scholarly journals Synthesis and Composition Study of Electrochemically Deposited Ni-P Coating with Increased Surface Area

Coatings ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1071
Author(s):  
Sergey S. Perevoznikov ◽  
Ilya V. Yakovlev ◽  
Ludmila S. Tsybulskaya ◽  
Olga B. Lapina
Keyword(s):  
Phase Composition ◽  
Surface Area ◽  
Elevated Temperatures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Turn On ◽  
Nickel Phosphides ◽  
Electrochemically Deposited ◽  
Composition Study ◽  
Binary Compounds

Nickel phosphides NixPy are a promising family of binary compounds that have shown much promise in various fields of technology, including energy storage, light absorption and heterogeneous catalysis in the reactions of biomass hydrogenation. The performance of NixPy-containing materials depends greatly on their morphology and phase composition and, in turn, on the synthesis technique. In this work, we have employed the electroplating approach to synthesize a Ni-P coating, which was treated with nitric acid in order to develop its surface area and enrich it with phosphorus. We have employed scanning electron microscopy, X-ray diffraction and 31P nuclear magnetic resonance techniques to characterize the particles separated from the coating with ultrasound for the convenience of the study. According to experimental data, the obtained powder contained a mixture of Ni3P and phosphorus oxides, which transformed into nickel phosphide phases richer with phosphorus, such as Ni5P2 and Ni12P5, after treatment at elevated temperatures. Thus, we have demonstrated that electroplating followed by acid treatment is a feasible approach for the synthesis of Ni-P coatings with increased surface area and variable phase composition.

scholarly journals X Preparation and Characterization of Carbon-Based Composite Nanofibers for Supercapacitor

2017 ◽  
Vol 17 (2) ◽  
pp. 129-134 ◽  
Author(s):  
Dawei Gao ◽  
Lili Wang ◽  
Chunxia Wang ◽  
Yuping Chang ◽  
Pibo Ma
Keyword(s):  
Carbon Nanotubes ◽  
Phase Composition ◽  
Electron Microscope ◽  
Surface Area ◽  
Composite Nanofibers ◽  
Carbon Composite ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

Abstract Polyacrylonitrile (PAN)/Co(OAc)2/carbon nanotubes (CNTs) composite nanofibers were fabricated via electrospinning with N,N-dimethylformamide (DMF) as solvent, and by carbonization and activation of the above precursor nanofibers, porous carbon composite nanofibers were successfully obtained. Scanning electron microscope, X-ray diffraction, ASAP 2020, and Solartron 1470 were used to characterize the surface morphology, the phase composition, specific surface area, and electrochemical property of the nanofibers, respectively. The result showed that some of the fibers were broken after sintering, and the surface area and pore volume of the porous C/Cu/CNTs were 771 m2/g and 0.347 cm3/g, respectively. The specific capacitance of the composite nanofibers reached up to 210 F/g at the current density of 1.0 A/g. Its energy density and power density were 3.1 Wh/Kg and 2,337 W/Kg, respectively, at the current of 0.5 and 5 mA.

Control of the phase composition of advanced calcium phosphates using an x-ray diffractometer with a curved position-sensitive detector

2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov
Keyword(s):  
Phase Composition ◽  
Calcium Phosphates ◽  
Position Sensitive Detector ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Impurity Phases ◽  
Position Sensitive ◽  
Diffraction Peaks ◽  
Diffraction Patterns

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.

Formation of nanoscale sodium dodecahydro-closo- dodecaborate Na2[B12H12] on silicate matrix surface

2019 ◽  
Vol 484 (1) ◽  
pp. 41-43
Author(s):  
E. A. Malinina ◽  
V. K. Skachkova ◽  
I. V. Kozerozhets ◽  
V. V. Avdeeva ◽  
L. V. Goeva ◽  
...  
Keyword(s):  
Phase Composition ◽  
Ammonium Salt ◽  
Liquid Glass ◽  
Silicate Matrix ◽  
X Ray Diffraction ◽  
X Ray ◽  
Salt Sample ◽  
Matrix Surface

The method of nanoscaled sodium dodecahydro-closo-dodecaborate Na2[B12H12] synthesis is presented. The composite is heated to 200°C to yield the desired product, forming with the introduction of triethyl- ammonium salt [Et3NH]2[B12H12] into the silicate matrix of a sodium liquid glass. The morphology and phase composition of the synthesized sample are studied through SEM and X-ray diffraction methods, in comparison to those of a standard salt sample Na2[B12H12]. Based on the obtained data, the sample under study is an amorphous composite, on the surface of which nanoscale crystals of Na2[B12H12] form.

The Application of X-Ray Diffraction at Elevated Temperatures to Study the Mechanism of Formation of Sodium Tripolyphosphate

1961 ◽  
Vol 5 ◽  
pp. 276-284
Author(s):  
E. L. Moore ◽  
J. S. Metcalf
Keyword(s):  
High Temperature ◽  
Low Temperature ◽  
Amorphous Phase ◽  
Elevated Temperatures ◽  
Sodium Tripolyphosphate ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Temperature Form ◽  
High Temperature Form

AbstractHigh-temperature X-ray diffraction techniques were employed to study the condensation reactions which occur when sodium orthophosphates are heated to 380°C. Crystalline Na4P2O7 and an amorphous phase were formed first from an equimolar mixture of Na2HPO4·NaH2PO4 and Na2HPO4 at temperatures above 150°C. Further heating resulted in the formation of Na5P3O10-I (high-temperature form) at the expense of the crystalline Na4P4O7 and amorphous phase. Crystalline Na5P3O10-II (low-temperature form) appears after Na5P3O10-I.Conditions which affect the yield of crystalline Na4P2O7 and amorphous phase as intermediates and their effect on the yield of Na5P3O10 are also presented.

scholarly journals Hydrochloric Acid Modification and Lead Removal Studies on Naturally Occurring Zeolites from Nevada, New Mexico, and Arizona

Processes ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 1238
Author(s):  
Garven M. Huntley ◽  
Rudy L. Luck ◽  
Michael E. Mullins ◽  
Nick K. Newberry
Keyword(s):  
New Mexico ◽  
Surface Area ◽  
Bet Surface Area ◽  
Lead Removal ◽  
X Ray Diffraction ◽  
Sem Images ◽  
X Ray ◽  
Naturally Occurring ◽  
27Al Mas Nmr ◽  
Modified Zeolites

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.

scholarly journals A Highly Selective Turn-On Fluorescent Probe for the Detection of Zinc

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3825
Author(s):  
Ling-Yi Shen ◽  
Xiao-Li Chen ◽  
Xian-Jiong Yang ◽  
Hong Xu ◽  
Ya-Li Huang ◽  
...  
Keyword(s):  
High Selectivity ◽  
Fluorescence Probe ◽  
Stoichiometric Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Turn On ◽  
Imine Nitrogen ◽  
System A ◽  
Plot Analysis ◽  
L System

A novel turn-on fluorescence probe L has been designed that exhibits high selectivity and sensitivity with a detection limit of 9.53 × 10−8 mol/L for the quantification of Zn2+. 1H-NMR spectroscopy and single crystal X-ray diffraction analysis revealed the unsymmetrical nature of the structure of the Schiff base probe L. An emission titration experiment in the presence of different molar fractions of Zn2+ was used to perform a Job’s plot analysis. The results showed that the stoichiometric ratio of the complex formed by L and Zn2+ was 1:1. Moreover, the molecular structure of the mononuclear Cu complex reveals one ligand L coordinates with one Cu atom in the asymmetric unit. On adding CuCl2 to the ZnCl2/L system, a Cu-Zn complex was formed and a strong quenching behavior was observed, which inferred that the Cu2+ displaced Zn2+ to coordinate with the imine nitrogen atoms and hydroxyl oxygen atoms of probe L.

Phase composition depth profiles using spatially resolved energy dispersive X-ray diffraction

2004 ◽  
Vol 37 (6) ◽  
pp. 967-976 ◽  
Author(s):  
Andrew C. Jupe ◽  
Stuart R. Stock ◽  
Peter L. Lee ◽  
Nikhila N. Naik ◽  
Kimberly E. Kurtis ◽  
...  
Keyword(s):  
Phase Composition ◽  
Spatial Resolution ◽  
Zinc Coating ◽  
High Energy ◽  
Sulfate Attack ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
X Ray ◽  
Spatially Resolved ◽  
Composition Profiles

Spatially resolved energy dispersive X-ray diffraction, using high-energy synchrotron radiation (∼35–80 keV), was used nondestructively to obtain phase composition profiles along the radii of cylindrical cement paste samples to characterize the progress of the chemical changes associated with sulfate attack on the cement. Phase distributions were acquired to depths of ∼4 mm below the specimen surface with sufficient spatial resolution to discern features less than 200 µm thick. The experimental and data analysis methods employed to obtain quantitative composition profiles are described. The spatial resolution that could be achieved is illustrated using data obtained from copper cylinders with a thin zinc coating. The measurements demonstrate that this approach is useful for nondestructively visualizing the sometimes complex transformations that take place during sulfate attack on cement-based materials. These transformations can be spatially related to microstructure as seen by computed microtomography.

Physico-Chemical and Morphological Changes of Sayong Kaolinite Clay Treated with Sulphuric Acid for Enzyme Immobilization

2013 ◽  
Vol 832 ◽  
pp. 589-595 ◽  
Author(s):  
N.A. Edama ◽  
A. Sulaiman ◽  
K.H. Ku Hamid ◽  
M.N. Muhd Rodhi ◽  
Mohibah Musa ◽  
...  
Keyword(s):  
Surface Area ◽  
Sulphuric Acid ◽  
Enzyme Immobilization ◽  
Morphological Changes ◽  
Chemical Properties ◽  
X Ray Diffraction ◽  
Kaolinite Clay ◽  
X Ray ◽  
Mineral Oxides ◽  
Physico Chemical

This study analyzed the effects of sulphuric acid (H2SO4) treatment on pysico-chemical properties and morphological changes of clay obtained from Sg. Sayong, Perak. The clay was ground and sieved to <150μm and treated with different concentrations of H2SO4. The treatment was completed by refluxing the clay with different concentration of H2SO4 (1M, 5M and 10M ) at 100 °C for 4 hours and followed by calcination at 500 °C for 1 hour. The physic-chemical properties and morphological changes of the untreated and treated clay were compared using Surface Area Analyser, X-Ray Diffraction (XRD), Field Emission Scanning Electron Micrograph (FESEM), X-Ray Diffraction (XRD) and Fourier Transformed Infrared Spectroscopy (FTIR). The results showed that acid treatment of 5M increased the surface area from 25 m2/g to 75 m2/g and the pore volume increased from 0.1518 cc/g to 0.3546 cc/g. The nanopore size of the clay decreased from 24.8 nm to 19.4 nm after treated with acid. This can be explained due to the elimination of the exchangeable cations and generation of microporosity. The results of XRF showed SiO2 increased from 58.34% to 74.52% and Al2O3 reduced from 34.6% to 18.31%. The mineral oxides such as Fe2O3, MgO, CaO, K2O and TiO2 also reduced. This concluded that H2SO4 treatment has led to significant removal of octahedral Al3+, Fe3+ cations and other impurities. In conclusion, this study showed the physico-chemical properties and morphology of Sayong clay were improved once treated with H2SO4 and therefore suggests better supporting material for enzyme immobilization.

Hydrothermal Treatment of Coprecipitated YSZ Powders

2010 ◽  
Vol 660-661 ◽  
pp. 983-988 ◽  
Author(s):  
Alexander Rodrigo Arakaki ◽  
Walter Kenji Yoshito ◽  
Valter Ussui ◽  
Dolores Ribeiro Ricci Lazar
Keyword(s):  
Surface Area ◽  
Hydrothermal Treatment ◽  
Gas Adsorption ◽  
X Ray Diffraction ◽  
Electronic Microscopy ◽  
Immersion Method ◽  
Cubic Symmetry ◽  
X Ray ◽  
Granulometric Analysis ◽  
Symmetry Surface

Zirconia stabilized with 8.5 mol% yttria (YSZ) were synthesized by coprecipitation and resulting gels were hydrothermallly treated at 200°C and 220 PSI for 4, 8 and 16 hours. Products were oven dried at 70°C for 24 hours, isostatically pressed as pellets and sintered at 1500 °C for 1 hour. Powders were characterized for surface area with N2 gas adsorption, X-ray diffraction, laser diffraction granulometric analysis and scanning and transmission electronic microscopy. Density of ceramics was measured by an immersion method based on the Archimedes principle. Results showed that powders dried at 70°C are amorphous and after treatment has tetragonal/cubic symmetry. Surface area of powders presented a significant reduction after hydrothermal treatment. Ceramics prepared from hydrothermally treated powders have higher green density but sintered pellets are less dense when compared to that made with powders calcined at 800°C for 1 hour due to the agglomerate state of powders. Solvothermal treatment is a promising procedure to enhance density.

Synthesis of CaWO4:(Eu3+,Tb3+) Thin Films by a Two-Step Method at Room Temperature

2013 ◽  
Vol 710 ◽  
pp. 170-173
Author(s):  
Lian Ping Chen ◽  
Yuan Hong Gao
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Phase Composition ◽  
Room Temperature ◽  
Electrochemical Techniques ◽  
Luminescent Properties ◽  
X Ray Diffraction ◽  
Step Method ◽  
X Ray ◽  
Rare Earth Doped

It is hardly possible to obtain rare earth doped CaWO4thin films directly through electrochemical techniques. A two-step method has been proposed to synthesize CaWO4:(Eu3+,Tb3+) thin films at room temperature. X-ray diffraction, energy dispersive X-ray analysis, spectrophotometer were used to characterize their phase, composition and luminescent properties. Results reveal that (Eu3+,Tb3+)-doped CaWO4films have a tetragonal phase. When the ratio of n (Eu)/n (Tb) in the solution is up to 3:1, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Tb element; on the contrary, when the ratio in the solution is lower than 1:4, CaWO4:(Eu3+,Tb3+) thin film will be enriched with Eu element. Under the excitation of 242 nm, sharp emission peaks at 612, 543, 489 and 589 nm have been observed for CaWO4:(Eu3+,Tb3+) thin films.

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