scholarly journals Nitriding and Denitriding of Nanocrystalline Iron System with Bimodal Crystallite Size Distribution

Materials ◽  
2021 ◽  
Vol 15 (1) ◽  
pp. 143
Author(s):  
Aleksander Albrecht ◽  
Dariusz Moszyński
Keyword(s):  
Phase Transformations ◽  
Crystallite Size ◽  
Size Distribution ◽  
Diffraction Method ◽  
Mass Ratio ◽  
Iron Sample ◽  
Mass Conversion ◽  
Crystallite Sizes ◽  
Nanocrystalline Iron

An artificially prepared nanocrystalline iron sample with bimodal crystallite size distribution was nitrided and denitrided in the NH3/H2 atmosphere at 350 °C and 400 °C. The sample was a 1:1 mass ratio mixture of two iron samples with mean crystallite sizes of 48 nm and 21 nm. Phase transformations between α-Fe, γ’-Fe4N and ε-Fe3-2N were observed by the in situ X-ray powder diffraction method. At selected steps of nitriding or denitriding, phase transformations paused at 50% of mass conversion and resumed after prominent variation of the nitriding atmosphere. This effect was attributed to the separation of phase transformations occurring between sets of iron crystallites of 48 nm and 21 nm, respectively. This was due to the Gibbs–Thomson effect, which establishes the dependence of phase transformation conditions on crystallite sizes.

XRPD/TEM studies of model high-temperature shift catalysts

2006 ◽  
Vol 39 (4) ◽  
pp. 519-526 ◽  
Author(s):  
Rune E. Johnsen ◽  
Alfons M. Molenbroek ◽  
Kenny Ståhl
Keyword(s):  
High Temperature ◽  
Iron Oxide ◽  
Crystallite Size ◽  
Rietveld Method ◽  
Temperature Shift ◽  
Average Crystallite Size ◽  
Model Catalysts ◽  
Crystallite Sizes ◽  
Scherrer Equation

The combination of transmission electron microscopy (TEM) andin situX-ray powder diffraction (XRPD) for the investigation of four model high-temperature shift catalysts makes it possible to obtain and compare information concerning the crystallite and particle shapes and sizes before, during and after the reduction of the synthesized hematite-based model catalyst to the active magnetite-based catalyst. Two chromium-containing iron oxide model catalysts and two pure iron oxide model catalysts were synthesized from hydrated chloride or nitrate salts, resulting in particles with different shapes and sizes. The average crystallite sizes of four model catalysts were determined by XRPD using the Scherrer equation before and after the reduction. The crystallite sizes determined before the reduction were compared with particles sizes determined from TEM images of the same samples. These sizes were generally in good agreement. By using the Rietveld method combined with the Scherrer equation and the Lorentzian Scherrer broadening parameters, the development of the average crystallite size during thein situreduction was demonstrated. This showed that the average crystallite size of the remaining hematite increases when the reduction begins. Additionally, the average crystallite sizes of the reduced samples showed that the chromium-containing model catalysts have the smallest increase in the overall crystallite size.

Effect of crystallite size on the performance and phase transformation of Co3O4/Al2O3 catalysts during CO-PrOx – an in situ study

2017 ◽  
Vol 197 ◽  
pp. 269-285 ◽  
Author(s):  
Thulani M. Nyathi ◽  
Nico Fischer ◽  
Andy P. E. York ◽  
Michael Claeys
Keyword(s):  
Co Oxidation ◽  
Crystallite Size ◽  
Surface Area ◽  
Oxidation Activity ◽  
Temperature Range ◽  
Reformate Gas ◽  
Crystallite Sizes ◽  
Average Size ◽  
Water Gas

The preferential oxidation of carbon monoxide has been identified as an effective route to remove trace amounts of CO (approx. 0.5–1.0 vol%) in the H2-rich reformate gas stream after the low-temperature water–gas shift. Instead of noble metal-based catalysts, Co3O4-based catalysts were investigated in this study as cheaper and more readily available alternatives. This study aimed at investigating the effect of crystallite size on the mass- and surface area-specific CO oxidation activity as well as on the reduction behaviour of Co3O4. Model Co3O4 catalysts with average crystallite sizes between 3 and 15 nm were synthesised using the reverse micelle technique. Results from the catalytic tests revealed that decreasing the size of the Co3O4 crystallites increased the mass-specific CO oxidation activity in the 50–200 °C temperature range. On the other hand, the surface area-specific CO oxidation activity displayed a volcano-type behaviour where crystallites with an average size of 8.5 nm were the most active within the same temperature range. In situ characterisation in the magnetometer revealed that the Co3O4 crystallites are partially reduced to metallic Co above 225 °C with crystallites larger than 7.5 nm showing higher degrees of reduction under the H2-rich environment of CO-PrOx. In situ PXRD experiments further showed the presence of CoO concurrently with metallic fcc Co in all the catalysts during the CO-PrOx runs. In all experiments, the formation of fcc Co coincided with the formation of CH4. Upon decreasing the reaction temperature below 250 °C under the reaction gas, both in situ techniques revealed that the fcc Co previously formed is partially re-oxidised to CoO.

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.

Measurement of soil dry aggregate size distribution using the laser diffraction method

2021 ◽  
Vol 211 ◽  
pp. 105023
Author(s):  
C. Polakowski ◽  
A. Sochan ◽  
M. Ryżak ◽  
M. Beczek ◽  
R. Mazur ◽  
...  
Keyword(s):  
Size Distribution ◽  
Diffraction Method ◽  
Aggregate Size ◽  
Laser Diffraction ◽  
Aggregate Size Distribution

scholarly journals Particle Size Distribution of Various Soil Materials Measured by Laser Diffraction—The Problem of Reproducibility

Minerals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 465
Author(s):  
Cezary Polakowski ◽  
Magdalena Ryżak ◽  
Agata Sochan ◽  
Michał Beczek ◽  
Rafał Mazur ◽  
...  
Keyword(s):  
Particle Size ◽  
Particle Size Distribution ◽  
Normal Distribution ◽  
Size Distribution ◽  
Precise Measurement ◽  
Soil Analysis ◽  
Statistical Tests ◽  
Diffraction Method ◽  
Laser Diffraction ◽  
Method Analysis

Particle size distribution is an important soil parameter—therefore precise measurement of this characteristic is essential. The application of the widely used laser diffraction method for soil analysis continues to be a subject of debate. The precision of this method, proven on homogeneous samples, has been implicitly extended to soil analyses, but this has not been sufficiently well confirmed in the literature thus far. The aim of this study is to supplement the information available on the precision of the method in terms of reproducibility of soil measurement and whether the reproducibility of soil measurement is characterized by a normal distribution. To estimate the reproducibility of the laser diffraction method, thirteen various soil samples were characterized, and results were analysed statistically. The coefficient of variation acquired was lowest (3.44%) for silt and highest for sand (23.28%). Five of the thirteen tested samples were characterized by a normal distribution. The fraction content of eight samples was not characterized by normal distribution, but the extent of this phenomenon varied between soils. Although the laser diffraction method is repeatable, the measurement of soil particle size distribution can have limited reproducibility. The main cause seems to be small amounts of sand particles. The error can be amplified by the construction of the dispersion unit. Non-parametric statistical tests should be used by default for soil laser diffraction method analysis.

scholarly journals Long-range terrestrial laser scanning measurements of annual and intra-annual mass balances for Urumqi Glacier No. 1, eastern Tien Shan, China

2019 ◽  
Vol 13 (9) ◽  
pp. 2361-2383 ◽  
Author(s):  
Chunhai Xu ◽  
Zhongqin Li ◽  
Huilin Li ◽  
Feiteng Wang ◽  
Ping Zhou
Keyword(s):  
Mass Balance ◽  
Long Range ◽  
Tien Shan ◽  
Glacier Mass Balance ◽  
Surface Mass Balance ◽  
Mass Balances ◽  
Surface Mass ◽  
Mass Conversion ◽  
Geodetic Mass Balance

Abstract. The direct glaciological method provides in situ observations of annual or seasonal surface mass balance, but can only be implemented through a succession of intensive in situ measurements of field networks of stakes and snow pits. This has contributed to glacier surface mass-balance measurements being sparse and often discontinuous in the Tien Shan. Nevertheless, long-term glacier mass-balance measurements are the basis for understanding climate–glacier interactions and projecting future water availability for glacierized catchments in the Tien Shan. Riegl VZ®-6000 long-range terrestrial laser scanner (TLS), typically using class 3B laser beams, is exceptionally well suited for repeated glacier mapping, and thus determination of annual and seasonal geodetic mass balance. This paper introduces the applied TLS for monitoring summer and annual surface elevation and geodetic mass changes of Urumqi Glacier No. 1 as well as delineating accurate glacier boundaries for 2 consecutive mass-balance years (2015–2017), and discusses the potential of such technology in glaciological applications. Three-dimensional changes of ice and firn–snow bodies and the corresponding densities were considered for the volume-to-mass conversion. The glacier showed pronounced thinning and mass loss for the four investigated periods; glacier-wide geodetic mass balance in the mass-balance year 2015–2016 was slightly more negative than in 2016–2017. Statistical comparison shows that agreement between the glaciological and geodetic mass balances can be considered satisfactory, indicating that the TLS system yields accurate results and has the potential to monitor remote and inaccessible glacier areas where no glaciological measurements are available as the vertical velocity component of the glacier is negligible. For wide applications of the TLS in glaciology, we should use stable scan positions and in-situ-measured densities of snow–firn to establish volume-to-mass conversion.

scholarly journals Evaluating model parameterizations of submicron aerosol scattering and absorption with in situ data from ARCTAS 2008

2016 ◽  
Vol 16 (14) ◽  
pp. 9435-9455 ◽  
Author(s):  
Matthew J. Alvarado ◽  
Chantelle R. Lonsdale ◽  
Helen L. Macintyre ◽  
Huisheng Bian ◽  
Mian Chin ◽  
...  
Keyword(s):  
Optical Properties ◽  
Size Distribution ◽  
Aerosol Size Distribution ◽  
Visible Radiation ◽  
Submicron Aerosol ◽  
In Situ Data ◽  
Aerosol Absorption ◽  
Aerosol Scattering ◽  
The Impact

Abstract. Accurate modeling of the scattering and absorption of ultraviolet and visible radiation by aerosols is essential for accurate simulations of atmospheric chemistry and climate. Closure studies using in situ measurements of aerosol scattering and absorption can be used to evaluate and improve models of aerosol optical properties without interference from model errors in aerosol emissions, transport, chemistry, or deposition rates. Here we evaluate the ability of four externally mixed, fixed size distribution parameterizations used in global models to simulate submicron aerosol scattering and absorption at three wavelengths using in situ data gathered during the 2008 Arctic Research of the Composition of the Troposphere from Aircraft and Satellites (ARCTAS) campaign. The four models are the NASA Global Modeling Initiative (GMI) Combo model, GEOS-Chem v9-02, the baseline configuration of a version of GEOS-Chem with online radiative transfer calculations (called GC-RT), and the Optical Properties of Aerosol and Clouds (OPAC v3.1) package. We also use the ARCTAS data to perform the first evaluation of the ability of the Aerosol Simulation Program (ASP v2.1) to simulate submicron aerosol scattering and absorption when in situ data on the aerosol size distribution are used, and examine the impact of different mixing rules for black carbon (BC) on the results. We find that the GMI model tends to overestimate submicron scattering and absorption at shorter wavelengths by 10–23 %, and that GMI has smaller absolute mean biases for submicron absorption than OPAC v3.1, GEOS-Chem v9-02, or GC-RT. However, the changes to the density and refractive index of BC in GC-RT improve the simulation of submicron aerosol absorption at all wavelengths relative to GEOS-Chem v9-02. Adding a variable size distribution, as in ASP v2.1, improves model performance for scattering but not for absorption, likely due to the assumption in ASP v2.1 that BC is present at a constant mass fraction throughout the aerosol size distribution. Using a core-shell mixing rule in ASP overestimates aerosol absorption, especially for the fresh biomass burning aerosol measured in ARCTAS-B, suggesting the need for modeling the time-varying mixing states of aerosols in future versions of ASP.

Zirconium phase transformations observed by “in-situ” XRD analysis

Vacuum ◽  
2012 ◽  
Vol 86 (6) ◽  
pp. 785-788 ◽  
Author(s):  
Jan Riha ◽  
Pavol Sutta ◽  
Andrej Vincze ◽  
Rostislav Medlin
Keyword(s):  
Phase Transformations ◽  
Xrd Analysis ◽  
In Situ Xrd

Preparation and Characterization of Hexadecane Microcapsule Phase Change Materials by In Situ Polymerization

2013 ◽  
Vol 815 ◽  
pp. 367-370 ◽  
Author(s):  
Xiao Qiu Song ◽  
Yue Xia Li ◽  
Jing Wen Wang
Keyword(s):  
Particle Size ◽  
Phase Change ◽  
Phase Change Materials ◽  
In Situ Polymerization ◽  
Urea Formaldehyde ◽  
Agitation Speed ◽  
Urea Formaldehyde Resin ◽  
Formaldehyde Resin ◽  
Mass Ratio

Hexadecane microcapsule phase change materials were prepared by the in-situ polymerization method using hexadecane as core materials, urea-formaldehyde resin and urea-formaldehyde resin modified with melamine as shell materials respectively. Effect of melamine on the properties of microcapsules was studied by FTIR, biomicroscopy (UBM), TGA and HPLC. The influences of system concentration, agitation speed and mass ratio of wall to core were also investigated. The results indicated that hexadecane was successfully coated by the two types of shell materials. The addition of melamine into the urea-formaldehyde resin microcapsule reduced microcapsule particle size and microencapsulation efficiency. The influences of factors such as system concentration, agitation speed and mass ratio of wall to core to different wall materials microcapsules presented different variety trends of the microcapsule particle size.

scholarly journals Reversible Phase Transformations during In-Situ Heating of Uncapped Ge2Sb2Te5 Films

2021 ◽  
Vol 27 (S1) ◽  
pp. 2412-2414
Author(s):  
Chanchal Ghosh ◽  
Manish Singh ◽  
Paul Kotula ◽  
Helena Silva ◽  
C. Barry Carter
Keyword(s):  
Phase Transformations ◽  
In Situ Heating ◽  
Reversible Phase
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