scholarly journals Hydrothermal Sintering and Oxidation of an Alumina-Supported Nickel Methanation Catalyst Studied Using In Situ Magnetometry

Catalysts ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 636
Author(s):  
Malebelo Maphutha ◽  
Dominic de Oliveira ◽  
Thulani M. Nyathi ◽  
Mohamed I. Fadlalla ◽  
Robert Henkel ◽  
...  
Keyword(s):  
Elevated Temperatures ◽  
Pressure Ratio ◽  
Particle Growth ◽  
Bimodal Distribution ◽  
Ex Situ ◽  
Hydrothermal Conditions ◽  
Co Conversion ◽  
Average Size ◽  
In Situ Magnetometry

The presented study investigated the effects of temperature (350–650 °C) and gas environment (pure Ar versus a H2O/H2 partial pressure ratio (PH2O/PH2) of 5) on the extent of sintering and oxidation of Al2O3-supported Ni0 nanoparticles (≈4 nm). We note that a PH2O/PH2 of 5 corresponds to a simulated CO conversion of 94% during methanation. Sintering and oxidation were studied using in situ magnetometry, while ex situ TEM analyses confirmed the particle sizes before and after the magnetometry-based experiments. It was found that increasing the temperature from 350 to 650 °C in Ar at atmospheric pressure causes a negligible change to the average size and degree of reduction (DOR) of the starting Ni0 nanoparticles. However, studying the same temperature window under hydrothermal conditions at 10 bar causes significant particle growth (≈9 nm) and the development of a bimodal distribution. Furthermore, the presence of steam decreases the DOR of Ni0 from 86.2% after initial activation to 22.2% due to oxidation. In summary, this study reports on the expected sintering and oxidation of Ni-based catalysts under high CO conversion conditions at elevated temperatures during methanation. Importantly, we were able to demonstrate how magnetometry-based analyses can provide similar size information (and changes thereof) as those observed with TEM but with the added advantage that this information can be obtained in situ.

Phase Evolution of Thermally Treated Amorphous Tricalcium Phosphate Nanoparticles

2008 ◽  
Vol 396-398 ◽  
pp. 595-598 ◽  
Author(s):  
Nicola Döbelin ◽  
Tobias J. Brunner ◽  
Wendelin J. Stark ◽  
Manuel Eggimann ◽  
Martin Fisch ◽  
...  
Keyword(s):  
Tricalcium Phosphate ◽  
Elevated Temperatures ◽  
Particle Growth ◽  
Phase Evolution ◽  
Flame Spray ◽  
Crystallite Growth ◽  
X Ray ◽  
Heat Treated ◽  
Flame Spray Synthesis

X-ray amorphous tricalcium-phosphate nanoparticles (ATCP) produced by flame spray synthesis were heat-treated at temperatures between 500 and 1000 °C and analyzed in situ by X-ray powder diffraction. The main phase occurring after crystallisation at 525 °C was α-TCP, minor phases were identified as β-TCP and hydroxyapatite. More elevated temperatures induced crystallite growth and the transformation of α-TCP into β-TCP. Above 900 °C no α-TCP was traceable anymore. α’-TCP was not observed in the experiment. This study shows that nanoparticulate α-TCP can be obtained by thermal treatment of an amorphous TCP nanoparticle in a temperature range where sintering effects such as particle growth and densification are moderate or nearly negligible.

High-temperature oxidation of CoGa: Influence of the crystallographic orientation on the oxidation rate

2002 ◽  
Vol 17 (10) ◽  
pp. 2489-2498 ◽  
Author(s):  
U. Koops ◽  
D. Hesse ◽  
M. Martin
Keyword(s):  
High Temperature ◽  
Crystallographic Orientation ◽  
High Temperature Oxidation ◽  
Elevated Temperatures ◽  
Electron Backscatter Diffraction ◽  
Ex Situ ◽  
Temperature Oxidation ◽  
Transmission Electron ◽  
Backscatter Diffraction

The crystallographic orientation plays an important role in high-temperature oxidation of the intermetallic compound CoGa. When CoGa is exposed to air at elevated temperatures, the oxide β–Ga2O3 is formed, and different scale growth rates are observed, depending on the crystallographic orientation of the CoGa grains. This dependence is a consequence of the anisotropy of the gallium diffusion rate through the β–Ga2O3 scale and of a topotaxial orientation relationship occurring between β–Ga2O3 and CoGa. The combination of ex situ techniques, such as transmission electron microscopy and electron backscatter diffraction with optical microscopy, applied in situ resulted in a thorough understanding of these relations and of the oxidation process in general.

Film/substrate interactions and superconducting properties of Tl(Ba1−xSrx)2Ca2Cu3Oy thin films on (001) SrTiO3 and SrTiO3-buffered (001) MgO substrates

1998 ◽  
Vol 13 (8) ◽  
pp. 2057-2066 ◽  
Author(s):  
A. P. Bramley ◽  
C. R. M. Grovenor ◽  
M. J. Goringe ◽  
J. D. O'Connor ◽  
A. P. Jenkins ◽  
...  
Keyword(s):  
Magnetron Sputtering ◽  
Elevated Temperatures ◽  
Rf Magnetron Sputtering ◽  
Buffer Layers ◽  
Ex Situ ◽  
Superconducting Film ◽  
Superconducting Transition ◽  
Current Densities ◽  
Film Substrate

We have developed a process for the fabrication of (001) oriented SrTiO3 buffer layers onto (001) MgO substrates by rf magnetron sputtering followed by a post-deposition heat treatment in air. Precursor films with Tl :Ba : Ca : Cu ratio 2 : 2 : 2 : 3 were deposited by dc magnetron sputtering onto both these buffered substrates and directly onto (001) SrTiO3 single-crystal substrates, and thalliated at elevated temperatures. Because of Sr diffusion from the substrate/buffer layer, and its subsequent substitution for Ba in the superconducting film, the single Tl–O layer phase Tl(Ba1−xSrx)2Ca2Cu3Oy was stabilized. Diffusion of Ba and Ca in the opposite direction led to the formation of a Ba–Ca–Ti–O compound at the interface. The Tl(Ba1xSrx)2Ca2Cu3Oy films typically have superconducting transition temperatures (Tc's) > 103 K and critical current densities (Jc's) > 2.9 × 105 A cm−2 at 77 K. Rs values measured on these films and scaled to 10 GHz were 3.0 mΩ at 80 K and <200 µΩ at 50 K for the film grown on SrTiO3 buffered MgO, and 2.0 mΩ and 1.0 mΩ at 50 K for the film grown directly onto the (001) SrTiO3 substrate. Films fabricated on (001) SrTiO3 using an in situ deposition technique with a substrate temperature around 100 °C lower than the ex situ thalliation temperature showed no evidence of an interfacial reaction layer.

Formation of Nickel Ferrite Films by Solid-State Reaction

1997 ◽  
Vol 3 (S2) ◽  
pp. 739-740
Author(s):  
Matthew T. Johnson ◽  
Paul G. Kotula ◽  
C. Barry Carter
Keyword(s):  
Thin Films ◽  
Solid State ◽  
Solid State Reaction ◽  
Nickel Ferrite ◽  
Elevated Temperatures ◽  
Film Growth ◽  
Ex Situ ◽  
First Case ◽  
Morphological Differences

Nickel ferrite (NiFe2O4) thin films are of potential interest for magnetic applications. In the present study, the production of NiFe2O4 by solid-state reaction between thin films of hematite (α-Fe2O3) and nickel oxide (NiO) on (0001) sapphire (α-Fe2O3) substrates has been examined. The NiFe2O4 thin films were prepared by two different methods. In the first case the NiFe2O4film was grown in situ in the deposition system, while in the second case the NiFe2O4 film was formed ex situ by reacting at elevated temperatures in air. These two methods of reaction lead to interesting morphological differences in the ferrite layers.Epilayers of α-Fe2O3 followed by NiO were deposited onto (0001) α-Al2O3 by pulsed-laser deposition (PLD) in 6 mTorr O2. NiFe2O4 films were obtained by reacting the starting films in two different ways: in situ (during film growth) and ex situ.. In both cases, the α-Fe2O3 films were grown under the same conditions while those for the deposition of the NiO layers were different.

Formation Two Dimensional Negative Islands At High Rate Cooling Of Ultra-Flat Surface Si(111)

2016 ◽  
Vol 11 (1) ◽  
pp. 94-99
Author(s):  
Sergey Sitnikov ◽  
Sergey Kosolobov ◽  
Aleksandr Latyshev
Keyword(s):  
Elevated Temperatures ◽  
High Rate ◽  
Ex Situ ◽  
Two Dimensional ◽  
Island Nucleation ◽  
Force Microscopy ◽  
Atomic Force ◽  
Atomic Mechanism ◽  
Negative Islands

In situ ultrahigh vacuum reflection electron and ex situ atomic force microscopy have been applied to investigate morphology transformations of the ultra-flat stepped Si(111) surface with wide (20–50 µm in diameter) singular terraces during sublimation and quenching from elevated temperatures. The formation of two dimensional negative (vacancy) islands has been observed on the wide terraces after the quenching from temperatures above 1 200°C. The increasing of the critical terrace size for the two-dimensional negative island nucleation has been explained by the changing of the atomic mechanism of mass transport on silicon surface.

scholarly journals High-temperature Fe oxidation coupled with redistribution of framework cations in lobanovite, K2Na(Fe2+ 4Mg2Na)Ti2(Si4O12)2O2(OH)4 – the first titanosilicate case

2019 ◽  
Vol 75 (4) ◽  
pp. 578-590 ◽  
Author(s):  
Elena S. Zhitova ◽  
Andrey A. Zolotarev ◽  
Frank C. Hawthorne ◽  
Sergey V. Krivovichev ◽  
Viktor N. Yakovenchuk ◽  
...  
Keyword(s):  
High Temperature ◽  
Elevated Temperatures ◽  
Iron Oxidation ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Different Temperatures ◽  
Bond Strengths ◽  
Increasing Temperature

The high-temperature (HT) behaviour of lobanovite, K2Na(Fe2+ 4Mg2Na)Ti2(Si4O12)2O2(OH)4, was studied using in situ powder X-ray diffraction in the temperature range 25–1000°C and ex situ single-crystal X-ray diffraction of 17 crystals quenched from different temperatures. HT iron oxidation associated with dehydroxylation starts at 450°C, similar to other ferrous-hydroxy-rich heterophyllosilicates such as astrophyllite and bafertisite. A prominent feature of lobanovite HT crystal chemistry is the redistribution of Fe and Mg+Mn cations over the M(2), M(3), M(4) sites of the octahedral (O) layer that accompanies iron oxidation and dehydroxylation. This HT redistribution of cations has not been observed in titanosilicates until now, and seems to be triggered by the need to maintain bond strengths at the apical oxygen atom of the TiO5 pyramid in the heteropolyhedral (H) layer during oxidation–dehydroxylation. Comparison of the HT behaviour of lobanovite with five-coordinated Ti and astrophyllite with six-coordinated Ti shows that the geometry of the Ti polyhedron plays a key role in the HT behaviour of heterophyllosilicates. The thermal expansion, geometrical changes and redistribution of site occupancies which occur in lobanovite under increasing temperature are reported. A brief discussion is given of minerals in which the cation ordering (usually for Fe and Mg) occurs together with iron oxidation–dehydroxylation at elevated temperatures: micas, amphiboles and tourmalines. Now this list is expanded by the inclusion of titanosilicate minerals.

scholarly journals In situ growth of SrFe12O19

2014 ◽  
Vol 70 (a1) ◽  
pp. C505-C505
Author(s):  
Cecilia Granados ◽  
Espen Bøjesen ◽  
Kirsten Jensen ◽  
Mogens Christensen
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Permanent Magnets ◽  
Elevated Pressure ◽  
Ex Situ ◽  
High Coercivity ◽  
Hydrothermal Conditions ◽  
Time Resolved ◽  
Kinetics Of

SrFe12O19 is a highly anisotropic ferrimagnetic compound with relatively high remanence and high coercivity, which is used in permanent magnets. Permanent magnets are everywhere in our daily life and they are responsible for the interconversion between motion and electricity in electrical components ranging from headphones to wind turbines. Three key parameters, important for making permanent magnets, are an anisotropic structure, size of the nanocrystallites and the microstructure. In situ X-ray powder diffraction has been used to follow the growth kinetics of SrFe12O19 under hydrothermal conditions. Synthesis of SrFe12O19 (Sr-Hexaferrite) nanocrystals by hydrothermal methods have the advantage of allowing exhaustive control of the reaction parameters. We have studied the growth and kinetics of SrFe12O19 by carring out time resolved synchrotron experiments at MAX-lab, Sweden. The experiments were carried out at elevated pressure (250 bar) and in temperatures ranging from 250 to 400 oC. The diffraction data allow us to follow the evolution of the crystallite size as function of temperature, time and composition. By controlling the composition of the precursor we can tailor the size of the nanocrystallites. The obtained data have shown that the synthesis takes place through a conversion of tiny hexagonal shaped FeOOH nanocrystallites into the SrFe12O19. Several ex situ studies under comparable conditions have been carried out to compare the magnetic properties and the obtained nanocrystallites have been investigated using high resolution laboratory powder diffraction data.

scholarly journals Growth and transgenerational acclimatization of juvenile Pocillopora damicornis

2020 ◽  
Author(s):  
Lev Gerstle
Keyword(s):  
Elevated Temperatures ◽  
Past Research ◽  
Lunar Cycle ◽  
Ex Situ ◽  
Life Stages ◽  
Pocillopora Damicornis ◽  
Transgenerational Plasticity ◽  
Important Exception

AbstractGlobal carbon emissions and associated increase in ocean temperatures are understood to be the main driving force in the degradation of coral reefs. Elevated temperatures impact various life stages of scleractinian corals, from the free-floating planulae of brooding corals to older, sexually viable individuals. With global warming, questions have arisen over whether organismal adaptation will be enough to keep up with the pace of environmental change. Researchers have pursued investigations of whether or not rapid acclimatization, through transgenerational plasticity, can help protect populations until genetic adaptation occurs. Acclimatization in corals has been widely studied in all life stages of corals, with the important exception of recently settled juveniles. In this study, I built upon past research by exposing adult Pocillopora damicornis colonies to elevated (28.5°C) or ambient (25.5°C) temperatures and examining the settlement ability and growth of their planulae ex situ. Juveniles from preconditioned parents fared better in higher temperatures compared to their naïve counterparts. Lunar timing of planula release between treatments peaked at different times in the lunar cycle. Peak planula release occurred on lunar day 23 for prestressed corals and on lunar day 7 for corals from ambient temperature seawaters. While future projects should follow up on these preliminary trials with in situ experiments to assess this phenomenon in the field, this study represents an important step in understanding how corals may be able to acclimatize and eventually adapt to climate change.

An in situ and ex situ TEM study of the formation of thin cobalt silicide films by molecular beam epitaxy on the silicon (100) surface

1988 ◽  
Vol 46 ◽  
pp. 884-885
Author(s):  
D. Loretto ◽  
J. M. Gibson ◽  
S. M. Yalisove ◽  
R. T. Tung
Keyword(s):  
Molecular Beam Epitaxy ◽  
Molecular Beam ◽  
Defect Density ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Ex Situ ◽  
Metal Base ◽  
In Situ Experiments ◽  
Potential Applications

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.

The use of transmission and analytical electron microscopy in studying reactions and phase transformations in thin film

1993 ◽  
Vol 51 ◽  
pp. 842-843
Author(s):  
K. Barmak
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Phase Transformations ◽  
Analytical Electron Microscopy ◽  
Ex Situ ◽  
Multilayer Thin Films ◽  
Absolute Concentration ◽  
Analytical Electron ◽  
Deposition Step

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.

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