Chemical Synthesis and Properties of Layered Co1-yNiyO2-δOxides (0≤y≤1)

2000 ◽  
Vol 658 ◽  
Author(s):  
A. Manthiram ◽  
R. V. Chebiam ◽  
F. Prado
Keyword(s):  
Layer Structure ◽  
Magnetic Data ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
X Ray ◽  
Ni Content ◽  
Wet Chemical ◽  
Oxide Ions ◽  
Structure Layer

ABSTRACTLayered Co1-yNiyO2-δ oxides with 0≤y≤1 have been synthesized by chemically extracting lithium from LiNi1-yCoyO2 with NO2PF6 at ambient temperature. The samples have been characterized by X-ray diffraction, wet-chemical analyses, infrared spectroscopy, and magnetic susceptibility measurements. While NiO2-δ retains the initial O3 (CdCl2 structure) layer structure of LiNiO2, CoO2-δ consists of a mixture of P3 and O1 (CdI2 structure) phases that are formed by a sliding of the oxide ions in the initial O3 structure. CoO2-δ and NiO2-δ have oxygen contents of, respectively, 1.67 and 1.95 and the oxygen content increases with increasing Ni content, y, in Co1-yNiyO2-δ. While CoO2-δ exhibits metallic conductivity as revealed by theabsence of absorption bands in the infrared spectrum, NiO2-δ exhibits semiconducting behavior due to a completely filled t2g band. Magnetic data reveal a transition from antiferromagnetic to ferromagnetic correlations as the Ni content in Co1-yNiyO2-δ increases.

scholarly journals Spectroscopic and Crystal-Chemical Features of Sodalite-Group Minerals from Gem Lazurite Deposits

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1042
Author(s):  
Nikita V. Chukanov ◽  
Anatoly N. Sapozhnikov ◽  
Roman Yu. Shendrik ◽  
Marina F. Vigasina ◽  
Ralf Steudel
Keyword(s):  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Visible Spectroscopy ◽  
X Ray ◽  
Spin Resonance ◽  
Incommensurate Modulation ◽  
Wet Chemical ◽  
Uv Visible ◽  
Diffraction Patterns ◽  
Subordinate Role

Five samples of differently colored sodalite-group minerals from gem lazurite deposits were studied by means of electron microprobe and wet chemical analyses, infrared, Raman, electron spin resonance (ESR) and UV-Visible spectroscopy, and X-ray diffraction. Various extra-framework components (SO42−, S2− and Cl− anions, S3•−, S2•− and SO3•− radical anions, H2O, CO2, COS, cis- as well as trans- or gauche-S4 neutral molecules have been identified. It is shown that S3•− and S4 are the main blue and purple chromophores, respectively, whereas the S2•− yellow chromophore and SO3•− blue chromophore play a subordinate role. X-ray diffraction patterns of all samples of sodalite-group minerals from lazurite deposits studied in this work contain superstructure reflections which indicate different kinds of incommensurate modulation of the structures.

Carbon incorporation in plumbogummite-group minerals

2011 ◽  
Vol 75 (1) ◽  
pp. 145-158 ◽  
Author(s):  
I. E. Grey ◽  
F. L. Shanks ◽  
N. C. Wilson ◽  
W. G. Mumme ◽  
W. D. Birch
Keyword(s):  
Organic Carbon ◽  
Rietveld Analysis ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Carbon Incorporation ◽  
X Ray ◽  
Wet Chemical ◽  
Difference Fourier ◽  
Large Contraction ◽  
Direct Confirmation

AbstractNon-stoichiometric, carbon-containing crandallite from Guatemala and plumbogummite from Cumbria have been characterized using electron microprobe (EMPA) and wet-chemical analyses, Rietveld analysis of powder X-ray diffraction (PXRD) patterns, and infrared (IR), Raman and cathodoluminescence (CL) spectroscopies. The samples contain 11.0 and 4.8 wt.% CO2, respectively. The IR spectra for both samples show a doublet in the range 1410–1470 cm–1, corresponding to CO3 vibrations. Direct confirmation of CO3 replacing PO4 was obtained from difference Fourier maps in the Rietveld analysis. Carbonate accounts for 67% of the C in the plumbogummite and 20% of the C in the Guatemalan crandallite, the remainder being present as nano-scale organic carbon. The CO3 substitution for PO4 is manifested in a large contraction of the tetrahedral volume (14–19%) and by a contraction of the a axis, analogous to observations for carbonate-containing fluorapatites. Stoichiometric crandallite from Utah was characterized using the same methods, for comparison with the non-stoichiometric, carbon-bearing phases.

scholarly journals Characterization of ferrite nanoparticles for preparation of biocomposites

2017 ◽  
Vol 8 ◽  
pp. 1257-1265 ◽  
Author(s):  
Urszula Klekotka ◽  
Magdalena Rogowska ◽  
Dariusz Satuła ◽  
Beata Kalska-Szostko
Keyword(s):  
Chemical Method ◽  
Ferrite Nanoparticles ◽  
Chemical Activity ◽  
Nominal Composition ◽  
X Ray Diffraction ◽  
Wet Chemical Method ◽  
X Ray ◽  
Transmission Electron ◽  
Wet Chemical

Ferrite nanoparticles with nominal composition Me0.5Fe2.5O4 (Me = Co, Fe, Ni or Mn) have been successfully prepared by the wet chemical method. The obtained particles have a mean diameter of 11–16 ± 2 nm and were modified to improve their magnetic properties and chemical activity. The surface of the pristine nanoparticles was functionalized afterwards with –COOH and –NH2 groups to obtain a bioactive layer. To achieve our goal, two different modification approaches were realized. In the first one, glutaraldehyde was attached to the nanoparticles as a linker. In the second one, direct bonding of such nanoparticles with a bioparticle was studied. In subsequent steps, the nanoparticles were immobilized with enzymes such as albumin, glucose oxidase, lipase and trypsin as a test bioparticles. The characterization of the nanoparticles was acheived by transmission electron microscopy, X-ray diffraction, energy dispersive X-ray and Mössbauer spectroscopy. The effect of the obtained biocomposites was monitored by Fourier transform infrared spectroscopy. The obtained results show that in some cases the use of glutaraldehyde was crucial (albumin).

Effect of Yttria-Stabilized Zirconia Concentration in an Electroless Bath on Microstructure and Composition of Ni/Yttria-Stabilized Zirconia Nanocomposite

2021 ◽  
Vol 21 (11) ◽  
pp. 5592-5602
Author(s):  
Samira Almasi ◽  
Ali Mohammad Rashidi
Keyword(s):  
High Performance ◽  
Yttria Stabilized Zirconia ◽  
X Ray Diffraction ◽  
Stabilized Zirconia ◽  
Nickel Ion ◽  
Nanocomposite Particles ◽  
X Ray ◽  
Ni Content ◽  
Naoh Solution ◽  
Average Size

The effect of the yttria-stabilized zirconia (YSZ) nanoparticle loading in an electro-less bath was considered as one of the vital synthesis variables for control Ni content and microstructure of prepared nanocomposite particles, which are two crucial factors to achieving high-performance SOFC anode. Nanocomposite particles were prepared using a simple electroless method without any expensive pretreatment of sensitizing by Sn2+ ions as well as activating by Pd2+ ions that are usually used to apply nickel coating on the surface of a non-conductive substrate. The process was performed by adding YSZ nanoparticles into NaOH solution, separating them from the solution by the centrifugal method, then providing several water-based nanofluids with different concentrations of activated YSZ nanoparticles, mixing them with NiCI2 solution, followed by adding the hydrazine and then NaOH solution. X-ray diffraction and scanning electron microscopy coupled with energy dispersive X-ray analysis were used to analyze the prepared nanocomposite particles. It is observed that after adding YSZ nanoparticles into the NaOH solution, the pH of the solution varied gradually from a starting pH of 10.2 to 9. Also, by increasing the YSZ nanoparticles loading in the electroless bath from 76 mg/l to 126 mg/l, the grain size of Ni deposits, the Ni content and the average size of the prepared nanocomposite particles decreased. The electrochemical mechanism previously proposed for the nickel ion reduction was modified, and a novel analytical model was proposed for variation of the efficiency of Ni deposition with YSZ nanoparticles loading.

A (4,4)-connected zinc(II) coordination polymer constructed with the flexible 2-carboxy phenoxyacetate ligand: synthesis, conformation alteration and fluorescent properties

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Jun-Xia Li ◽  
Tian Zhang ◽  
He-Jun Chen ◽  
Zhong-Xiang Du
Keyword(s):  
Coordination Polymer ◽  
Hydrothermal Reaction ◽  
Layer Structure ◽  
Fluorescence Emission ◽  
Phenoxyacetic Acid ◽  
X Ray Diffraction ◽  
Fluorescent Properties ◽  
Sulfate Heptahydrate ◽  
X Ray ◽  
Related Compounds

Abstract A new binary ZnII coordination polymer, [Zn(2-cpa)(H2O)] n (2D-Zn) has been prepared by a 120 °C hydrothermal reaction of zinc(II) sulfate heptahydrate and 2-carboxy phenoxyacetic acid (2-H2cpa) in the presence of potassium hydroxide. Single-crystal X-ray diffraction analysis shows that the ZnII ion is located in a deformed ZnO6 octahedron bonded by one water and three 2-carboxy phenoxyacetate (2-cpa) ligands. The 2-cpa exhibits pentadentate double bridging chelate-μ 3 coordination mode and connects adjacent ZnII ions to generate a corrugated (4,4)-connected layer structure. The structures, conformation of 2-cpa and photoluminescence spectra for 2D-Zn have been carefully analyzed and compared with its two closely related compounds ̶ 1D [Zn(2-cpa)(H2O)] n (1D-Zn) and mononuclear [Zn(2-cpa)(H2O)3] (0D-Zn). The results showed that the conformation of 2-cpa in 2D-Zn has the maximum alteration and the corresponding fluorescence emission peak of 2D-Zn has the largest red-shift of 62 nm compared with that of free 2-H2cpa.

Synthesis of Galactomannan Sulfate-Citrate

2022 ◽  
Vol 1049 ◽  
pp. 218-223
Author(s):  
Aleksandr S. Kazachenko ◽  
Yuriy N. Malyar ◽  
Anna S. Kazachenko
Keyword(s):  
Biological Activity ◽  
Ftir Spectroscopy ◽  
X Ray Diffraction ◽  
Absorption Bands ◽  
X Ray ◽  
Mixed Ester ◽  
First Time ◽  
Derivatives Of

Sulfated derivatives of polysaccharides have anticoagulant, hypolipedimic and other biological activity. In this work, a complex mixed ester of galactomannan, its sulfate-citrate, was obtained for the first time. The introduction of citrate and sulfate groups was proved by FTIR spectroscopy by the appearance of corresponding absorption bands. It was shown by X-ray diffraction that the introduction of the citrate group leads to the amorphization of the galactomannan structure.

Study on Synthesis of Calcium Phosphate Biomaterials Containing SMB

2007 ◽  
Vol 330-332 ◽  
pp. 1033-1036 ◽  
Author(s):  
M.H. Li ◽  
Shu Xin Qu ◽  
R. Shen ◽  
N. Yao ◽  
P.D. Ren ◽  
...  
Keyword(s):  
Calcium Phosphate ◽  
Salvia Miltiorrhiza ◽  
Reaction System ◽  
Absorption Peak ◽  
X Ray Diffraction ◽  
Wet Chemical Method ◽  
Obvious Effect ◽  
X Ray ◽  
Wet Chemical ◽  
Wet Synthesis

Calcium phosphate (CaP) biomaterials containing Chinese medicine, Danshen (Salvia Miltiorrhiza Bunge, SMB), have been synthesized in our previous study via the wet chemical method. However, CaP biomaterials were generally synthesized in the alkaline solution. The purpose of the present study was to investigate the effect of pH on SMB and the influence of SMB on the synthesis of CaP biomaterials. The SMB solutions of different pH from 5.0 to 10.0, were scanned with the UV-VIS spectrophotometer (UV-VIS) in the wavelength ranged from 200.00 to 400.00 nm. CaP biomaterials containing SMB were synthesized from (NH4)2HPO4, Ca(NO3)2, NH4OH and SMB. The filtrates of the wet synthesis of CaP biomaterials containing SMB were measured by UV-VIS. The synthesized CaP biomaterials containing SMB were characterized by the X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR). The results showed that the maximum absorption peak appeared at 281.00 nm for solutions of pH 5.0, 6.0 and 7.0. Although there were a new absorption peaks as the pH were 8.0 and 9.0, the absorption curves of SMB became similar to that of SMB as pH at 7.0 after the pH were readjusted to 7.0. The absorption peak appeared an Einstein shift to 347.00 nm at pH 10.0, which did not return to 281.00 nm when the pH of SMB solution was readjusted to 7.0. The absorption peak of filtrates containing SMB of CaP biomaterials reaction system was still at 281.00 nm when their pH was 7.0 and 8.0. Moreover, SMB had no obvious effect on the phase component and functional groups of products. Hence, it could be predicted that calcium phosphate biomaterials containing SMB, such as DCPD and TCP containing SMB, which could be prepared at the pH ranged from 5.0 to 9.0.

The crystal structure of gatehouseite

2011 ◽  
Vol 75 (6) ◽  
pp. 2823-2832
Author(s):  
P. Elliott ◽  
A. Pring
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Direct Methods ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
X Ray ◽  
Manganese Phosphate ◽  
Phosphate Mineral ◽  
Unit Formula

AbstractThe crystal structure of the manganese phosphate mineral gatehouseite, ideally Mn52+(PO4)2(OH)4, space group P212121, a = 17.9733(18), b = 5.6916(11), c = 9.130(4) Å, V= 933.9(4) Å3, Z = 4, has been solved by direct methods and refined from single-crystal X-ray diffraction data (T = 293 K) to an R index of 3.76%. Gatehouseite is isostructural with arsenoclasite and with synthetic Mn52+(PO4)2(OH)4. The structure contains five octahedrally coordinated Mn sites, occupied by Mn plus very minor Mg with observed <Mn—O> distances from 2.163 to 2.239 Å. Two tetrahedrally coordinated P sites, occupied by P, Si and As, have <P—O> distances of 1.559 and 1.558 Å. The structure comprises two types of building unit. A strip of edge-sharing Mn(O,OH)6 octahedra, alternately one and two octahedra wide, extends along [010]. Chains of edge- and corner-shared Mn(O,OH)6 octahedra coupled by PO4 tetrahedra extend along [010]. By sharing octahedron and tetrahedron corners, these two units form a dense three-dimensional framework, which is further strengthened by weak hydrogen bonding. Chemical analyses by electron microprobe gave a unit formula of (Mn4.99Mg0.02)Σ5.01(P1.76Si0.07(As0.07)Σ2.03O8(OH)3.97.

scholarly journals Alkali Fusion-Leaching Method For Comprehensive Processing Of Fly Ash

2017 ◽  
Vol 2 (2) ◽  
pp. 89 ◽  
Author(s):  
A.A. Shoppert ◽  
I.V. Loginova ◽  
L.I. Chaikin ◽  
D.A. Rogozhnikov
Keyword(s):  
Fly Ash ◽  
Power Plant ◽  
X Ray Diffraction ◽  
Water Leaching ◽  
X Ray ◽  
Comprehensive Utilization ◽  
Alkali Fusion ◽  
Wet Chemical ◽  
Promising Source ◽  
Comprehensive Processing

<p>Fly ash, composed of mullite, hematite, amorphous silica and quartz, is a promising source for the recovery of alumina and silica. Desilication with help of NaOH and alkali fusion-leaching method and utilization of alumina and silica in the fly ash for preparation of sodalite and silica white were explored in this research. The samples were characterized by using wet chemical analysis and X-ray diffraction. The optimal extraction of SiO<sub>2</sub> from Reftinskaya power plant fly ash was 46.2% with leaching at 95 <sup>o</sup>C for 3 h. Sodalite was synthesized at 200 °C for 1 h followed water leaching at 95 °C for 1 h. Silica white with specific surface area 180-220 m2/g was prepared by carbonation of the Na<sub>2</sub>SiO<sub>3</sub> solution at 40 <sup>o</sup>C for 90-120 min. The as-prepared silica has a purity of 98,8%.</p><p>The proposed method is suitable for the comprehensive utilization of the fly ash.</p>

scholarly journals THE INFLUENCE OF THE META-STABLE TRIPLE POINT SOLUTION OF MONOCALCIUM PHOSPHATE MONOHYDRATE UPON THE CLAY SEPARATES OF TWO ONTARIO SOILS

1963 ◽  
Vol 43 (2) ◽  
pp. 260-267
Author(s):  
A. F. MacKenzie ◽  
C. A. Campbell
Keyword(s):  
Electron Microscope ◽  
Triple Point ◽  
Thermal Analyses ◽  
Chemical Analyses ◽  
Clay Loam ◽  
X Ray Diffraction ◽  
Monocalcium Phosphate ◽  
X Ray ◽  
Point Solution ◽  
Soil Clay

Samples of material less than 2 μ in diameter were obtained from the surface horizon of a Guelph loam and of a Haldimand clay loam. These samples were subjected to six successive treatments with the meta-stable triple point solution of monocalcium phosphate monohydrate (MTPS) to simulate the environment near a dissolving superphosphate granule. Samples of montmorillonite and illite standard clays were also included. The dissolution losses in per cent were: Guelph clay 59.5, Haldimand clay 40.4, montmorillonite 3.4, and illite 8.1. Total chemical analyses, X-ray diffraction techniques, differential thermal analyses and electron microscope observations were used to determine the nature of these losses. In the soil clay separates, vermiculite and interstratified montmorillonite were more susceptible to the action of MTPS than were the illite or halloysite clay minerals.

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