Pressure acid leaching of nickel laterite ores: anin situdiffraction study of the mechanism and rate of reaction

2005 ◽  
Vol 38 (6) ◽  
pp. 927-933 ◽  
Author(s):  
Ian C. Madsen ◽  
Nicola V. Y. Scarlett ◽  
Barry I. Whittington
Keyword(s):  
Acid Leaching ◽  
Negative Temperature ◽  
Ex Situ ◽  
Nickel Laterite ◽  
X Ray ◽  
Laterite Ores ◽  
Wide Range ◽  
Processing Plants ◽  
Pressure Acid Leaching

This paper outlines the use of an innovative system for thein situinvestigation of hydrothermal reactions by X-ray diffraction. The key features are the use of: (i) a purpose-built capillary reaction vessel which allows close emulation of the conditions present in mineral processing plants; (ii) MoKα radiation, to ensure that the X-ray beam penetrates through the capillary, and (iii) an Inel CPS120 position-sensitive detector, to enable simultaneous collection of a wide range (120° 2θ) of diffraction data. The pressure acid leaching (PAL) of nickel laterite ores is used to illustrate the capabilities of this system, with a particular focus on the PAL of saprolite in strong H2SO4at 493 K. Saprolitic ore, which largely consists of serpentine mineral phases [(Mg,Fe,Ni,Al)3(Si,Al)2O5(OH)4], undergoes a number of mineralogical changes during both the acid leaching reaction and subsequent cooling, thus making it difficult to examine accurately using traditional post-reactionex situtechniques. In particular, kieserite (MgSO4.H2O), which forms during leaching, has a negative temperature coefficient of solubility, causing it to dissolve on cooling. Thein situtechnique described in this paper allows the direct observation of kieserite formation during the saprolite PAL at 493 K and its dissolution upon cooling to ambient temperature.

Time-resolved diffraction studies into the pressure acid leaching of nickel laterite ores: a comparison of laboratory and synchrotron X-ray experiments

2008 ◽  
Vol 41 (3) ◽  
pp. 572-583 ◽  
Author(s):  
Nicola V. Y. Scarlett ◽  
Ian C. Madsen ◽  
Barry I. Whittington
Keyword(s):  
Method Development ◽  
Acid Leaching ◽  
Ex Situ ◽  
Nickel Laterite ◽  
Time Resolved ◽  
X Ray ◽  
Laterite Ores ◽  
A Minor ◽  
Pressure Acid Leaching ◽  
Kinetics Of

This paper compares time-resolved diffraction experiments that have been performed using laboratory and synchrotron X-ray sources. The experiments investigated the mechanism and kinetics of pressure acid leaching of nickel laterite ores. The sample environment was a purpose-built capillary reaction vessel, and extensive method development was conducted in the laboratory using Mo Kα radiation prior to repeating and extending the experiments at the Daresbury Synchrotron Radiation Source, beamline MPW6.2. In general, the synchrotron results confirmed the findings from previously reported laboratory work and also confirmed the presence of a minor phase that had been ambiguous in the laboratory experiments,i.e.the formation of hematite in the pressure acid leaching of saprolite. The synchrotron measurements also extended the experimental programme to include poorly diffracting laterite components that could not be examined in the laboratory,e.g.nontronite. The results from these components supported the reaction mechanisms determined fromex-situanalyses conducted in larger scale autoclaves.

In Situ Studies of the Processing of Sol-Gel Produced Amorphous Materials Using Xanes, Saxs and Curved Image Plate XRD

1999 ◽  
Vol 590 ◽  
Author(s):  
DM Pickup ◽  
G Mountjoy ◽  
RJ Newport ◽  
ME Smith ◽  
GW Wallidge ◽  
...  
Keyword(s):  
Amorphous Materials ◽  
Sol Gel ◽  
Heat Treatments ◽  
Silica Gels ◽  
Ex Situ ◽  
High Count ◽  
X Ray ◽  
Image Plate ◽  
Wide Range

ABSTRACTSol-gel produced mixed oxide materials have been extensively studied using conventional, ex situ structural techniques. Because the structure of these materials is complex and dependent on preparation conditions, there is much to be gained from in situ techniques: the high brightness of synchrotron x-ray sources makes it possible to probe atomic structure on a short timescale, and hence in situ. Here we report recent results for mixed titania- (and some zirconia-) silica gels and xerogels. Titania contents were in the range 8–18 mol%, and heat treatments up to 500°C were applied. The results have been obtained from intrinsically rapid synchrotron x-ray experiments: i) time-resolved small angle scattering, using a quadrant detector, to follow the initial stages of aggregation between the sol and the gel; ii) the use of a curved image plate detector in diffraction, which allowed the simultaneous collection of data across a wide range of scattering at high count rate, to study heat treatments; and iii) x-ray absorption spectroscopy to explore the effects of ambient moisture on transition metal sites.

In Situ Synchrotron X-ray Absorption Experiments and Modelling of the Growth Rates of Electrochemically Deposited ZnO Nanostructures

2007 ◽  
Vol 1017 ◽  
Author(s):  
Bridget Ingham ◽  
Benoit N. Illy ◽  
Jade R. Mackay ◽  
Stephen P. White ◽  
Shaun C. Hendy ◽  
...  
Keyword(s):  
Growth Rates ◽  
High Resolution Electron Microscopy ◽  
Ex Situ ◽  
X Ray ◽  
Deposition Parameters ◽  
Wide Range ◽  
Electrochemically Deposited ◽  
Electrochemical Current ◽  
X Ray Absorption

AbstractZnO is known to produce a wide variety of nanostructures that have enormous scope for optoelectronic applications. Using an aqueous electrochemical deposition technique, we are able to tightly control a wide range of deposition parameters (Zn2+ concentration, temperature, potential, time) and hence the resulting deposit morphology. By simultaneously conducting synchrotron x-ray absorption spectroscopy (XAS) experiments during the deposition, we are able to directly monitor the growth rates of the nanostructures, as well as providing direct chemical speciation of the films. In situ experiments such as these are critical to understanding the nucleation and growth of such nanostructures.Recent results from in situ XAS synchrotron experiments demonstrate the growth rates as a function of potential and Zn2+ concentration. These are compared with the electrochemical current density recorded during the deposition, and the final morphology revealed through ex situ high resolution electron microscopy. The results are indicative of two distinct growth regimes, and simultaneous changes in the morphology are observed.These experiments are complemented by modelling the growth of the rods in the transport-limited case, using the Nernst-Planck equations in 2 dimensions, to yield the growth rate of the volume, length, and radius as a function of time.

scholarly journals Behavior of Iron Under Pressure Acid Leaching of Nickel Laterite Ores

2017 ◽  
Vol 133 (4) ◽  
pp. 68-75
Author(s):  
Shinichi HEGURI ◽  
Hirofumi SHOJI ◽  
Isao NISHIKAWA ◽  
Hiroshi KOBAYASHI ◽  
Atsushi IDEGAMI
Keyword(s):  
Acid Leaching ◽  
Nickel Laterite ◽  
Laterite Ores ◽  
Pressure Acid Leaching

scholarly journals Laser-heating system for high-pressure X-ray diffraction at the Extreme Conditions beamline I15 at Diamond Light Source

2018 ◽  
Vol 25 (6) ◽  
pp. 1860-1868 ◽  
Author(s):  
Simone Anzellini ◽  
Annette K. Kleppe ◽  
Dominik Daisenberger ◽  
Michael T. Wharmby ◽  
Ruggero Giampaoli ◽  
...  
Keyword(s):  
Light Source ◽  
Laser Heating ◽  
Theoretical Data ◽  
Heating System ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Diamond Anvil

In this article, the specification and application of the new double-sided YAG laser-heating system built on beamline I15 at Diamond Light Source are presented. This system, combined with diamond anvil cell and X-ray diffraction techniques, allows in situ and ex situ characterization of material properties at extremes of pressure and temperature. In order to demonstrate the reliability and stability of this experimental setup over a wide range of pressure and temperature, a case study was performed and the phase diagram of lead was investigated up to 80 GPa and 3300 K. The obtained results agree with previously published experimental and theoretical data, underlining the quality and reliability of the installed setup.

Atomic Layer Deposition of LiF and Lithium Ion Conducting (AlF3)(LiF)x Alloys Using Trimethylaluminum, Lithium Hexamethyldisilazide and Hydrogen Fluoride

2017 ◽  
Author(s):  
Younghee Lee ◽  
Daniela M. Piper ◽  
Andrew S. Cavanagh ◽  
Matthias J. Young ◽  
Se-Hee Lee ◽  
...  
Keyword(s):  
Lithium Ion ◽  
Atomic Layer ◽  
Mass Gain ◽  
Alloy Film ◽  
Ex Situ ◽  
X Ray ◽  
Layer Deposition ◽  
Ion Conducting ◽  
Good Agreement

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH<sub>3</sub>)<sub>3</sub> as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm<sup>2</sup> cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF<sub>3</sub> and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF<sub>3</sub>)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF<sub>3</sub>)(LiF)<sub>x</sub> alloy film was measured as σ = 7.5 × 10<sup>-6</sup> S/cm.</div>

In Situ X-Ray Diffraction Investigations during Diffusion Anneals of Ni-Cu Thin Film Diffusion Couples

2010 ◽  
Vol 89-91 ◽  
pp. 503-508 ◽  
Author(s):  
J. Sheng ◽  
U. Welzel ◽  
Eric J. Mittemeijer
Keyword(s):  
Thermal Stresses ◽  
Stress Generation ◽  
Ex Situ ◽  
Diffusion Annealing ◽  
X Ray Diffraction ◽  
Individual Layer ◽  
X Ray ◽  
Bilayer System ◽  
Stress Changes

The stress evolution during diffusion annealing of Ni-Cu bilayers (individual layer thicknesses of 50 nm) was investigated employing ex-situ and in-situ X-ray diffraction measurements. Annealing at relatively low homologous temperatures (about 0.3 - 0.4 Tm) for durations up to about 100 hours results in considerable diffusional intermixing, as demonstrated by Auger-electron spectroscopy investigations (in combination with sputter-depth profiling). In addition to thermal stresses due to differences of the coefficients of thermal expansion of layers and substrate, tensile stress con-tributions in the sublayers arise during the diffusion anneals. The obtained stress data have been discussed in terms of possible mechanisms of stress generation. The influence of diffusion on stress development in the sublayers of the diffusion couple during heating and isothermal annealing was investigated by comparing stress changes in the bilayer system with corresponding results obtained under identical conditions for single layers of the components in the bilayer system. The specific residual stresses that emerge due to diffusion between the (sub)layers in the bilayer could thereby be identified.

In situ X-ray Scattering Study of the Formation of Au Nano Crystals During Thermal Annealing

2007 ◽  
Vol 1027 ◽  
Author(s):  
Do Young Noh ◽  
Ki-Hyun Ryu ◽  
Hyon Chol Kang
Keyword(s):  
Thermal Annealing ◽  
Bragg Reflection ◽  
Ex Situ ◽  
X Ray ◽  
Force Microscopy ◽  
X Ray Scattering ◽  
Atomic Force ◽  
Au Thin Films ◽  
Ray Scattering

AbstractThe transformation of Au thin films grown on sapphire (0001) substrates into nano crystals during thermal annealing was investigated by in situ synchrotron x-ray scattering and ex situ atomic force microscopy (AFM). By monitoring the Au(111) Bragg reflection and the low Q reflectivity and comparing them with ex situ AFM images, we found that polygonal-shape holes were nucleated and grow initially. As the holes grow larger and contact each other, their boundary turns into Au nano crystals. The Au nano crystals have a well-defined (111) flat top surface and facets in the in-plane direction.

Size dependent behavior of Fe3O4crystals during electrochemical (de)lithiation: an in situ X-ray diffraction, ex situ X-ray absorption spectroscopy, transmission electron microscopy and theoretical investigation

2017 ◽  
Vol 19 (31) ◽  
pp. 20867-20880 ◽  
Author(s):  
David C. Bock ◽  
Christopher J. Pelliccione ◽  
Wei Zhang ◽  
Janis Timoshenko ◽  
K. W. Knehr ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
X Ray ◽  
Size Dependent ◽  
Transmission Electron ◽  
Dependent Behavior ◽  
X Ray Absorption

Crystal and atomic structural changes of Fe3O4upon electrochemical (de)lithiation were determined.

scholarly journals X-Ray Fluorescence Analysis of a Gold Ibex and other Artifacts from Akrotiri

2019 ◽  
Vol 11 ◽  
Author(s):  
A. G. Karydas ◽  
T. Pantazis ◽  
C. Doumas ◽  
A. Vlachopoulos ◽  
P. Nomikos ◽  
...  
Keyword(s):  
Bulk Composition ◽  
Fluorescence Analysis ◽  
Wall Painting ◽  
Inorganic Elements ◽  
X Ray ◽  
Wide Range ◽  
Soldering Technology ◽  
Excavation Area

In-situ X-ray fluorescence analysis (XRF) of ancient artifacts from the excavation area was performed using a novel X-ray instrumentation, composed of a portable silicon PIN thermoelectrically cooled X-ray detector, a miniature X-ray source, and portable data acquisition devices. The main objective of the analyses in Akrotiri was to explore the potential of the technique to provide answers to a wide range of archaeometric questions regarding the bulk composition of metal alloys, especially of gold, the characterization of corrosion products in bronze artifacts, identification of inorganic elements which are fingerprints of the minerals used in wall-painting pigments, and of the painting materials and techniques used for the decoration of clay vase surfaces. Among the analysed artifacts are a unique gold ibex, a bronze dagger and blade, various pigments from the wall paintings of room 3 in Xeste 3, decoration pigments from rosettes of faience, a bichrome jug, and other clay vases. The results of the in-situ XRF survey, primarily those of the bulk composition and soldering technology of the gold ibex, are discussed and compared with literature.

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