Cu-MCM-22 zeolite: A combined X-ray powder diffraction and computational study of the local structure of extra-framework copper ions

The crystal structures of loxapine succinate [systematic name: 4-(2-chlorodibenzo[b,f][1,4]oxazepin-11-yl)-1-methylpiperazin-1-ium 3-carboxypropanoate], C18H19ClN3O+·C4H5O4−, and loxapine succinate monohydrate {systematic name: bis[4-(2-chlorodibenzo[b,f][1,4]oxazepin-11-yl)-1-methylpiperazin-1-ium] succinate succinic acid dihydrate}, 2C18H19ClN3O+·C4H4O42−·C4H6O4·2H2O, have been determined using X-ray powder diffraction and single-crystal X-ray diffraction, respectively. Fixed cell geometry optimization calculations using density functional theory confirmed that the global optimum powder diffraction derived structure also matches an energy minimum structure. The energy calculations proved to be an effective tool in locating the positions of the H atoms reliably and verifying the salt configuration of the structure determined from powder data. Crystal packing analysis of these structures revealed that the loxapine succinate structure is based on chains of protonated loxapine molecules while the monohydrate contains dispersion stabilized centrosymmetric dimers. Incorporation of water molecules within the crystal lattice significantly alters the molecular packing and protonation state of the succinic acid.

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Synthesis and Investigation of Antimicrobial Activity of Cu2O Nanoparticles/Zeolite

Journal of Nanoparticles ◽

10.1155/2017/7056864 ◽

2017 ◽

Vol 2017 ◽

pp. 1-6 ◽

Cited By ~ 12

Author(s):

Bui Duy Du ◽

Dang Van Phu ◽

Le Anh Quoc ◽

Nguyen Quoc Hien

Keyword(s):

Electron Microscopy ◽

Cuprous Oxide ◽

Large Scale ◽

Copper Ions ◽

Zeolite A ◽

X Ray Diffraction ◽

X Ray ◽

Agricultural Application ◽

Transmission Electron ◽

Cu2o Nanoparticles

Cuprous oxide (Cu2O) nanoparticles in zeolite A were synthesized by two steps: (i) ion-exchange of copper ions into the zeolite and (ii) reduction of copper ions in cages of the zeolite by hydrazine hydrate in base medium. The Cu2O nanoparticles/zeolite product was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDX). The particle size of Cu2O nanoparticles was of 40 nm. The antibacterial activity of the as-synthesized Cu2O nanoparticles/zeolite against Escherichia coli was also investigated. Cu2O NPs/zeolite product can be favorably produced on large scale for water treatment and agricultural application as antimicrobial agent.

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Hydrothermal Synthesis of Zeolite a Using Non-Calcined Diatomite

Materials Science Forum ◽

10.4028/www.scientific.net/msf.930.3 ◽

2018 ◽

Vol 930 ◽

pp. 3-7 ◽

Cited By ~ 1

Author(s):

Alexandre Fontes Melo de Carvalho ◽

Tiago Roberto da Costa ◽

Gilvan Pereira de Figueredo ◽

José Antônio Barros Leal Reis Alves ◽

Rodrigo César Santiago ◽

...

Keyword(s):

Electron Microscopy ◽

Scanning Electron Microscopy ◽

Hydrothermal Synthesis ◽

Crystallite Size ◽

Powder Diffraction ◽

Average Crystallite Size ◽

Zeolite A ◽

X Ray ◽

Prepared Sample ◽

Scanning Electron

Optimization and reduction of zeolite A synthesis costs are the focus of several studies. Attention has been given to the use of residues and natural materials rich in Si and Al, such as diatomite. Diatomite needs to be calcined above 500°C to be used, which increases processing costs. This study aimed at evaluating the use of diatomite without calcination in preparing zeolite A. Alkaline hydrothermal synthesis melting and 24 h of crystallization were carried out. The materials were characterized by XRD (X-ray powder diffraction), XRF (X-ray fluorescence), BET (N2physisorption) and SEM (Scanning Electron Microscopy). XRD data and refinement show that the obtained material presents 99.84% crystallinity, average crystallite size of 54.92 nm, and a semi-quantitative percentage of 79% zeolite A. SiO2and Al2O3contents in the prepared sample proved the ratio SiO2/Al2O3= 2. The micrographies show cubic particles and agglomerated sodalite.

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Mitigated phase transition during first cycle of a Li-rich layered cathode studied by in operando synchrotron X-ray powder diffraction

Physical Chemistry Chemical Physics ◽

10.1039/c5cp04801j ◽

2016 ◽

Vol 18 (6) ◽

pp. 4745-4752 ◽

Cited By ~ 23

Author(s):

Bohang Song ◽

Sarah J. Day ◽

Tan Sui ◽

Li Lu ◽

Chiu C. Tang ◽

...

Keyword(s):

Phase Transition ◽

Diffraction Study ◽

Powder Diffraction ◽

Local Structure ◽

X Ray ◽

In Operando ◽

Cr Doping

In operando synchrotron X-ray powder diffraction study of pristine and Cr-doped Li-rich battery cathodes during the first charge cycle shows the benefit of Cr-doping in stabilizing the local structure by suppressing the activation of Li2MnO3 domains.

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A Synthesis, MAS NMR, Synchrotron X-ray Powder Diffraction, and Computational Study of Zeolite SSZ-23

Chemistry of Materials ◽

10.1021/cm991057r ◽

1999 ◽

Vol 11 (10) ◽

pp. 2878-2885 ◽

Cited By ~ 25

Author(s):

Miguel A. Camblor ◽

María-José Díaz-Cabañas ◽

Paul A. Cox ◽

Ian J. Shannon ◽

Paul A. Wright ◽

...

Keyword(s):

Powder Diffraction ◽

Computational Study ◽

Mas Nmr ◽

X Ray

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X-ray and neutron powder diffraction studies of (Ba1−xSrx)Y2CuO5

Powder Diffraction ◽

10.1154/1.2217029 ◽

2006 ◽

Vol 21 (3) ◽

pp. 200-209

Author(s):

Z. Yang ◽

W. Wong-Ng ◽

L. P. Cook ◽

J. A. Kaduk ◽

Q. Z. Huang

Keyword(s):

Powder Diffraction ◽

Single Phase ◽

Copper Ions ◽

General Structure ◽

Three Dimensional ◽

Neutron Powder Diffraction ◽

Powder Diffraction File ◽

Triangular Face ◽

X Ray ◽

Orthorhombic Cell

This paper reports the results of crystallography and crystal chemistry investigation of the (Ba1−xSrx)Y2CuO5 (“green phase”) solid solution series by X-ray powder diffraction (XPD) and neutron powder diffraction techniques. The single phase regions for (Ba1−xSrx)Y2CuO5 were determined to be 0⩽x⩽0.3 for samples prepared at 810 °C in 100 Pa pO2, and 0⩽x⩽0.7 for samples prepared at 930 °C in air. All single phase (Ba1−xSrx)Y2CuO5 samples are isostructural to BaY2CuO5 and can be indexed using an orthorhombic cell with the space group Pnma. Lattice parameters, a,b,c and the cell volume, V, of the (Ba1−xSrx)Y2CuO5 members decrease linearly with increasing Sr substitution (x) on the Ba site. The general structure of (Ba1−xSrx)Y2CuO5 can be considered as having a three-dimensional interconnected network of [YO7],[(Ba,Sr)O11], and [CuO5] polyhedra. The copper ions are located inside distorted [CuO5] “square” pyramids. These pyramids are connected by the [Y2O11] groups that are formed from two monocapped [YO7] trigonal prisms sharing a triangular face. The Ba2+ ions are found to reside in distorted 11-fold coordinated cages. The oxygen sites are essentially fully occupied. XPD reference patterns of two members of the series, (Ba0.3Sr0.7)Y2CuO5 and (Ba0.7Sr0.3)Y2CuO5, were prepared for inclusion in the powder diffraction file.

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X-ray microprobe for materials science

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100168013 ◽

1994 ◽

Vol 52 ◽

pp. 56-57

Author(s):

G.E. Ice

Keyword(s):

Crystallographic Orientation ◽

Local Structure ◽

Materials Science ◽

Chemical Information ◽

X Ray Diffraction ◽

Ray Optics ◽

X Ray ◽

Novel Materials ◽

New Information ◽

Elemental Sensitivity

The increasing availability of synchrotron x-ray sources has stimulated the development of advanced hard x-ray (E≥5 keV) microprobes. With new x-ray optics these microprobes can achieve micron and submicron spatial resolutions. The inherent elemental and crystallographic sensitivity of an x-ray microprobe and its inherently nondestructive and penetrating nature will have important applications to materials science. For example, x-ray fluorescent microanalysis of materials can reveal elemental distributions with greater sensitivity than alternative nondestructive probes. In materials, segregation and nonuniform distributions are the rule rather than the exception. Common interfaces to whichsegregation occurs are surfaces, grain and precipitate boundaries, dislocations, and surfaces formed by defects such as vacancy and interstitial configurations. In addition to chemical information, an x-ray diffraction microprobe can reveal the local structure of a material by detecting its phase, crystallographic orientation and strain.Demonstration experiments have already exploited the penetrating nature of an x-ray microprobe and its inherent elemental sensitivity to provide new information about elemental distributions in novel materials.

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