scholarly journals Correlation between Structural and Transport Properties of Ca-Doped La Nickelates and Their Electrochemical Performance

Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 297
Author(s):  
Elena Pikalova ◽  
Vladislav Sadykov ◽  
Ekaterina Sadovskaya ◽  
Nikita Yeremeev ◽  
Alexander Kolchugin ◽  
...  
Keyword(s):  
Transport Properties ◽  
Oxygen Transport ◽  
Structural Features ◽  
Surface Reactivity ◽  
Excess Oxygen ◽  
Organic Nitrate ◽  
Oxygen Mobility ◽  
X Ray Diffraction ◽  
Cell Parameters ◽  
In Situ Xrd

This work presents the results from a study of the structure and transport properties of Ca-doped La2NiO4+δ. La2−xCaxNiO4+δ (x = 0–0.4) materials that were synthesized via combustion of organic-nitrate precursors and characterized by X-ray diffraction (XRD), in situ XRD using synchrotron radiation, thermogravimetric analysis (TGA) and isotope exchange of oxygen with C18O2. The structure was defined as orthorhombic (Fmmm) for x = 0 and tetragonal (I4/mmm) for x = 0.1–0.4. Changes that occurred in the unit cell parameters and volume as the temperature changed during heating were shown to be caused by the excess oxygen loss. Typical for Ruddlesden–Popper phases, oxygen mobility and surface reactivity decreased as the Ca content was increased due to a reduction in the over-stoichiometric oxygen content with the exception of x = 0.1. This composition demonstrated its superior oxygen transport properties compared to La2NiO4+δ due to the enhanced oxygen mobility caused by structural features. Electrochemical data obtained showed relatively low polarization resistance for the electrodes with a low Ca content, which correlates well with oxygen transport properties.

scholarly journals Lead-antimony sulfosalts from Tuscany (Italy). XVIII. New data on the crystal-chemistry of boscardinite

2017 ◽  
Vol 81 (1) ◽  
pp. 47-60 ◽  
Author(s):  
Cristian Biagioni ◽  
Yves Moëlo
Keyword(s):  
Single Crystal ◽  
Diffraction Study ◽  
Type Specimen ◽  
Structural Features ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Mineral Associations ◽  
Crystal Chemical Data ◽  
New Findings

AbstractBoscardinite, ideally TlPb4(Sb7As2)∑9S18, has been described recently as a new homeotypic derivative of baumhauerite, found at Monte Arsiccio mine, Apuan Alps, Tuscany, Italy. New findings of boscardinite in different mineral associations of this deposit have allowed the collection of new crystal-chemical data. Electron-microprobe analysis of the crystal used for the single-crystal X-ray diffraction study gave (in wt.%): Ag 1.81(5), Tl 12.60(21), Pb 17.99(12), Hg 0.14(5), As 9.36(12), Sb 33.60(27), S 23.41(30),Cl 0.06(1), total 98.97(100). On the basis of ∑Me= 14 apfu, it corresponds to Ag0.42Tl1.52Pb2.14Hg0.02(Sb6.82As3.08)∑9.90S18.04Cl0.04. With respect to the type specimen, these new findings are characterized by a strong Pb depletion, coupled with higher Tl contents, and a significant As enrichment. The single-crystal X-ray diffraction study of this (Tl,As)-enriched boscardinite confirms the structural features described for the type sample. The unit-cell parameters area= 8.1017(4),b= 8.6597(4),c= 22.5574(10) Å, α = 90.666(2), β = 97.242(2), γ = 90.850(2)°,V= 1569.63(12) Å3, space groupP̄1. The crystal structure was refined down toR1= 0.0285 on the basis of 6582 reflections withFo> 4σ(Fo). Arsenic is dominant in threeMeS3sites, compared to one in type boscardinite. The main As-enrichment is observed in the sartorite-type sub-layer. Owing to this chemical peculiarity, (Tl, As)-rich boscardinite shows alternation, alongb, of Sb-rich sites and As-rich sites; this feature represents the main factor controlling the 8 Å superstructure. The chemical variability of boscardinite is discussed; the Ag increase observed here gets closer to stoichiometric AgTl3Pb4(Sb14As6)∑20S36(Z= 1), against possible extension up to AgTl2Pb6(Sb15As4)∑19S36for type boscardinite.

scholarly journals The structure of kaliophilite KAlSiO4, a long-lasting crystallographic problem

IUCrJ ◽  
2020 ◽  
Vol 7 (6) ◽  
pp. 1070-1083 ◽  
Author(s):  
Enrico Mugnaioli ◽  
Elena Bonaccorsi ◽  
Arianna E. Lanza ◽  
Erik Elkaim ◽  
Virginia Diez-Gómez ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Rietveld Method ◽  
Structural Features ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Channel System ◽  
X Ray ◽  
Cell Parameters ◽  
Peak Broadening ◽  
Structure Solution

Kaliophilite is a feldspathoid mineral found in two Italian magmatic provinces and represents one of the 12 known phases with composition close to KAlSiO4. Despite its apparently simple formula, the structure of this mineral revealed extremely complex and resisted structure solution for more than a century. Samples from the Vesuvius–Monte Somma and Alban Hills volcanic areas were analyzed through a multi-technique approach, and finally the crystal structure of kaliophilite was solved using 3D electron diffraction and refined against X-ray diffraction data of a twinned crystal. Results were also ascertained by the Rietveld method using synchrotron powder intensities. It was found that kaliophilite crystallizes in space group P3 with unit-cell parameters a = 27.0597 (16), c = 8.5587 (6) Å, V = 5427.3 (7) Å3 and Z = 54. The kaliophilite framework is a variant of the tridymite topology, with alternating SiO4 and AlO4 tetrahedra forming sheets of six-membered rings (63 nets), which are connected along [001] by sharing the apical oxygen atoms. Considering the up (U) and down (D) orientations of the linking vertex, kaliophilite is the first framework that contains three different ring topologies: nine (1-3-5) (UDUDUD) rings, six (1-2-3) (UUUDDD) rings and twelve (1-2-4) (UUDUDD) rings. This results in a relatively open (19.9 tetrahedra nm−3) channel system with multiple connections between the double six-ring cavities. Such a framework requires a surprisingly large unit cell, 27 times larger than the cell of kalsilite, the simplest phase with the same composition. The occurrence of some Na for K substitution (3–10%) may be related to the characteristic structural features of kaliophilite. Micro-twinning, pseudo-symmetries and anisotropic hkl-dependent peak broadening were also detected, and they may account for the elusive character of the kaliophilite crystal structure.

Solid-state transformation of nanocrystalline phyllomanganate into tectomanganate: influence of initial layer and interlayer structure

2014 ◽  
Vol 70 (5) ◽  
pp. 828-838 ◽  
Author(s):  
Sylvain Grangeon ◽  
Bruno Lanson ◽  
Martine Lanson
Keyword(s):  
Ageing Time ◽  
Surface Reactivity ◽  
X Ray Diffraction ◽  
Solid State Transformation ◽  
Surface Complexes ◽  
Teller Distortion ◽  
X Ray ◽  
Cell Parameters ◽  
Decreasing Ph ◽  
Xrd Patterns

In surficial environments, the fate of many elements is influenced by their interactions with the phyllomanganate vernadite, a nano-sized and turbostratic variety of birnessite. To advance our understanding of the surface reactivity of vernadite as a function of pH, synthetic vernadite (δ-MnO2) was equilibrated at pH ranging from 3 to 10 and characterized structurally using chemical methods, thermogravimetry and modelling of powder X-ray diffraction (XRD) patterns. With decreasing pH, the number of vacant layer sites increases in the octahedral layers of δ-MnO2(from 0.14 per layer octahedron at pH 10 to 0.17 at pH 3), whereas the number of layer Mn3+is, within errors, equal to 0.12 per layer octahedron over the whole pH range. Vacant layer sites are capped by interlayer Mn3+sorbed as triple corner-sharing surface complexes (TC sites). The increasing number of interlayer Mn3+with decreasing pH (from 0.075 per layer octahedron at pH 10 to 0.175 at pH 3) results in the decrease of the average Mn oxidation degree (from 3.80 ± 0.01 at pH 10 to 3.70 ± 0.01 at pH 3) and in the lowering of the Na/Mn ratio (from 27.66 ± 0.20 at pH 10 to 6.99 ± 0.16 at pH 3). In addition, in-plane unit-cell parameters are negatively correlated to the number of interlayer Mn at TC sites and decrease with decreasing pH (fromb= 2.842 Å at pH 10 tob= 2.834 Å at pH 3), layer symmetry being systematically hexagonal witha=b× 31/2. Finally, modelling of X-ray diffraction (XRD) patterns indicates that crystallite size in theabplane and along thec* axis decreases with decreasing pH, ranging respectively from 7 nm to 6 nm, and from 1.2 nm to 1.0 nm (pH 10 and 3, respectively). Following their characterization, dry samples were sealed in polystyrene vials, kept in the dark, and re-analysed 4 and 8 years later. With ageing time and despite the dry state, layer Mn3+extensively migrates to the interlayer most likely to minimize steric strains resulting from the Jahn–Teller distortion of Mn3+octahedra. When the number of interlayer Mn3+at TC sites resulting from this migration reaches the maximum value of ∼ 1/3 per layer octahedron, interlayer species from adjacent layers share their coordination sphere, resulting in cryptomelane-like tunnel structure fragments (with a 2  × 2 tunnel size) with a significantly improved layer stacking order.

scholarly journals The crystal structure of dihydrodipicolinate reductase from the human-pathogenic bacteriumBartonella henselaestrain Houston-1 at 2.3 Å resolution

2016 ◽  
Vol 72 (12) ◽  
pp. 885-891 ◽  
Author(s):  
Ali R. Cala ◽  
Maria T. Nadeau ◽  
Jan Abendroth ◽  
Bart L. Staker ◽  
Alexandra R. Reers ◽  
...  
Keyword(s):  
Sodium Citrate ◽  
Bartonella Henselae ◽  
Three Dimensional ◽  
Structural Features ◽  
Cat Scratch Disease ◽  
X Ray Diffraction ◽  
Cell Parameters ◽  
Human Pathogenic Bacterium ◽  
Peg 4000 ◽  
Causative Bacterium

In bacteria, the second committed step in the diaminopimelate/lysine anabolic pathways is catalyzed by the enzyme dihydrodipicolinate reductase (DapB). DapB catalyzes the reduction of dihydrodipicolinate to yield tetrahydrodipicolinate. Here, the cloning, expression, purification, crystallization and X-ray diffraction analysis of DapB from the human-pathogenic bacteriumBartonella henselae, the causative bacterium of cat-scratch disease, are reported. Protein crystals were grown in conditions consisting of 5%(w/v) PEG 4000, 200 mMsodium acetate, 100 mMsodium citrate tribasic pH 5.5 and were shown to diffract to ∼2.3 Å resolution. They belonged to space groupP4322, with unit-cell parametersa= 109.38,b= 109.38,c= 176.95 Å.Rr.i.m.was 0.11,Rworkwas 0.177 andRfreewas 0.208. The three-dimensional structural features of the enzymes show that DapB fromB. henselaeis a tetramer consisting of four identical polypeptides. In addition, the substrate NADP+was found to be bound to one monomer, which resulted in a closed conformational change in the N-terminal domain.

Novel K/Mn phosphate hydrates, K2Mn3(H2O)2[P2O7]2 and KMn(H2O)2[Al2(PO4)3]: hydrothermal synthesis and crystal chemistry

2020 ◽  
Vol 76 (3) ◽  
pp. 302-310
Author(s):  
Galina V. Kiriukhina ◽  
Olga V. Yakubovich ◽  
Larisa V. Shvanskaya ◽  
Ekaterina M. Kochetkova ◽  
Olga V. Dimitrova ◽  
...  
Keyword(s):  
Hydrothermal Synthesis ◽  
Crystal Structures ◽  
Structural Features ◽  
X Ray Diffraction ◽  
Crystal Chemical Analysis ◽  
Cell Parameters ◽  
Paramagnetic Behaviour ◽  
New Compounds ◽  
Anionic Framework ◽  
Synthesis Experiment

Two novel K/Mn phosphate hydrates, namely, dipotassium trimanganese dipyrophosphate dihydrate, K2Mn3(H2O)2[P2O7]2, (I), and potassium manganese dialuminium triphosphate dihydrate, KMn(H2O)2[Al2(PO4)3], (II), were obtained in the form of single crystals during a single hydrothermal synthesis experiment. Their crystal structures were studied by X-ray diffraction. Both new compounds are members of the morphotropic series of phosphates with the following formulae: A 2 M 3(H2O)2[P2O7]2, where A = K, NH4, Rb or Na and M = Mn, Fe, Co or Ni, and AM 2+(H2O)2[M 3+ 2(PO4)3], where A = Cs, Rb, K, NH4 or (H3O); M 2+ = Mn, Fe, Co or Ni; and M 3+ = Al, Ga or Fe. A detailed crystal chemical analysis revealed correlations between the unit-cell parameters of the members of the series, their structural features and the sizes of the cations. It has been shown that a mixed type anionic framework is formed in (II) by aluminophosphate [(AlO2)2(PO4)2]∞ layers, with a cationic topology similar to the Si/Al-topology of the crystal structures of feldspars. A study of the magnetic susceptibility of (II) demonstrates a paramagnetic behaviour of the compound.

Structural Study of a new Compound Based on Acid 1,4-Cyclohexanedicarboxylic (1,4-CDC)

2010 ◽  
Vol 6 (1) ◽  
pp. 891-896
Author(s):  
Manel Halouani ◽  
M. Dammak ◽  
N. Audebrand ◽  
L. Ktari
Keyword(s):  
Aqueous Solution ◽  
Water Molecules ◽  
Carboxyl Group ◽  
X Ray Diffraction ◽  
Compound I ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Parameters ◽  
Cyclohexanedicarboxylic Acid

One nickel 1,4-cyclohexanedicarboxylate coordination polymers, Ni2 [(O10C6H4)(COO)2].2H2O  (I), was hydrothermally synthesized from an aqueous solution of Ni (NO3)2.6H2O, (1,4-CDC) (1,4-CDC = 1,4-cyclohexanedicarboxylic acid) and tetramethylammonium nitrate. Compound (I) crystallizes in the monoclinic system with the C2/m space group. The unit cell parameters are a = 20.1160 (16) Å, b = 9.9387 (10) Å, c = 6.3672 (6) Å, β = 97.007 (3) (°), V= 1263.5 (2) (Å3) and Dx= 1.751g/cm3. The refinement converged into R= 0.036 and RW = 0.092. The structure, determined by single crystal X-ray diffraction, consists of two nickel atoms Ni (1) and Ni (2). Lots of ways of which is surrounded by six oxygen atoms, a carboxyl group and two water molecules.

Transformation of Structure, Magnetic Properties and Microwave Absorption Capability in Nd-Doped Strontium Hexaferrite

2020 ◽  
Vol 855 ◽  
pp. 255-260
Author(s):  
Mukhtar Effendi ◽  
Efi Solihah ◽  
Candra Kurniawan ◽  
Wahyu Tri Cahyanto ◽  
Wahyu Widanarto
Keyword(s):  
Magnetic Properties ◽  
Microwave Absorption ◽  
Solid State Reaction Method ◽  
Strontium Hexaferrite ◽  
Basic Material ◽  
X Ray Diffraction ◽  
Cell Parameters ◽  
Tetragonal Crystal ◽  
Capability Analysis ◽  
Natural Iron

The synthesize of Nd3+-strontium hexaferrite magnetic material by the solid-state reaction method has been successfully carried out. This study aims to determine the effect of Nd3+ on the structure, magnetic properties, and microwave absorption capability of the material. Preparation of (1-x)SrO:xNd2O3:6Fe2O3 where x = 0, 10, 20, and 30 mol% using basic material in the form of SrCO3 powder, Nd2O3 powder and Fe3O4 from natural iron sand. The characterization includes the X-Ray Diffraction (XRD) examination to determine the crystal structure, the Scanning Electron Microscope (SEM) for exploring the surface morphology, Vibrating Sample Magnetometer (VSM) for the magnetic properties investigation of material, and Vector Network Analyzer (VNA) for microwave absorption capability analysis. The XRD results show that the addition of Nd3+ doping increases the number of SrNdFeO4 phases. The phase has a tetragonal crystal system that has cell parameters a = b = 3.846 Å, and c = 12.594 Å. The magnetic properties of the material showed that the addition of Nd3+ decreased the saturation and remanence magnetization values, whereas the value of the coercivity field increased. Meanwhile, the best microwave absorption occurs in samples with the addition of Nd3+ as much as 0.3 mol, which results in a reflection loss value of -18.9 dB with a frequency bandwidth of 3.9 GHz.

scholarly journals Struvite Grown in Gel, Its Crystal Structure at 90 K and Thermoanalytical Study

Crystals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 89 ◽  
Author(s):  
Jolanta Prywer ◽  
Lesław Sieroń ◽  
Agnieszka Czylkowska
Keyword(s):  
Thermal Analysis ◽  
Sodium Metasilicate ◽  
X Ray Diffraction ◽  
Gel Growth ◽  
Growth Technique ◽  
Thermoanalytical Study ◽  
X Ray ◽  
Cell Parameters ◽  
Thermal Analysis Techniques ◽  
Derivative Thermogravimetry

In this article, we report the crystallization of struvite in sodium metasilicate gel by single diffusion gel growth technique. The obtained crystals have a very rich morphology displaying 18 faces. In this study, the habit and morphology of the obtained struvite crystals are analyzed. The crystals were examined and identified as pure struvite by single X-ray diffraction (XRD). The orthorhombic polar noncentrosymmetric space group Pmn21 was identified. The structure of the crystal was determined at a temperature of 90 K. Our research indicates a lack of polymorphism, resulting from the temperature lowering to 90 K, which has not been previously reported. The determined unit cell parameters are as follows a = 6.9650(2) Å, b = 6.1165(2) Å, c = 11.2056(3) Å. The structure of struvite is presented here with a residual factor R1 = 1.2% at 0.80 Å resolution. We also present thermoanalytical study of struvite using thermal analysis techniques such as thermogravimetry (TG), derivative thermogravimetry (DTG) and differential thermal analysis (DTA).

scholarly journals Structural and Enhanced Optical Properties of Stabilized γ‒Bi2O3 Nanoparticles: Effect of Oxygen Ion Vacancies

Nanomaterials ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 1023 ◽  
Author(s):  
Ashish Chhaganlal Gandhi ◽  
Chia-Liang Cheng ◽  
Sheng Yun Wu
Keyword(s):  
Room Temperature ◽  
Excess Oxygen ◽  
Ambient Atmosphere ◽  
Photoluminescence Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Band Emission ◽  
Oxygen Ion ◽  
Integrated Intensity ◽  
Effect Of Oxygen

We report the synthesis of room temperature (RT) stabilized γ–Bi2O3 nanoparticles (NPs) at the expense of metallic Bi NPs through annealing in an ambient atmosphere. RT stability of the metastable γ–Bi2O3 NPs is confirmed using synchrotron radiation powder X-ray diffraction and Raman spectroscopy. γ–Bi2O3 NPs exhibited a strong red-band emission peaking at ~701 nm, covering 81% integrated intensity of photoluminescence spectra. Our findings suggest that the RT stabilization and enhanced red-band emission of γ‒Bi2O3 is mediated by excess oxygen ion vacancies generated at the octahedral O(2) sites during the annealing process.

scholarly journals Tamuraite, Ir5Fe10S16, a New Species of Platinum-Group Mineral from the Sisim Placer Zone, Eastern Sayans, Russia

Minerals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 545
Author(s):  
Andrei Y. Barkov ◽  
Nadezhda D. Tolstykh ◽  
Robert F. Martin ◽  
Andrew M. McDonald
Keyword(s):  
National Laboratory ◽  
X Ray Diffraction ◽  
Calculated Density ◽  
Cell Parameters ◽  
Reflected Light ◽  
Platinum Group Minerals ◽  
Platinum Group ◽  
Probable Space ◽  
Layered Complex ◽  
Residual Melt

Tamuraite, ideally Ir5Fe10S16, occurs as discrete phases (≤20 μm) in composite inclusions hosted by grains of osmium (≤0.5 mm across) rich in Ir, in association with other platinum-group minerals in the River Ko deposit of the Sisim Placer Zone, southern Krasnoyarskiy Kray, Russia. In droplet-like inclusions, tamuraite is typically intergrown with Rh-rich pentlandite and Ir-bearing members of the laurite–erlichmanite series (up to ~20 mol.% “IrS2”). Tamuraite is gray to brownish gray in reflected light. It is opaque, with a metallic luster. Its bireflectance is very weak to absent. It is nonpleochroic to slightly pleochroic (grayish to light brown tints). It appears to be very weakly anisotropic. The calculated density is 6.30 g·cm−3. The results of six WDS analyses are Ir 29.30 (27.75–30.68), Rh 9.57 (8.46–10.71), Pt 1.85 (1.43–2.10), Ru 0.05 (0.02–0.07), Os 0.06 (0.03–0.13), Fe 13.09 (12.38–13.74), Ni 12.18 (11.78–13.12), Cu 6.30 (6.06–6.56), Co 0.06 (0.04–0.07), S 27.23 (26.14–27.89), for a total of 99.69 wt %. This composition corresponds to (Ir2.87Rh1.75Pt0.18Ru0.01Os0.01)Σ4.82(Fe4.41Ni3.90Cu1.87Co0.02)Σ10.20S15.98, calculated based on a total of 31 atoms per formula unit. The general formula is (Ir,Rh)5(Fe,Ni,Cu)10S16. Results of synchrotron micro-Laue diffraction studies indicate that tamuraite is trigonal. Its probable space group is R–3m (#166), and the unit-cell parameters are a = 7.073(1) Å, c = 34.277(8) Å, V = 1485(1) Å3, and Z = 3. The c:a ratio is 4.8462. The strongest eight peaks in the X-ray diffraction pattern [d in Å(hkl)(I)] are: 3.0106(26)(100), 1.7699(40)(71), 1.7583(2016)(65), 2.7994(205)(56), 2.9963(1010)(50), 5.7740(10)(45), 3.0534(20)(43) and 2.4948(208)(38). The crystal structure is derivative of pentlandite and related to that of oberthürite and torryweiserite. Tamuraite crystallized from a residual melt enriched in S, Fe, Ni, Cu, and Rh; these elements were incompatible in the Os–Ir alloy that nucleated in lode zones of chromitites in the Lysanskiy layered complex, Eastern Sayans, Russia. The name honors Nobumichi Tamura, senior scientist at the Advanced Light Source of the Lawrence Berkeley National Laboratory, Berkeley, California.

Sign in / Sign up

Export Citation Format

Share Document