scholarly journals In-situ high-temperature diffraction studies of ion-exchanged umbite

2014 ◽  
Vol 70 (a1) ◽  
pp. C70-C70
Author(s):  
Stephen Grieve ◽  
Hayley Green ◽  
Reece Hall ◽  
Jennifer Readman

Microporous materials such as zirconium silicates have the potential to be of importance in the nuclear industry for the selective uptake of cationic radionuclides and environmental pollutants. The structural behaviour of these materials at elevated temperatures is of interest for two reasons, the first is the densification of the exchanged materials prior to long term storage and the second is the formation of new porous phases which may have increased ion exchanged affinity for certain cations. The work presented here focuses on the umbite system. Umbite is a naturally occurring microporous zirconium titanium silicate found in northern Russia and synthetic analogues, K2ZrSi3O9·H2O, can be prepared using hydrothermal methods. It has an orthorhombic cell with a = 10.2977(2)Å, b = 13.3207(3)Å and c = 7.1956(1)Å. The ion-exchange of umbite with cations such as rubidium, caesium and strontium and the structures of the resulting exchanged materials have been studied. Exchanges with certain cations were found to cause a change in crystal system to a monoclinic cell. Recently Rocha and co-workers found that synthetic umbite will undergo a topotactic transformation when heated 9100C to form a new microporous zirconium silicate (AV-15) with the formula K2ZrSi3O9·2H2O, but to date no in-situ work has been carried out on this phase transition. In this work the high temperature structural behaviour of five umbite samples with different exchanged cations (K+, Na+, Mg2+Ca2+and Cu2+) was studied up to a temperature of 10000C. All samples behaved very differently, indicating that the nature and location of the charge balancing cation plays an important part in determining which high temperature phases are formed. Certain general trends were observed, with group 1 cations the samples remain crystalline to high temperatures. With group 2 cations dense phases are formed at high temperatures and with transition metal cations there is a loss of crystallinity at low temperature.

2000 ◽  
Vol 64 (2) ◽  
pp. 255-266 ◽  
Author(s):  
J. J. Reece ◽  
S. A. T. Redfern ◽  
M. D. Welch ◽  
C. M. B. Henderson

AbstractThe crystal structure of a manganoan cummingtonite, composition [M4](Na0.13Ca0.41Mg0.46Mn1.00) [M1,2,3](Mg4.87Mn0.13)(Si8O22)(OH)2, (Z = 2), a = 9.5539(2) Å, b = 18.0293(3) Å, c = 5.2999(1) Å, β = 102.614(2)° from Talcville, New York, has been refined at high temperature using in situ neutron powder diffraction. The P21/m to C2/m phase transition, observed as spontaneous strains +ε1 = −ε2, occurs at ˜107°C. Long-range disordering between Mg2+ and Mn2+ on the M(4) and M(2) sites occurs above 550°C. Mn2+ occupies the M(4) and M(2) sites preferring M(4) with a site-preference energy of 24.6±1.5 kJ mol−1. Disordering induces an increase in XMnM2 and decrease in XMnM4 at elevated temperatures. Upon cooling, the ordered states of cation occupancy are ‘frozen in’ and strains in lattice parameters are maintained, suggesting that re-equilibration during cooling has not taken place.


2019 ◽  
Vol 187 (1) ◽  
pp. 17-20
Author(s):  
Andrew Villanueva ◽  
Braden Goddard

Abstract While it is known that temperatures above 100°C have an effect on the reported dose of a TLD, it is less widely known what the susceptibility is to temperatures below 100°C, temperatures humans could reasonably expect to be exposed to. With the expanding nuclear industry in climates with more extreme temperatures, (e.g. United Arab Emirates and Saudi Arabia) the effect on a TLD if left on a dashboard of a car need to be evaluated. This research experimentally determined the extent of this thermal susceptibility by testing a range of high temperatures, 40°C – 90°C. The experimental results found that there is a statistically significant reduction in TLD-100H (natLiF:Mg,Cu,P) light output for TLDs there were exposed to temperatures as low as 40°C for 8 hour durations and 50°C for 2 hour durations. There is statistical difference in TLD-100H light output for elevated temperature durations of 8 hours compared to 24 hours.


2020 ◽  
Vol 8 (22) ◽  
pp. 11346-11353
Author(s):  
José A. Márquez ◽  
Jon-Paul Sun ◽  
Helena Stange ◽  
Hasan Ali ◽  
Leo Choubrac ◽  
...  

The decomposition mechanism of Cu2BaSnS4 is studied by in situ diffraction and fluorescence analysis revealing “Sn loss” and Cu2Ba3Sn2S8 at high temperatures.


2019 ◽  
Vol 57 (6) ◽  
pp. 843-851
Author(s):  
Alan J. Anderson ◽  
Robert A. Mayanovic ◽  
Thomas Lee

Abstract The local structure of Ta(V) in high-temperature fluoride- and chloride-bearing acidic solutions was investigated using in situ X-ray absorption spectroscopy (XAS). All XAS spectra were collected from two solutions, designated A and B, at beamline ID-20-C at the Advanced Photon Source, Argonne National Laboratory. Spectra were collected from solution A at 350 and 400 °C and from solution B at 25, 360, and 400 °C after the solutions were sealed in a hydrothermal diamond anvil cell. Solution A was prepared by dissolving Ta2O5 powder in 5% HF solution; solution B consisted of TaCl5 dissolved in 2% HF. The dominant tantalum species in solution A at elevated temperatures was TaF83–. In contrast, TaCl6–, which was the dominant complex in solution B at room temperature, disappeared as hydroxide complexes with an average ligand number between 5 and 7 became the dominant species at 350 and 400 °C. The XAS results confirm the previously recognized effect of fluoride activity on Ta speciation in hydrothermal fluids and suggest that both fluoride and hydroxide complexes play an important role in the transport of Ta in acidic fluoride-bearing solutions involved in the formation of mineralized mica-rich replacement units in granitic pegmatites.


2003 ◽  
Vol 69 (8) ◽  
pp. 4575-4582 ◽  
Author(s):  
Hassan Brim ◽  
Amudhan Venkateswaran ◽  
Heather M. Kostandarithes ◽  
James K. Fredrickson ◽  
Michael J. Daly

ABSTRACT Deinococcus geothermalis is an extremely radiation-resistant thermophilic bacterium closely related to the mesophile Deinococcus radiodurans, which is being engineered for in situ bioremediation of radioactive wastes. We report that D. geothermalis is transformable with plasmids designed for D. radiodurans and have generated a Hg(II)-resistant D. geothermalis strain capable of reducing Hg(II) at elevated temperatures and in the presence of 50 Gy/h. Additionally, D. geothermalis is capable of reducing Fe(III)-nitrilotriacetic acid, U(VI), and Cr(VI). These characteristics support the prospective development of this thermophilic radiophile for bioremediation of radioactive mixed waste environments with temperatures as high as 55°C.


2002 ◽  
Vol 8 (1) ◽  
pp. 16-20 ◽  
Author(s):  
S. Arai ◽  
K. Suzuki ◽  
H. Saka

Behavior of fine crystalline particles of W5Si3 on a β-Si3N4 substrate at high temperatures was observed by an in situ heating experiment in a transmission electron microscope. Some of the fine particles of W5Si3 moved in a to-and-fro manner.


2018 ◽  
Vol 9 (3) ◽  
pp. 203-221 ◽  
Author(s):  
Muhammad Masood Rafi ◽  
Abdul Basit Dahar ◽  
Tariq Aziz

Purpose The purpose of this paper is to present the results of experimental testing of steel rebars at elevated temperatures. Three types of bars available in the local market in Pakistan were used. These data are not available in Pakistan. Design/methodology/approach Three types of bars were used, which included cold-twisted ribbed (CTR), hot-rolled deformed (HRD) and thermo-mechanically treated (TMT) bars. The diameter of the bar of each type was 16 mm. The bars were heated in an electrical furnace at temperatures which were varied from 100°C to 900°C in increment of 100°C. Bars of each type were also tested at ambient temperature as control specimens. The change of strength, strain and modulus of elasticity of the bars at high temperatures were determined. Findings The mechanical properties of the bars were nearly unaffected by the temperatures up to 200°C. CTR bars did not show yield plateau and strain hardening both at ambient and high temperatures. The high temperature yield strength and elastic modulus for all the three types of bars were similar at all temperatures. The yield plateau of both the HRD and TMT bars disappeared at temperatures greater than 300°C. The ultimate strength at high temperature of the HRD and TMT bars was also similar. The behaviours of the HRD and TMT bars changed to brittle beyond 400°C as compared to their behaviours at ambient temperature. The CTR bars exhibited ductile characteristics at failure at all the exposure temperatures relative to their behaviour at ambient temperature. Research limitations/implications The parameters of the paper included the rebar type and heating temperature and the effects of temperature on strength and stiffness properties of the steel bars. Practical implications Building fire incidents have increased in Pakistan. As reinforced concrete (RC) buildings exist in the country in significant numbers, the data related to elevated temperature properties of steel is required. These data are not available in Pakistan presently. The presented paper aims at providing this information for the design engineers to enable them to assess and increase fire resistance of RC structural members. Originality/value The presented paper is unique in its nature in that there is no published contribution to date, to the best of authors’ knowledge, which has been carried out to assess the temperature-dependent mechanical properties of steel reinforcing bars available in Pakistan.


2016 ◽  
Vol 49 (4) ◽  
pp. 1253-1265 ◽  
Author(s):  
Ralph Gilles ◽  
Debashis Mukherji ◽  
Lukas Karge ◽  
Pavel Strunz ◽  
Premysl Beran ◽  
...  

Co–Re alloys are being developed for ultra-high-temperature applications to supplement Ni-based superalloys in future gas turbines. The main goal of the alloy development is to increase the maximum service temperature of the alloy beyond 1473 K,i.e.at least 100 K more than the present single-crystal Ni-based superalloy turbine blades. Co–Re alloys are strengthened by carbide phases, particularly the monocarbide of Ta. The binary TaC phase is stable at very high temperatures, much greater than the melting temperature of superalloys and Co–Re alloys. However, its stability within the Co–Re–Cr system has never been studied systematically. In this study an alloy with the composition Co–17Re–23Cr–1.2Ta–2.6C was investigated using complementary methods of small-angle neutron scattering (SANS), scanning electron microscopy, X-ray diffraction and neutron diffraction. Samples heat treated externally and samples heatedin situduring diffraction experiments exhibited stable TaC precipitates at temperatures up to 1573 K. The size and volume fraction of fine TaC precipitates (up to 100 nm) were characterized at high temperatures within situSANS measurements. Moreover, SANS was used to monitor precipitate formation during cooling from high temperatures. When the alloy is heated the matrix undergoes an allotropic phase transformation from the ∊ phase (hexagonal close-packed) to the γ phase (face-centred cubic), and the influence on the strengthening TaC precipitates was also studied within situSANS. The results show that the TaC phase is stable and at these high temperatures the precipitates coarsen but still remain. This makes the TaC precipitates attractive and the Co–Re alloys a promising candidate for high-temperature application.


1998 ◽  
Vol 4 (3) ◽  
pp. 226-234 ◽  
Author(s):  
Ulrich Messerschmidt ◽  
Dietmar Baither ◽  
Martin Bartsch ◽  
Bernd Baufeld ◽  
Bert Geyer ◽  
...  

Design rules are described here for high-temperature straining stages for transmission electron microscopy. Temperatures above 1000°C can be attained by electron bombardment of the specimen grips. Thermal equilibrium can be reached in a short time by carrying off the heat by water cooling. Some applications of this stage are described. Ferroelastic deformation was observed at 1150°C in t′ and partially stabilized zirconia, which changes the microstructure for successive dislocation plasticity. In the oxide-dispersion-strengthened alloy INCOLOY MA 956, dislocations are impeded by oxide particles and move smoothly between the particles. At high temperatures, both the resting and traveling times control the average dislocation velocity. In MoSi2 single crystals of a soft orientation, dislocations with 1/2〈111〉 Burgers vectors are created in localized sources and move on {110} planes in a viscous manner. The dislocations in Al-Pd-Mn single quasicrystals are oriented in preferred crystallographic directions and move in a viscous way as well. On the basis of in situ observations, conclusions are drawn for interpreting macroscopic deformation behavior at high temperatures.


2019 ◽  
Vol 624 ◽  
pp. A136
Author(s):  
S. P. Thompson ◽  
A. Herlihy ◽  
C. A. Murray ◽  
A. R. Baker ◽  
S. J. Day ◽  
...  

Context. Laboratory analogues can provide physical constraints to the interpretation of astronomical observations of cosmic dust but clearly do not experience the same formation conditions. To distinguish between properties intrinsic to the material and properties imprinted by their means of formation requires extensive characterisation. Aims. Sol–gel methods can produce amorphous silicates with potentially high reproducibility, but often require long drying times (24+ h) at elevated temperatures in air, controlled atmosphere, or vacuum. We investigate the possibility that microwave drying can be used to form amorphous silicate on a timescale of ∼10 min and characterise their structural and spectroscopic properties relative to silicates produced by other drying methods. Methods. Microwave-dried amorphous MgSiO3, Fe0.1Mg0.9SiO3 and Mg2SiO4 are characterised using X-ray powder diffraction, total X-ray scattering, small angle X-ray scattering and mid-IR FTIR spectroscopy, and compared to samples produced from the same gels but dried in-air and under vacuum. The development of crystalline structure in the microwave-dried silicates via thermal annealing up to 999°C is also investigated using in situ X-ray powder diffraction. Results. At the inter-atomic level the silicate structures are largely independent of drying method, however larger-scale structured domains, ranging from a ∼few × 10 Å to ∼100’s Å in size, are observed. These are ordered as mass fractals with discernible variation caused by the drying processes. The mid-IR 10 μm band profile is also found to be influenced by the drying process, likely due to the way removal of water and bonded OH influences the distribution of tetrahedral species. However, microwave drying also allows Fe to be easily incorporated into the silicate structure. In situ annealing shows that for amorphous MgSiO3 crystalline forsterite, enstatite and cristobalite are high temperature phases, while for Mg2SiO4 forsterite crystallises at lower temperatures followed by cristobalite at high temperature. For Fe0.1Mg0.9SiO3 the crystallisation temperature is significantly increased and only forsterite is observed. Crystalline SiO2 may be diagnostic of Mg-rich, Fe-poor grain mineralogies. The results are discussed in relation to the different thermal conditions required for dust to crystallise within protoplanetary disk lifetimes. Conclusions. Sol–gel microwave drying provides a fast and easy method of producing amorphous Mg- and Fe,Mg-silicates of both pyroxene and olivine compositions. Their structure and spectroscopic characteristics although similar to silicates produced using other drying methods, exhibit subtle variations which are particularly manifest spectroscopically in the mid-IR, and structurally over medium- and long-range length scales.


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