A structural study of the (Na1−xKx)0.5Bi0.5TiO3 perovskite series as a function of substitution (x) and temperature

2002 ◽  
Vol 17 (4) ◽  
pp. 301-319 ◽  
Author(s):  
G. O. Jones ◽  
J. Kreisel ◽  
P. A. Thomas
Keyword(s):  
Phase Transitions ◽  
Phase Space ◽  
Room Temperature ◽  
Profile Analysis ◽  
Rhombohedral Phase ◽  
Polar Axis ◽  
Detailed Characterization ◽  
Space Group ◽  
Structural Modifications

Rietveld neutron powder profile analysis of the (Na1−xKx)0.5Bi0.5TiO3 (NKBT) series (x=0, 0.2, 0.4, 0.5, 0.6, 0.8, 1.0) is reported over the temperature range 293–993 K. A detailed characterization of the structures and phase transitions occurring across this series as a function of temperature has been made. Room-temperature refinements have revealed a rhombohedral phase, space group R3c for x=0, 0.2, and 0.4, which exhibits an antiphase, a−a−a− oxygen tilt system with parallel cation displacements along [111]p. An intermediate zero-tilt rhombohedral phase, space group R3m possessing cation displacements along [111]p, has been established for x=0.5 and 0.6. At the potassium-rich end of the series at x=0.8 and 1.0, a tetragonal phase, space group P4mm is observed possessing cation displacements along [001]. At the sodium-rich end of the series for x=0.2, the unusual tetragonal structure with space group P4bm is seen for Na0.5Bi0.5TiO3 which possesses a combination of in-phase a0a0c+ tilts and antiparallel cation displacements along the polar axis. Temperature-induced phase transitions are reported and structural modifications are discussed.

Investigation of the structure and phase transitions in the novel A-site substituted distorted perovskite compound Na0.5Bi0.5TiO3

2002 ◽  
Vol 58 (2) ◽  
pp. 168-178 ◽  
Author(s):  
G. O. Jones ◽  
P. A. Thomas
Keyword(s):  
Phase Transitions ◽  
Phase Space ◽  
Profile Analysis ◽  
Second Harmonic ◽  
Rhombohedral Phase ◽  
Polar Axis ◽  
Temperature Limit ◽  
Space Group ◽  
Systematic Behaviour ◽  
A Site

Rietveld neutron powder profile analysis of the compound Na0.5Bi0.5TiO3 (NBT) is reported over the temperature range 5–873 K. The sequence of phase transitions from the high-temperature prototypic cubic structure (above 813 K), to one of tetragonal (673–773 K) and then rhombohedral structures (5–528 K) has been established. Coexisting tetragonal/cubic (773–813 K) and rhombohedral/tetragonal (with an upper temperature limit of 145 K between 528 and 673 K) phases have also been observed. Refinements have revealed that the rhombohedral phase, space group R3c, with a H = 5.4887 (2), c H = 13.5048 (8) Å, V = 352.33 (3) Å3, Z = 6 and D x = 5.99 Mg m−3, exhibits an antiphase, a − a − a − oxygen tilt system, ω = 8.24 (4)°, with parallel cation displacements at room temperature. The tetragonal phase, space group P4bm, with a T = 5.5179 (2), c T = 3.9073 (2) Å, V = 118.96 (1) Å3, Z = 2 and D x = 5.91 Mg m−3, possesses an unusual combination of in-phase, a 0 a 0 c + oxygen octahedra tilts, ω = 3.06 (2)°, and antiparallel cation displacements along the polar axis. General trends of cation displacements and the various deviations of the octahedral network from the prototypic cubic perovskite structure have been established and their systematic behaviour with temperature is reported. An investigation of phase transition behaviour using second harmonic generation (SHG) to establish the centrosymmetric or non-centrosymmetric nature of the various phases is also reported.

Phase transitions and twinned low-temperature structures of tetraethylammonium tetrachloridoferrate(III)

2014 ◽  
Vol 70 (5) ◽  
pp. 470-476 ◽  
Author(s):  
Martin Lutz ◽  
Yuxing Huang ◽  
Marc-Etienne Moret ◽  
Robertus J. M. Klein Gebbink
Keyword(s):  
Phase Transitions ◽  
Room Temperature ◽  
Polar Axis ◽  
Temperature Structure ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Space Groups ◽  
Disordered Structure ◽  
Compound C ◽  
Three Space

The title compound, [(C2H5)4N][FeCl4], has at room temperature a disordered structure in the high-hexagonal space group P63 mc. At 230 K, the structure is merohedrally twinned in the low-hexagonal space group P63. The volume has increased by a factor of 9 with respect to the room-temperature structure. At 170 and 110 K, the structure is identical in the orthorhombic space group Pca21 and twinned by reticular pseudomerohedry. The volume has doubled with respect to the room-temperature structure. All three space groups, viz. P63 mc, P63 and Pca21, are polar and the direction of the polar axis is not affected by the twinning. In the P63 and Pca21 structures, all cations and anions are well ordered.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

Structures and phase transitions in barium sodium niobate tungsten bronze (BNN)

2021 ◽  
Vol 77 (6) ◽  
Author(s):  
Thomas A. Whittle ◽  
Christopher J. Howard ◽  
Siegbert Schmid
Keyword(s):  
Phase Transitions ◽  
Room Temperature ◽  
Tungsten Bronze ◽  
Standard Setting ◽  
Experimental Results ◽  
Temperature Structure ◽  
Sodium Niobate ◽  
Tetragonal Tungsten Bronze ◽  
Space Group ◽  
The Subject

The room-temperature structure of the filled tetragonal tungsten bronze, Ba2NaNb5O15 (BNN), has been the subject of a number of studies, and these studies have given an almost corresponding number of different results. From a group theoretical examination of the different possibilities and a review of the published experimental results we conclude that the room-temperature structure is that proposed by Labbé et al. [J. Phys. Condens. Matter (1989), 2, 25–43] in the space group Bbm2 (Ama2 in standard setting) on a 2\sqrt{2}a × \sqrt{2}a × 2c cell. Upon heating, the structure remains ferroelectric but becomes tetragonal (space group P4bm) at 550 K, then paraelectric (space group P4/mbm) at and above 860 K.

The structures and phase transitions in 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2]

2019 ◽  
Vol 75 (6) ◽  
pp. 1144-1151
Author(s):  
Tamara J. Bednarchuk ◽  
Wolfgang Hornfeck ◽  
Vasyl Kinzhybalo ◽  
Zhengyang Zhou ◽  
Michal Dušek ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Single Crystal ◽  
Room Temperature ◽  
Variable Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Hybrid Compound ◽  
Space Group ◽  
X Ray

The organic–inorganic hybrid compound 4-aminopyridinium tetraaquabis(sulfato)iron(III), (C5H7N2)[FeIII(H2O)4(SO4)2] (4apFeS), was obtained by slow evaporation of the solvent at room temperature and characterized by single-crystal X-ray diffraction in the temperature range from 290 to 80 K. Differential scanning calorimetry revealed that the title compound undergoes a sequence of three reversible phase transitions, which has been verified by variable-temperature X-ray diffraction analysis during cooling–heating cycles over the temperature ranges 290–100–290 K. In the room-temperature phase (I), space group C2/c, oxygen atoms from the closest Fe-atom environment (octahedral) were disordered over two equivalent positions around a twofold axis. Two intermediate phases (II), (III) were solved and refined as incommensurately modulated structures, employing the superspace formalism applied to single-crystal X-ray diffraction data. Both structures can be described in the (3+1)-dimensional monoclinic X2/c(α,0,γ)0s superspace group (where X is ½, ½, 0, ½) with modulation wavevectors q = (0.2943, 0, 0.5640) and q = (0.3366, 0, 0.5544) for phases (II) and (III), respectively. The completely ordered low-temperature phase (IV) was refined with the twinning model in the triclinic P{\overline 1} space group, revealing the existence of two domains. The dynamics of the disordered anionic substructure in the 4apFeS crystal seems to play an essential role in the phase transition mechanisms. The discrete organic moieties were found to be fully ordered even at room temperature.

Phase Stability and Sintering Behavior of 10mol%Sc2O3–1mol%CeO2–ZrO2 Ceramics

2009 ◽  
Vol 6 (2) ◽  
Author(s):  
Sergey Yarmolenko ◽  
Jag Sankar ◽  
Nicholas Bernier ◽  
Michael Klimov ◽  
Jay Kapat ◽  
...  
Keyword(s):  
Phase Transitions ◽  
Room Temperature ◽  
Rhombohedral Phase ◽  
Impurity Level ◽  
Cubic Phase ◽  
Sintering Behavior ◽  
X Ray Diffraction ◽  
Chemical Route ◽  
Heating And Cooling ◽  
Secondary Ion

The phase composition and sintering behavior of two commercially available 10mol%Sc2O3–1mol%CeO2–ZrO2 ceramics produced by Daiichi Kigenso Kagaku Kogyo (DKKK) and Praxair have been studied. DKKK powders have been manufactured using a wet coprecipitation chemical route, and Praxair powders have been produced by spray pyrolysis. The morphology of the powders, as studied by scanning electron microscopy, has been very different. DKKK powders were presented as soft (∼100μm) spherical agglomerates containing 60–100nm crystalline particles, whereas the Praxair powders were presented as sintered platelet agglomerates, up to 30μm long and 3–4μm thick, which consisted of smaller 100–200nm crystalline particles. X-ray diffraction analysis has shown that both DKKK and Praxair powders contained a mixture of cubic (c) and rhombohedral (r) phases: 79% cubic +21% rhombohedral for DKKK powders and 88% cubic +12% rhombohedral for Praxair powders. Higher quantities of the Si impurity level have been detected in Praxair powder as compared to DKKK powder by secondary ion mass spectroscopy. The morphological features, along with differences in composition and the impurity level of both powders, resulted in significantly different sintering behaviors. The DKKK powders showed a more active sintering behavior than of Praxair powders, reaching 93–95% of theoretical density when sintered at 1300°C for 2h. Comparatively, the Praxair powders required high sintering temperatures at 1500–1600°C. However, even at such high sintering temperatures, a significant amount of porosity was observed. Both DKKK and Praxair ceramics sintered at 1300°C or above exist in a cubic phase at room temperature. However, if sintered at 1100°C and 1200°C, the DKKK ceramics exist in a rhombohedral phase at room temperature. The DKKK ceramics sintered at 1300°C or above exhibit cubic to rhombohedral and back to cubic phase transitions upon heating at a 300–500°C temperature range, while Praxair ceramics exist in a pure cubic phase upon heating from room temperature to 900°C. However, if heated rather fast, the cubic to rhombohedral phase transformation could be avoided. Thus it is not expected that the observed phase transitions play a significant role in developing transformation stresses in ScCeZrO2 electrolyte upon heating and cooling down from the operation temperatures.

TEM characterization of the α' and β phases in polycrystalline distrontium silicate (Sr2SiO4)

1992 ◽  
Vol 50 (1) ◽  
pp. 354-355
Author(s):  
Y. J. Kim ◽  
J. L. Shull ◽  
W. M. Kriven
Keyword(s):  
Electron Beam ◽  
Phase Space ◽  
Atmospheric Pressure ◽  
Sintering Temperature ◽  
Major Phase ◽  
Space Group ◽  
Temperature Range ◽  
Β Phase ◽  
Tem Characterization

Two polymorphs, α' and β, are known to be major phases in pure distrontium silicate (Sr2SiO4) at atmospheric pressure. Fully dense pellets were fabricated by sintering chemically prepared powders in the temperature range of 900° to 1400°C for 1 to 5 hours. Their phases and microstructures were studied by TEM. At lower sintering temperatures such as 900°C, the major phase was orthorhombic α' (space group, Pmnb). The euhedral α' grains had a size of about 1 μm diameter (Fig. la). As the sintering temperature increased, the amount of monoclinic β phase (space group, P21/n) tended to increase. These β grains were usually irregular and twinned on {100}β or {001}β planes. Concentration of the electron beam on the grains gave rise to a disappearance of twins (Fig. lb).

Characterization and dielectric properties of sodium fluoride doped talc

Clay Minerals ◽  
2014 ◽  
Vol 49 (4) ◽  
pp. 551-558
Author(s):  
S. Gümüştas ◽  
K. Köseoğlu ◽  
E. E. Yalçinkaya ◽  
M. Balcan
Keyword(s):  
Dielectric Constant ◽  
Dielectric Properties ◽  
Dielectric Loss ◽  
Firing Temperature ◽  
Room Temperature ◽  
Dielectric Measurements ◽  
Frequency Range ◽  
Detailed Characterization ◽  
Circuit Element

AbstractThe purpose of this paper is to determine the effect of NaF and firing temperature on the dielectric properties (dielectric constant and dielectric loss) of talc, which is used in the electrical and electronic industries as a circuit element. A detailed characterization of the samples was made by XRD, FTIR, SEM and TG-DTG methods. Dielectric measurements were performed in the frequency range from 1 MHz to 80 MHz at room temperature. The dielectric constant value increased with an increase in firing temperature due to the removal of polarizable compounds from the talc structure. The higher dielectric constant values were obtained by addition of NaF. The dielectric loss of NaF doped talc decreased with the increase of firing temperature and increased with the increase of the amount of NaF.

Untersuchungen zur Polymorphie der Cäsium-Dodekahalogeno-closo-Dodekaborate Cs2[B12X12] (X = Cl–I)

2020 ◽  
Vol 75 (8) ◽  
pp. 777-790
Author(s):  
Ioannis Tiritiris ◽  
Kevin U. Bareiß ◽  
Thomas Schleid
Keyword(s):  
Phase Transitions ◽  
Defect Structure ◽  
Room Temperature ◽  
Solid Phase ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
Space Group ◽  
X Ray ◽  
Cubic System ◽  
Cesium Salts

AbstractThermoanalytic DSC and temperature-dependent X-ray diffraction investigations on the cesium dodecahalogeno-closo-dodecaborates Cs2[B12X12] (X = Cl–I) have revealed solid-solid phase transitions from their trigonal room-temperature α-forms (e.g. α-Cs2[B12Cl12]: a = 959.67(3) pm, c = 4564.2(2) pm, Z = 6, space group R$\overline{3}$) into cubic high-temperature modifications. The isotypic title compounds crystallize in the space group Pm$\overline{3}$n (e.g. β-Cs2[B12Cl12]: a = 1051.98(6) pm, Z = 2) with a W3O-type defect structure. The statistic occupation of six possible positions with only four Cs+ cations results in a cation-deficient A2B arrangement for Cs2[B12X12]. Upon cooling the β-phase, a third polymorph was observed, which also crystallizes in the cubic system, but now in the space group Ia$\overline{3}$d (e.g. γ-Cs2[B12Cl12]: a = 2102.2(3) pm, Z = 16), and has to be regarded as a phase with only a partially disordered cation substructure. In this crystal structure the [B12X12]2− anions exhibit a NaTl-type arrangement, in which the Cs+ cations occupy suitable interstices. The phase transitions of the differently halogenated cesium salts follow no specific trend as the transition from the trigonal α- to the cubic β-form occurs at 178 °C for the chlorinated, at 270 °C for the iodinated and at 325 °C for the brominated examples. On further heating however, β-Cs2[B12I12] starts to decompose at 945 °C first, followed by β-Cs2[B12Br12] and β-Cs2[B12Cl12] at 959 °C and 983 °C, respectively.

Temperature dependence of spontaneous strain in ferroelastic thallous nitrate

1989 ◽  
Vol 22 (2) ◽  
pp. 105-109 ◽  
Author(s):  
M. S. Somayazulu ◽  
V. K. Wadhawan
Keyword(s):  
Phase Transitions ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rhombohedral Phase ◽  
Lattice Parameter ◽  
Large Magnitude ◽  
Spontaneous Strain ◽  
X Ray ◽  
Strain Components ◽  
Temperature Lattice

TlNO3 is a ferroelastic crystal belonging to the orthorhombic Aizu species m3mFmmm(ss) at room temperature. Lattice-parameter measurements by X-ray powder diffraction at various temperatures are reported for this crystal. Spontaneous-strain components are calculated from the lattice parameters. The spontaneous strain has a large magnitude of 7.80 x 10−2 at room temperature. Its two components are found to be rather insensitive to change of temperature. This may be due in part to the improper nature of this ferroelastic. Anomalies indicating either new isomorphous phase transitions or crossover behaviour are observed at 309, 329 and 399 K. Between 352 and 416 K the crystal belongs to the rhombohedral Aizu species m3mF3. The critical exponent of the spontaneous strain for the rhombohedral phase is found to change from 0.72 (3) to 0.60 (5) at 399 K.

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