Synthesis and Characterizations of PdNi Carbon Supported Nanomaterials: Studies of Electrocatalytic Activity for Oxygen Reduction in Alkaline Medium

Electrocatalytic materials offer numerous benefits due to their wide range of applications. In this study, a polyol technique was used to synthesize PdNi nanoparticles (NPs) with different percent atomic compositions (Pd = 50 to 90%) to explore their catalytic efficiency. The produced nanoparticles were characterized using X-ray diffraction (XRD) and electrochemical investigations. According to XRD measurements, the synthesized NPs were crystalline in nature, with crystallite sizes of about 2 nm. The electrochemical properties of the synthesized NPs were studied in alkaline solution through a rotating ring-disk electrode (RRDE) technique of cyclic voltammetry. The PdNi nanoparticles supported on carbon (PdNi/C) were used as electrocatalysts and their activity and stability were compared with the homemade Pd/C and Pt/C. In alkaline solution, PdNi/C electrocatalysts showed improved oxygen reduction catalytic activity over benchmark Pd/C and Pt/C electrocatalysts in all composition ratios. Furthermore, stability experiments revealed that PdNi 50:50 is more stable in alkaline solution than pure Pd and other PdNi compositions.

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Multidimensional Ln-Aminophthalate Photoluminescent Coordination Polymers

Materials ◽

10.3390/ma14071786 ◽

2021 ◽

Vol 14 (7) ◽

pp. 1786

Author(s):

Carla Queirós ◽

Chen Sun ◽

Ana M. G. Silva ◽

Baltazar de Castro ◽

Juan Cabanillas-Gonzalez ◽

...

Keyword(s):

Water Content ◽

Coordination Polymers ◽

Metal Ion ◽

Low Cost ◽

Microwave Assisted Synthesis ◽

X Ray Diffraction ◽

X Ray ◽

Wide Range ◽

Ft Ir ◽

Ft Ir Spectroscopy

The development of straightforward reproducible methods for the preparation of new photoluminescent coordination polymers (CPs) is an important goal in luminescence and chemical sensing fields. Isophthalic acid derivatives have been reported for a wide range of applications, and in addition to their relatively low cost, have encouraged its use in the preparation of novel lanthanide-based coordination polymers (LnCPs). Considering that the photoluminescent properties of these CPs are highly dependent on the existence of water molecules in the crystal structure, our research efforts are now focused on the preparation of CP with the lowest water content possible, while considering a green chemistry approach. One- and two-dimensional (1D and 2D) LnCPs were prepared from 5-aminoisophthalic acid and Sm3+/Tb3+ using hydrothermal and/or microwave-assisted synthesis. The unprecedented LnCPs were characterized by single-crystal X-ray diffraction (SCRXD), powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM), and their photoluminescence (PL) properties were studied in the solid state, at room temperature, using the CPs as powders and encapsulated in poly(methyl methacrylate (PMMA) films, envisaging the potential preparation of devices for sensing. The materials revealed interesting PL properties that depend on the dimensionality, metal ion, co-ligand used and water content.

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Local atomic structure in tetragonal pure ZrO2nanopowders

Journal of Applied Crystallography ◽

10.1107/s0021889809054983 ◽

2010 ◽

Vol 43 (2) ◽

pp. 227-236 ◽

Cited By ~ 16

Author(s):

Leandro M. Acuña ◽

Diego G. Lamas ◽

Rodolfo O. Fuentes ◽

Ismael O. Fábregas ◽

Márcia C. A. Fantini ◽

...

Keyword(s):

Tetragonal Phase ◽

Local Structure ◽

X Ray Diffraction ◽

X Ray ◽

Atomic Structures ◽

Crystallite Sizes ◽

Exafs Study ◽

The Difference ◽

X Ray Absorption ◽

Good Agreement

The local atomic structures around the Zr atom of pure (undoped) ZrO2nanopowders with different average crystallite sizes, ranging from 7 to 40 nm, have been investigated. The nanopowders were synthesized by different wet-chemical routes, but all exhibit the high-temperature tetragonal phase stabilized at room temperature, as established by synchrotron radiation X-ray diffraction. The extended X-ray absorption fine structure (EXAFS) technique was applied to analyze the local structure around the Zr atoms. Several authors have studied this system using the EXAFS technique without obtaining a good agreement between crystallographic and EXAFS data. In this work, it is shown that the local structure of ZrO2nanopowders can be described by a model consisting of two oxygen subshells (4 + 4 atoms) with different Zr—O distances, in agreement with those independently determined by X-ray diffraction. However, the EXAFS study shows that the second oxygen subshell exhibits a Debye–Waller (DW) parameter much higher than that of the first oxygen subshell, a result that cannot be explained by the crystallographic model accepted for the tetragonal phase of zirconia-based materials. However, as proposed by other authors, the difference in the DW parameters between the two oxygen subshells around the Zr atoms can be explained by the existence of oxygen displacements perpendicular to thezdirection; these mainly affect the second oxygen subshell because of the directional character of the EXAFS DW parameter, in contradiction to the crystallographic value. It is also established that this model is similar to another model having three oxygen subshells, with a 4 + 2 + 2 distribution of atoms, with only one DW parameter for all oxygen subshells. Both models are in good agreement with the crystal structure determined by X-ray diffraction experiments.

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2D X-ray diffraction and molecular modelling of the crystalline structure of polyesters under uniaxial stress

Polymers and Polymer Composites ◽

10.1177/0967391121998225 ◽

2021 ◽

pp. 096739112199822

Author(s):

Ahmed I Abou-Kandil ◽

Gerhard Goldbeck

Keyword(s):

Crystalline Structure ◽

Molecular Modelling ◽

Three Dimensional ◽

Uniaxial Stress ◽

X Ray Diffraction ◽

X Ray ◽

Wide Range ◽

Modelling Techniques ◽

Diffraction Patterns

Studying the crystalline structure of uniaxially and biaxially drawn polyesters is of great importance due to their wide range of applications. In this study, we shed some light on the behaviour of PET and PEN under uniaxial stress using experimental and molecular modelling techniques. Comparing experiment with modelling provides insights into polymer crystallisation with extended chains. Experimental x-ray diffraction patterns are reproduced by means of models of chains sliding along the c-axis leading to some loss of three-dimensional order, i.e. moving away from the condition of perfect register of the fully extended chains in triclinic crystals of both PET and PEN. This will help us understand the mechanism of polymer crystallisation under uniaxial stress and the appearance of mesophases in some cases as discussed herein.

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Effect of Synthesis Temperature on Particles Size and Morphology of Zirconium Oxide Nanoparticle

Journal of Nano Research ◽

10.4028/www.scientific.net/jnanor.50.18 ◽

2017 ◽

Vol 50 ◽

pp. 18-31 ◽

Cited By ~ 6

Author(s):

Rudzani Sigwadi ◽

Simon Dhlamini ◽

Touhami Mokrani ◽

Patrick Nonjola

Keyword(s):

Electron Microscopy ◽

Particle Size ◽

Zirconium Oxide ◽

Thermo Gravimetric Analysis ◽

Gravimetric Analysis ◽

X Ray Diffraction ◽

X Ray ◽

Transmission Electron ◽

Crystallite Sizes ◽

Ft Ir

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.

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Theoretical study of the properties of X-ray diffraction moiré fringes. II. Illustration of angularly integrated moiré images

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s2053273319004601 ◽

2019 ◽

Vol 75 (4) ◽

pp. 610-623

Author(s):

Jun-ichi Yoshimura

Keyword(s):

Incident Wave ◽

Angular Width ◽

X Ray Diffraction ◽

Experimental Conditions ◽

Acta Cryst ◽

Low Contrast ◽

X Ray ◽

Moiré Fringes ◽

Wide Range ◽

Fringe Patterns

Using a theory of X-ray diffraction moiré fringes developed in a previous paper, labelled Part I [Yoshimura (2015). Acta Cryst. A71, 368–381], the X-ray moiré images of a silicon bicrystal having a weak curvature strain and an interspacing gap, assumed to be integrated for an incident-wave angular width, are simulation-computed over a wide range of crystal thicknesses and incident-wave angular width, likely under practical experimental conditions. Along with the simulated moiré images, the graphs of characteristic quantities on the moiré images are presented for a full understanding of them. The treated moiré images are all of rotation moiré. Mo Kα1 radiation and the 220 reflection were assumed in the simulation. The results of this simulation show that fringe patterns, which are significantly modified from simple straight fringes of rotation moiré, appear in some ranges of crystal thicknesses and incident-wave angular width, due to a combined effect of Pendellösung oscillation and an added phase difference from the interspacing gap, under the presence of a curvature strain. The moiré fringes which slope to the perpendicular direction to the diffraction vector in spite of the assumed condition of rotation moiré, and fringe patterns where low-contrast bands are produced with a sharp bend of fringes arising along the bands are examples of the modified fringe pattern. This simulation study provides a wide theoretical survey of the type of bicrystal moiré image produced under a particular condition.

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Charge Compensation in Europium-Doped Hafnia Nanoparticles: Solvothermal Synthesis and Colloidal Dispersion

Crystals ◽

10.3390/cryst11091042 ◽

2021 ◽

Vol 11 (9) ◽

pp. 1042

Author(s):

Xavier H. Guichard ◽

Francesco Bernasconi ◽

Alessandro Lauria

Keyword(s):

Low Temperature ◽

Hafnium Oxide ◽

Aqueous Media ◽

Charge Compensation ◽

Colloidal Dispersion ◽

X Ray Diffraction ◽

X Ray ◽

Wide Range ◽

Direct Formation ◽

Enhanced Luminescence

Effective charge compensation of europium in hafnium oxide nanoparticles was achieved at low temperature, allowing high doping incorporation (up to 6 at.%) and enhanced luminescence. The efficiency of the incorporation and charge compensation was confirmed by scanning electron microscope energy dispersive X-ray spectroscopy and powder X-ray diffraction measurements. Despite the known polymorphism of hafnium oxide, when doped to a concentration above 3 at.%, only the pure monoclinic phase was observed up to 6 at.% of europium. Furthermore, the low-temperature solvothermal route allowed the direct formation of stable dispersions of the synthesized material over a wide range of concentrations in aqueous media. The dispersions were studied by diffuse light scattering (DLS) to evaluate their quality and by photoluminescence to investigate the incorporation of the dopants into the lattice.

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In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

10.26434/chemrxiv.13252544 ◽

2020 ◽

Author(s):

Stephen Shearan ◽

Jannick Jacobsen ◽

Ferdinando Costantino ◽

Roberto D’Amato ◽

Dmitri Novikov ◽

...

Keyword(s):

Crystal Growth ◽

Metal Organic Frameworks ◽

Building Blocks ◽

Nucleation And Growth ◽

X Ray Diffraction ◽

X Ray ◽

Rate Determining Step ◽

Wide Range ◽

Metal Organic

We report on the results of a thorough in situ synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds in situ in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO3) and amount of the coordination modulator acetic acid (AcOH). When only HNO3 is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO3, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO3 slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO3 favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO3. Based on these in situ results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

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The Effect of Zinc Content on n-Pentane Isomerisation Over Zn–S2O82–/ZrO2–Al2O3 Catalyst

Progress in Reaction Kinetics and Mechanism ◽

10.3184/146867816x14696245116981 ◽

2017 ◽

Vol 42 (1) ◽

pp. 23-29

Author(s):

Hua Song ◽

Shengnan Li ◽

Hualin Song ◽

Feng Li ◽

Huapeng Cui

Keyword(s):

Zinc Content ◽

Space Velocity ◽

X Ray Diffraction ◽

Sulfate Ions ◽

X Ray ◽

Weight Hourly Space Velocity ◽

Mass Fractions ◽

Crystallite Sizes ◽

Temperature Programmed ◽

Al2o3 Catalyst

A number of Zn–S2O82–/ZrO2–Al2O3 (Zn( x)–SZA) catalysts with different Zn mass fractions were synthesised and characterised by using X-ray diffraction, the Brunauer–Emmett–Teller method, and H2 temperature-programmed reduction. The structure and isomerisation performance of Zn( x)–SZA catalysts were studied using n-pentane as a probe reaction. The results showed that a pure tetragonal ZrO2 phase was formed on Zn( x)–SZA, and the ZrO2 crystallite sizes of the tetragonal phase increased in the order: Zn(0.5)–SZA < Zn(1.0)–SZA < Zn(1.5)–SZA < Zn(2.0)–SZA < SZA. Zn can strengthen the interaction between persulfate ions and the support, promote the formation of stronger acidity, lead to a better dispersion of sulfate ions on the surface, and improve the redox performance of the catalysts. The Zn(1.0)–SZA catalyst exhibited the best catalytic activity for n-pentane isomerisation. At a temperature of 170 °C, a reaction pressure of 2.0 MPa, a molar H2/ n-pentane ratio of 4:1, and a weight hourly space velocity of 1.0 h−1, the isopentane yield reached 58.0%.

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

MRS Proceedings ◽

10.1557/proc-395-319 ◽

1995 ◽

Vol 395 ◽

Cited By ~ 2

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).

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Investigation of Amorphous/Crystalline State in Cu-Hf-Al Alloys

Materials Science Forum ◽

10.4028/www.scientific.net/msf.649.87 ◽

2010 ◽

Vol 649 ◽

pp. 87-92

Author(s):

E. Nagy ◽

Viktória Rontó ◽

Jenő Sólyom ◽

András Roósz

Keyword(s):

Amorphous Alloys ◽

Great Influence ◽

Amorphous State ◽

High Strength ◽

Al Alloys ◽

X Ray Diffraction ◽

X Ray ◽

Wide Range ◽

Different Shapes ◽

Important Purpose

Cu-Hf-Al alloys are considered to be relatively new ones among Cu-based bulk amorphous alloys. Cu-Hf-Al alloys have high strength in amorphous state and this property makes many applications feasible for the industry. During the production of amorphous alloys the most important purpose is to produce them in the biggest diameter to make them suitable for a wide range of applications. The circumstances of the production process have a great influence on the developing structure. In the present work solidification of Cu-Hf-Al alloys were investigated. The alloys were cast into different shapes with different Al contents with special regard to the appearance of the amorphous/crystalline structure. The appearance and the structure of crystalline phases were determined by X-ray diffraction and X-ray, DSC and metallographic measurements were used to investigate the developing structure.

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