scholarly journals Synthesis and Crystallographic Characterization of X-Substituted 2,4-Dinitrophenyl-4′-phenylbenzenesulfonates

Chemistry ◽  
2020 ◽  
Vol 2 (2) ◽  
pp. 591-599
Author(s):  
Brock A. Stenfors ◽  
Richard J. Staples ◽  
Shannon M. Biros ◽  
Felix N. Ngassa
Keyword(s):  
Diffraction Data ◽  
Pyridinium Salt ◽  
Environmentally Benign ◽  
Pyridinium Salts ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Aqueous Environments ◽  
Aqueous Base

Treatment of 2,4-dinitrophenol with sulfonyl chlorides in the presence of pyridine results in the formation of undesired pyridinium salts. In non-aqueous environments, the formation of the insoluble pyridinium salt greatly affects the formation of the desired product. A facile method of producing the desired sulfonate involves the use of an aqueous base with a water-miscible solvent. Herein, we present the optimization of methods for the formation of sulfonates and its application in the production of desired x-substituted 2,4-dinitrophenyl-4′-phenylbenzenesulfonates. This strategy is environmentally benign and supports a wide range of starting materials. Additionally, the intermolecular interactions of these sulfonate compounds were investigated using single-crystal x-ray diffraction data.

Single Crystal Wurtzitic Aluminum Nitride Growth on Silicon Using Supersonic Gas Jets

1995 ◽  
Vol 395 ◽  
Author(s):  
S. A. Ustin ◽  
L. Lauhon ◽  
K. A. Brown ◽  
D. Q. Hu ◽  
W. Ho
Keyword(s):  
Aluminum Nitride ◽  
Growth Rates ◽  
High Energy ◽  
X Ray Diffraction ◽  
Rutherford Back Scattering ◽  
X Ray ◽  
Supersonic Molecular Beam ◽  
Supersonic Beams ◽  
Wide Range

ABSTRACTHighly oriented aluminum nitride (0001) films have been grown on Si(001) and Si (111) substrates at temperatures between 550° C and 775° C with dual supersonic molecular beam sources. Triethylaluminum (TEA;[(C2H5)3Al]) and ammonia (NH3) were used as precursors. Hydrogen, helium, and nitrogen were used as seeding gases for the precursors, providing a wide range of possible kinetic energies for the supersonic beams due to the disparate masses of the seed gases. Growth rates of AIN were found to depend strongly on the substrate orientation and the kinetic energy of the incident precursor; a significant increase in growth rate is seen when seeding in hydrogen or helium as opposed to nitrogen. Growth rates were 2–3 times greater on Si(001) than on Si(111). Structural characterization of the films was done by reflection high energy electron diffraction (RHEED) and x-ray diffraction (XRD). X-ray rocking curve (XRC) full-width half-maxima (FWHM) were seen as small as 2.5°. Rutherford back scattering (RBS) was used to determine the thickness of the films and their chemical composition. Films were shown to be nitrogen rich, deviating from perfect stoichiometry by 10%–20%. Surface analysis was performed by Auger electron spectroscopy (AES).

Synthesis and Characterization of ALaFeNi0.5W0.5O6 (A= Sr or Ca), a New Structure Distorted Double Perovskite

2013 ◽  
Vol 717 ◽  
pp. 133-138
Author(s):  
A. Awad Allah ◽  
M. Elhadi ◽  
O.A. Yassien
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Double Perovskite ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
X Ray ◽  
Perovskite Materials ◽  
Ftir Spectrometer

The crystal structure of both samples has been solved by powder X-ray diffraction, data in the tetragonal space group I4/m (a= b= 5.55182 Å, c =7.86955 A0) for SrLaFeNi0.5W0.5O6sample and (a=b= 5.49129Å, c= 7.82233Å) for CaLaFeNi0.5W0.5O6 sample, and shows an almost perfect ordering between Ni2+ and W5+ cations at the B-site of the perovskite structure. The FTIR spectrometer used of the powders showed that the spectra of both are very similar, showing two strong and well-defined absorption bands, typical of perovskite materials.

scholarly journals Characterization of FeOOH Nanoparticles and Amorphous Silica Matrix in an FeOOH-SiO2Nanocomposite

2008 ◽  
Vol 2008 ◽  
pp. 1-6 ◽  
Author(s):  
Guido Ennas ◽  
Maria F. Casula ◽  
Sergio Marras ◽  
Gabriele Navarra ◽  
Alessandra Scano ◽  
...  
Keyword(s):  
Hydrochloric Acid ◽  
Amorphous Silica ◽  
Diffraction Data ◽  
Silica Matrix ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Matrix ◽  
Curve Method ◽  
Hydrolysis Of

A nanocomposite with an FeOOH/SiO2ratio equal to 17.7 wt% and the pertinent matrix, obtained by etching away the nanoparticles through reaction with hydrochloric acid, were investigated by XRD, TGA-DTA, heliostereopicnometry, BET, and TEM techniques. The study shows the presence in the nanocomposite of ferrihydrite nanoparticles phase with average dimensions around 4 nm. The FeOOH nanoparticles structure was analyzed by synchrotron X-ray diffraction data using the distribution difference curve method. The porous structure of the matrix resulting by etching away the nanoparticles differs significantly from that of a pureSiO2sample obtained by hydrolysis of TEOS under the same operative conditions followed in the nanocomposite preparation.

The characterization of serpentine minerals by X-ray diffraction

1956 ◽  
Vol 31 (233) ◽  
pp. 107-126 ◽  
Author(s):  
E. J. W. Whittaker ◽  
J. Zussman
Keyword(s):  
Diffraction Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Serpentine Minerals ◽  
Serpentine Mineral

SummaryX-ray diffraction data on serpentine minerals are discussed. There arc three structural varieties of chrysotile: ortho-chrysotile, clino-chrysotile, and para-chrysotile. Methods are described for the estimation of the proportions of the first two of these in mixed specimens, and their distribution in nature is reviewed. The variations observed in powder photographs of serpentine minerals are interpreted in accordance with this classification. The criteria proposed by Selfridge for distinguishing between chrysotile and antigorite are shown to be unreliable, but valid criteria are presented. The powder photographs also reveal the existence of a third serpentine mineral, distinct from chrysotile and antigorite, for which the name lizardite is proposed. Four samples of bastite are shown to consist of chrysotile or lizardite rather than antigorite. All the serpentine minerals examined consist either of antigorite or of one or more of the group comprising lizardite and the chrysotile varieties.

Characterization of the Aurivillius Type PbBi4Ti4O15 Piezoelectric Ceramic Doped with Eu3+

2006 ◽  
Vol 45 ◽  
pp. 2483-2488
Author(s):  
L. Pablos ◽  
Maria Elena Villafuerte-Castrejón ◽  
A. Ibarra-Palos ◽  
J. Ocotlán-Flores ◽  
R. Sato ◽  
...  
Keyword(s):  
Piezoelectric Ceramic ◽  
Solubility Limit ◽  
Lattice Parameter ◽  
Layered Oxides ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Density Measurements ◽  
X Ray ◽  
Wide Range

PbBi4Ti4O15 belongs to the bismuth oxide layers family discovered by Aurivillius more than 50 years ago. In the last few years, there has been considerable interest in layered oxides exhibiting ferroelectric, piezoelectric and other related properties due to their wide range of application in technical devices. In the present work the PbBi4Ti4O15 solid solution formed with Eu3+ was synthesized by coprecipitation method and solubility limit was found. All compounds were characterized by scanning electron microscopy, density measurements and X-ray diffraction. The variation of lattice parameter with the Eu3+ concentration was obtained. Raman spectroscopy was carried out in order to determine the Eu3+ site in the lattice. Thermal analysis (thermogravimetry and differencial scanning calorimetry) results are also presented.

Synthesis and structural characterization of Li3Y(BO3)2

2017 ◽  
Vol 72 (2) ◽  
pp. 153-158 ◽  
Author(s):  
Sebastian Bräuchle ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Solid State ◽  
Boric Acid ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Lithium Carbonate ◽  
X Ray Diffraction ◽  
X Ray

AbstractLi3Y(BO3)2 was prepared by high-temperature solid state synthesis at 900°C in a platinum crucible from lithium carbonate, boric acid, and yttrium(III) oxide. The compound crystallizes monoclinically in the space group P21/c (no. 14) (Z=4) isotypically to Li3Gd(BO3)2. The structure was refined from single-crystal X-ray diffraction data: a=8.616(3), b=6.416(3), c=10.014(2) Å, β=116.6(2)°, V=494.9(3) Å3, R1=0.0211, and wR2=0.0378 for all data. The crystal structure of Li3Y(BO3)2 consists of [Y2O14] dinuclear units, which are interconnected to each other by planar B(1)O3 groups and LiO4 tetrahedra via common edges and corners along the a axis.

Energetic Materials: The Preparation and Structural Characterization of Three Biguanidinium Dinitramides

1997 ◽  
Vol 53 (3) ◽  
pp. 504-512 ◽  
Author(s):  
A. Martin ◽  
A. A. Pinkerton ◽  
R. D. Gilardi ◽  
J. C. Bottaro
Keyword(s):  
Hydrogen Bonding ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Energetic Materials ◽  
Room Temperature ◽  
Asymmetric Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bond Lengths

Three biguanidinium salts of the energetic dinitramide anion have been prepared and structurally characterized from room-temperature X-ray diffraction data. Biguanidinium mono-dinitramide, (BIGH)(DN), triclinic, P\overline 1, a = 4.3686 (4), b = 9.404 (2), c = 10.742 (1) Å, \alpha = 83.54 (1), \beta = 80.386 (9), \gamma = 79.93 (1)°, V = 426.8 (1) Å3, Z = 2, D x = 1.62 g cm−3. Biguanidinium bis-dinitramide, (BIGH2)(DN)2, monoclinic, C2/c, a = 11.892 (2), b = 8.131 (1), c = 13.038 (2) Å, \beta = 115.79 (1)°, V = 1135.1 (3) Å3, Z = 4, D x = 1.84 g cm−3. Biguanidinium bis-dinitramide monohydrate, (BIGH2)(DN)2.H2O, orthorhombic, P212121, a = 6.4201 (6), b = 13.408 (1), c = 14.584 (2) Å, V = 1255.4 (4) Å3, Z = 4, D x = 1.76 g cm−3. All three structures are characterized by extensive hydrogen bonding. Both the mono- and diprotontated cations consist of two planar halves twisted with respect to each other. The dinitramide anion has a surprisingly variable and asymmetric structure. The two halves of the anion are twisted with respect to each other; however, the twist varies from 5.1 to 28.9°. In addition, the two ends of the anion have significantly different geometries, e.g. the `equivalent' N—N bond lengths differ by up to 0.045 Å.

Synthesis and structural characterization of BaSr2Ge3O9

2016 ◽  
Vol 71 (12) ◽  
pp. 1225-1232
Author(s):  
Sebastian Bräuchle ◽  
Clivia Hejny ◽  
Hubert Huppertz
Keyword(s):  
High Temperature ◽  
Solid State ◽  
Structural Characterization ◽  
Diffraction Data ◽  
Barium Carbonate ◽  
Strontium Carbonate ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray

AbstractBaSr2Ge3O9 was prepared by high-temperature solid-state synthesis at 1100°C in a platinum crucible from barium carbonate, strontium carbonate, and germanium(IV) oxide. The compound crystallizes in the triclinic space group P1̅ (no. 2) isotypically to walstromite BaCa2Si3O9. The structure was refined from single-crystal X-ray diffraction data: a=7.104(5), b=10.060(7), c=7.099(5) Å, α=83.0(2), β=77.0(2), γ=70.2(2)°, V=464.3(6) Å3, R1=0.0230, and wR2=0.0602 for all data. BaSr2Ge3O9 is characterized by three-membered rings of germanate tetrahedra. There are three crystallographically different Ge sites (Ge1, Ge2, and Ge3) in each [Ge3O9]6− ring. The rings occur in layers with the apices of alternating rings pointing in opposite directions. The Sr2+ and Ba2+ ions are located in between. The Sr1 cation is eight-fold coordinated, while Sr2 is octahedrally surrounded by oxide anions, and the Ba cation again eight-fold coordinated.

scholarly journals Alginate-Mediated Synthesis of Hetero-Shaped Silver Nanoparticles and their Hydrogen Peroxide Sensing ability

2020 ◽  
Author(s):  
Sneha Bhagyaraj ◽  
Igor Krupa
Keyword(s):  
Hydrogen Peroxide ◽  
Particle Size ◽  
Silver Nanoparticles ◽  
Environmentally Benign ◽  
X Ray Diffraction ◽  
Ag Nps ◽  
X Ray ◽  
Transmission Electron ◽  
Wide Range ◽  
Pollution Detection

Silver nanoparticles have been the focus of extensive research for many decades due to their unique physical, chemical and electrical properties. Introducing new environmentally benign methods for the synthesis of silver nanoparticles is of great interest in the research community. In this work we propose a new method for the simple synthesis of stable heterostructured biopolymer (sodium alginate)-capped silver nanoparticles (Ag-NPs) based on green chemistry.The as-prepared nanoparticles were characterized using the ultraviolet–visible (UV–Vis) absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and Dynamic light scattering (DLS) techniques. The results showed that the as-prepared Ag-NPs have a heterostructured morphology with particle size in the range 30 ± 18 – 60 ± 25 nm, showing a zeta potential of -62 mV. The silver nanoparticle formation was confirmed from UV-Vis spectra showing 424 nm as maximum absorption. The particle size and crystallinity of the as- synthesized nanoparticles were analyzed using TEM and XRD measurements respectively. FTIR spectra confirmed the presence of alginate as capping agent to stabilize the nanoparticles. The Ag-NPs also showed excellent sensing capability, with a linear response to hydrogen peroxide spanning a wide range of concentrations from 10-1 – 10-7 M, which indicates their high potential for water treatment applications, such as pollution detection and nanofiltration composites.

scholarly journals Growth and characterization of Cd1-xZnxTe (0 \leq x \leq 1) nanolayers grown by isothermal closed space atomic layer deposition on GaSb and GaAs

2018 ◽  
Vol 64 (3) ◽  
pp. 206
Author(s):  
R. S. Castillo Ojeda ◽  
Joel Díaz-Reyes ◽  
M. Galván-Arellano ◽  
K. N. Rivera-Hernández ◽  
M. S. Villa-Ramírez ◽  
...  
Keyword(s):  
High Resolution ◽  
Atomic Layer Deposition ◽  
Atomic Layer ◽  
Growth Surface ◽  
X Ray Diffraction ◽  
X Ray ◽  
Layer Deposition ◽  
Wide Range ◽  
Cdte Growth

In this work are presented the results obtained from the deposition ofCd1-xZnxTe nanolayers using as precursor the vapours of the elementsZn, Te, and a mixture of Cd and Zn on GaAs and GaSb (001) substrates by Atomic Layer Deposition technique (ALD), which allows the deposition of layers of nanometric dimensions. At each exposure of the growth surface to the of cation or anion precursors vapours, this surface is saturated. Therefore, it is considered that the process is self-regulated. The ZnTe layers were grown in a wide range of temperatures; however, ZnTe nanolayers with a shiny mirror-like surface could be grown at temperatures between 370 and 410oC. Temperatures higher than 400oC were necessary for the CdTe growth. The layers of the Cd1-xZnxTe ternary alloy were deposited at temperature range of 400 and 425oC. The grown nanofilms were characterized by Raman spectroscopy and high-resolution X-ray diffraction. The Raman spectrumshows the peak corresponding to LO-ZnTe at 208 cm-1, which is weak and is slightly redshifted in comparison with the reported for the bulk ZnTe. For the case of the CdTe nanolayers, Raman spectrum presents the LO-CdTe peak, which is indicative of the successfully growth of the nanolayers, its weakness and its slight redshifted in comparison with the reported for the bulk CdTe can be related with the nanometric characteristic of this layer. The performed high resolution X-ray diffraction measurements allowed to study some importantcharacteristics, as the crystallinity of the grown layers. Additionally, the performed HR-XRD measurements suggest that the crystalline quality have dependence with the growth temperature.

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