(s):  
Crystal Structure ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
X Ray ◽  
Distorted Octahedral ◽  
Ft Ir ◽  
A Chain ◽  
Coordinated Water ◽  
Dimensional Crystal

Bifunctional organic ligands are very popular for the design of coordination polymers because they allow the formation of a great diversity of structures. In the title coordination polymer, the new bifunctional inversion-symmetric ligand 2,5-bis(1H-1,2,4-triazol-1-yl)terephthalic acid (abbreviated as H2bttpa) links CdII cations, giving rise to the three-dimensional CdII coordination polymer catena-poly[diaqua[μ4-2,5-bis(1H-1,2,4-triazol-1-yl)terephthalato-κ4 O 1:O 4:N 4:N 4′]cadmium(II)], [Cd(C12H6N6O4)(H2O)2] n or [Cd(bttpa)(H2O)2] n . The asymmetric unit consists of half a CdII cation, half a bttpa2− ligand and one coordinated water molecule. The CdII cation is located on a twofold axis and is hexacoordinated in a distorted octahedral environment of four O and two N atoms. Four different bttpa2− ligands contribute to this coordination, with two carboxylate O atoms in trans positions and two triazole N atoms in cis positions. Two aqua ligands in cis positions complete the coordination sphere. The fully deprotonated bttpa2− ligand sits about a crystallographic centre of inversion and links two CdII cations to form a chain in a μ2-terephthalato-κ2 O 1:O 4 bridge. This chain extends in the other two directions via the triazole heterocycles, producing a three-dimensional framework. O—H...O hydrogen bonds and weak C—H...N interactions stabilize the three-dimensional crystal structure. The FT–IR spectrum, X-ray powder pattern, thermogravimetric behaviour and solid-state photoluminescence of the title polymer have been investigated. The photoluminescence is enhanced and red-shifted with respect to the uncoordinated ligand.

scholarly journals Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment

2016 ◽  
Vol 23 (5) ◽  
pp. 1241-1244 ◽  
Author(s):  
Wonsuk Cha ◽  
Wenjun Liu ◽  
Ross Harder ◽  
Ruqing Xu ◽  
Paul H. Fuoss ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Three Dimensions ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Individual Crystal ◽  
Sample Motion ◽  
Diffraction Imaging ◽  
Individual Grains

A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible within situsample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifyingin situchamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.

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