Ba1.2-xCsxM1.2-x/2Ti6.8+x/2O16 (M = Ni, Zn) hollandites for the immobilisation of radiocaesium

MRS Advances ◽  
2020 ◽  
Vol 5 (1-2) ◽  
pp. 55-64
Author(s):  
D. J. Bailey ◽  
M. C. Stennett ◽  
N. C. Hyatt
Keyword(s):  
Hot Isostatic Pressing ◽  
High Heat ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Host Matrix ◽  
Radiogenic Heating ◽  
High Level ◽  
Space Separation ◽  
Heat Loads ◽  
Resultant Material

ABSTRACTImproved budgeting of heat loads arising from radiogenic heating in high level wastes (HLW) could allow enhanced usage of geological disposal facility space. Separation of high heat generating nuclides from HLW, such as Cs, would simplify management of heat loads. A potential host matrix for Cs-disposal is hollandite. The incorporation of Cs into the hollandite phase is aided by substitution of cations on the B-site of the structure; these ions may include Ni and Zn. Two series of hollandites, Ni-substituted and Zn-substituted, were synthesised via an alkoxide-nitrate route and consolidated by cold uniaxial pressing and sintering or by hot isostatic pressing. Characterisation of the resultant material by X-ray diffraction and scanning electron microscopy found that hollandite was formed for all levels of substitution. Materials produced via HIP were found to be denser indicating lower Cs loss. HIPed Ni hollandites were found to contain fewer secondary phases and it was concluded that they were the most suitable candidates

Magnetic and dielectric properties of BiFeO3 nanoparticles

2015 ◽  
Vol 7 (2) ◽  
pp. 1393-1403
Author(s):  
Dr R.P VIJAYALAKSHMI ◽  
N. Manjula ◽  
S. Ramu ◽  
Amaranatha Reddy
Keyword(s):  
Diffuse Reflectance Spectrum ◽  
Precipitation Method ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Bifeo3 Nanoparticles ◽  
Transmission Electron ◽  
Multiferroic Bifeo3 ◽  
Pure Phase ◽  
Simple Chemical ◽  
Co Precipitation

Single crystalline nano-sized multiferroic BiFeO3 (BFO) powders were synthesized through simple chemical co-precipitation method using polyethylene glycol (PEG) as capping agent. We obtained pure phase BiFeO3 powder by controlling pHand calcination temperature. From X-ray diffraction studies the nanoparticles were unambiguously identified to have a rhombohedrally distorted perovskite structure belonging to the space group of R3c. No secondary phases were detected. It indicates single phase structure. EDX spectra indicated the appearance of three elements Bi, Fe, O in 1:1:3. From the UV-Vis diffuse reflectance spectrum, the absorption cut-off wavelength of the BFO sample is around 558nm corresponding to the energy band gap of 2.2 eV. The size (60-70 nm) and morphology of the nanoparticles have been analyzed using transmission electron microscopy (TEM).   Linear M−H behaviour and slight hysteresis at lower magnetic field is observed for BiFeO3 nanoparticles from Vibrating sample magnetometer studies. It indicates weak ferromagnetic behaviour at room temperature. From dielectric studies, the conductivity value is calculated from the relation s = L/RbA Sm-1 and it is around 7.2 x 10-9 S/m.

scholarly journals Upscaling of LATP synthesis: Stoichiometric screening of phase purity and microstructure to ionic conductivity maps

Ionics ◽  
2021 ◽  
Vol 27 (5) ◽  
pp. 2017-2025
Author(s):  
Nikolas Schiffmann ◽  
Ethel C. Bucharsky ◽  
Karl G. Schell ◽  
Charlotte A. Fritsch ◽  
Michael Knapp ◽  
...  
Keyword(s):  
Ionic Conductivity ◽  
Sol Gel ◽  
Ion Conductivity ◽  
Process Window ◽  
Lithium Aluminum ◽  
Potential Candidate ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Battery Cell ◽  
Li Ion

AbstractLithium aluminum titanium phosphate (LATP) is known to have a high Li-ion conductivity and is therefore a potential candidate as a solid electrolyte. Via sol-gel route, it is already possible to prepare the material at laboratory scale in high purity and with a maximum Li-ion conductivity in the order of 1·10−3 s/cm at room temperature. However, for potential use in a commercial, battery-cell upscaling of the synthesis is required. As a first step towards this goal, we investigated whether the sol-gel route is tolerant against possible deviations in the concentration of the precursors. In order to establish a possible process window for sintering, the temperature interval from 800 °C to 1100 °C and holding times of 10 to 480 min were evaluated. The resulting phase compositions and crystal structures were examined by X-ray diffraction. Impedance spectroscopy was performed to determine the electrical properties. The microstructure of sintered pellets was analyzed by scanning electron microscopy and correlated to both density and ionic conductivity. It is shown that the initial concentration of the precursors strongly influences the formation of secondary phases like AlPO4 and LiTiOPO4, which in turn have an influence on ionic conductivity, densification behavior, and microstructure evolution.

TEM and X-Ray Examinations of Intermetallic Phases and Carbides Precipitation in an Fe-Ni Superalloy during Prolonged Ageing

2013 ◽  
Vol 212 ◽  
pp. 15-20
Author(s):  
Kazimierz J. Ducki ◽  
Jacek Mendala ◽  
Lilianna Wojtynek
Keyword(s):  
Heat Treatment ◽  
Solution Heat Treatment ◽  
Intermetallic Phase ◽  
Intermetallic Phases ◽  
Precipitation Process ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Solid Samples ◽  
Structural Investigations ◽  
X Ray

The influence of prolonged ageing on the precipitation process of the secondary phases in an Fe-Ni superalloy of A-286 type has been studied. The samples were subjected to a solution heat treatment at 980°C for 2 h and water quenched, and then aged at temperatures of 715, 750 and 780°C at holding times from 0.5 to 500 h. Structural investigations were conducted using TEM and X-ray diffraction methods. The X-ray phase analyses performed on the isolates were obtained by anodic dissolution of the solid samples. After solution heat treatment the alloy has the structure of twinned austenite with a small amount of undissolved precipitates, such as carbide TiC, carbonitride TiC0.3N0.7, nitride TiN0.3, carbosulfide Ti4C2S2, Laves phase Ni2Si, and boride MoB. The application of ageing causes precipitation processes of γ-Ni3(Al,Ti), G (Ni16Ti6Si7), η (Ni3Ti), β (NiTi) and σ (Cr0.46Mo0.40Si0.14) intermetallic phases, as well as the carbide M23C6. It was found that the main phase precipitating during alloy ageing was the γ intermetallic phase.

Ba-, Si- and vacancy-rich phlogopites from the talc-bearing sulfide ore deposit of La Creuse, Beaujolais, France

2018 ◽  
Vol 82 (5) ◽  
pp. 1187-1210
Author(s):  
Marie-Lola Pascal ◽  
Michel Fonteilles ◽  
Véronique Tournis ◽  
Benoît Baptiste ◽  
Jean-Louis Robert ◽  
...  
Keyword(s):  
Goodness Of Fit ◽  
Monoclinic Space Group ◽  
Excess Charge ◽  
Formula Unit ◽  
X Ray Diffraction ◽  
Ore Deposit ◽  
Sulfide Ore ◽  
The Common ◽  
The Stability ◽  
High Level

ABSTRACTBa-rich and Si-rich phlogopites occur in the talc-bearing rocks of the La Creuse sulfide ore deposit in Beaujolais, France. They form a group of compositions completely separated from the common Al-rich phlogopites that occur in the surrounding talc-free metasiltites and metarhyolites, with higher Ba and Mg and lower Al contents. The Ba-rich phlogopites have a relatively narrow compositional range (0.24 to 0.80 Ba per formula unit, for 44 valencies) with high and constant Si (5.8 atoms per formula unit, apfu) and Mg + Fe (5.6 apfu), probably buffered by the presence of talc. Compared to low-Al phlogopites from talc-free rocks, the excess charge introduced by the BaK–1 substitution is compensated by interlayer vacancies. Such a high level of interlayer vacancy (0.56 pfu), related to the talc-producing metasomatic conditions, is essential for the stability of this special group of Ba-rich and Si-rich phlogopites.Single crystal X-ray diffraction analyses were performed. Ba-rich and Si-rich phlogopite is monoclinic, space group C2/m, (R = 5.31%) with a = 5.3185(5), b = 9.2136(9), c = 10.1349(11) Å and β = 100.131(11)°. The occupancies of Mg/Fe and K/Ba were refined exploring different vacancies. The solutions giving the best R factor (4.77%) and goodness-of-fit (1.06) are obtained with 15% < vacancy < 40% at the interlayer site.

Electrolytic phase extraction: a useful technique to evaluate precipitates in nitinol

2012 ◽  
Vol 27 (2) ◽  
pp. 136-139 ◽  
Author(s):  
Roy G. Baggerly
Keyword(s):  
Shape Memory ◽  
Matrix Composition ◽  
Precipitation Reaction ◽  
Phase Extraction ◽  
Secondary Phases ◽  
X Ray Diffraction ◽  
Solubility Range ◽  
Two Samples ◽  
Rich Alloy ◽  
Rich Side

Nitinol is a shape memory alloy based on the inter-atomic compound having a composition of 50  at% each of Ni and Ti, NiTi. The shape memory effect results from a reversible martensitic phase transformation. An increasing solubility range with temperature on the Ni-rich side can produce a precipitation reaction resulting in a slight matrix composition adjustment with appropriate heat treatment. Electrolytic phase extraction (Andrews and Hughes, 1957) is used to evaluate the secondary phases in the alloy and Ti2Ni and TiC are positively identified using powder wide-angle X-ray diffraction procedures. Two samples of an Ni-rich alloy at 57 and 60 at% are also analyzed. These Ni-rich samples show Ti2Ni and an additional phase, Ni3Ti.

Synthesis and Characterization of Brannerite Compositions for MOX Residue Disposal

MRS Advances ◽  
2016 ◽  
Vol 2 (10) ◽  
pp. 557-562 ◽  
Author(s):  
D.J. Bailey ◽  
M.C. Stennett ◽  
N.C. Hyatt
Keyword(s):  
Powder Diffraction ◽  
Microstructural Analysis ◽  
Charge Compensation ◽  
Phase Assemblage ◽  
Secondary Phases ◽  
Host Matrix ◽  
Neutron Absorber ◽  
X Ray ◽  
Valence States ◽  
Trivalent Cations

ABSTRACTDue to their high actinide content MOX residues require immobilization within a robust host matrix. Although it is possible to immobilize actinides in vitreous wasteforms; ceramic phases, such as brannerite (UTi2O6), are attractive due to their high waste loading capacity and relative insolubility. Brannerites Gd0.1U0.9Ti2O6, Ce0.1U0.9Ti2O6and Gd0.1U0.81Ce0.09Ti2O6were prepared using an oxide route. Charge compensation of trivalent cations was expected to occur via the oxidation of U (IV) to higher valence states (U (V) or U (VI)). Gd was added to act as a neutron absorber in the final Pu bearing wasteform and Ce was used as a structural surrogate for Pu. X-ray absorption spectroscopy showed that Ce (IV) was reduced to Ce (III) in all cases. X-ray powder diffraction of synthesized specimens found that the final phase assemblage was strongly affected by processing atmosphere (air or argon). Prototypical brannerite was formed in all compositions, secondary phases observed were found to vary according to processing atmosphere and stoichiometry. Microstructural analysis (SEM) of the sintered samples confirmed the results of the X-ray powder diffraction.

scholarly journals Znx-1CuxMn2O4 Spinels; Synthesis, Structural Characterization and Electrical Evaluation

2019 ◽  
Vol 54 (1) ◽  
Author(s):  
Francisco Méndez-Martínez ◽  
Federico González ◽  
Enrique Lima ◽  
Pedro Bosch ◽  
Heriberto Pfeiffer
Keyword(s):  
Impedance Spectroscopy ◽  
Structural Characterization ◽  
Morphological Changes ◽  
Secondary Phases ◽  
Varistor Ceramic ◽  
X Ray Diffraction ◽  
X Ray ◽  
Copper Addition ◽  
Partial Inverse ◽  
Scanning Electron

This work presents the structural characterization and electrical evaluation of Znx-1CuxMn2O4 spinels, which are materials presented as secondary phases into the varistor ceramic systems. Samples were analyzed by X-ray diffraction, solid-state nuclear magnetic resonance, infrared spectroscopy, scanning electron microscopy and impedance spectroscopy. Although, the addition of copper to the ZnMn2O4 spinel did not produce morphological changes, the structure and electrical behaviors changed considerably. Structurally, copper addition induced the formation of partial inverse spinels, and its addition increases significantly the electrical conductivity. Therefore, the formation of Znx-1CuxMn2O4 spinels, as secondary phases into the varistor materials, may compromise significantly the varistor efficiency.   Ceramic, Impedance Spectroscopy, spinel, Varistor, XRD.

Investigation of Loop Heat Pipe Startup Using Liquid Core Visualization

2008 ◽  
Author(s):  
B. P. d’Entremont ◽  
J. M. Ochterbeck
Keyword(s):  
Heat Pipe ◽  
Liquid Core ◽  
High Heat ◽  
Working Fluid ◽  
Loop Heat Pipe ◽  
Two Phase ◽  
Buoyancy Driven Flows ◽  
Compensation Chamber ◽  
Fill Level ◽  
Heat Loads

In this investigation, a Loop Heat Pipe (LHP) evaporator has been studied using a borescope inserted through the compensation chamber into the liquid core. This minimally intrusive technique allows liquid/vapor interactions to be observed throughout the liquid core and compensation chamber. A low conductivity ceramic was used for the wick and ammonia as the working fluid. Results indicate that buoyancy driven flows, both two-phase and single-phase, play essential roles in evacuating excess heat from the core, which explains the several differences in performance between horizontal and vertical orientations of the evaporator. This study also found no discernable effect of the pre-start fill level of the compensation chamber on thermal performance during startup at moderate and high heat loads.

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