An ESCA and SEM Study of Changes in the Surface Composition and Morphology of Low-Calcium Coal Fly Ash as a Function of Aqueous Leaching

1986 ◽  
Vol 86 ◽  
Author(s):  
Myra M. Soroczak ◽  
H. C. Eaton ◽  
M. E. Tittlebaum

ABSTRACTThe reactivity of coal fly ash is dependent on the chemical composition of the surface. As reactions occur the ash particle size decreases and new material is available for reaction. This means that the near-surface chemistry can also be important. In the present study the surface chemistries of three ashes are determined by x-ray photoelectron spectroscopy both before and after exposure to a hydrating/leaching environment. Scanning electron microscopy is used to reveal ash morphology. The concentration of sulfur, found at the ash surfaces as a sulfate, and sodium decreased after leaching while the amount of iron and aluminum increased. Other elements, including calcium, increased and decreased with leaching depending on which ash was analyzed. Changes which occurred in the ash morphology after the removal of leachable elements are discussed.

Clay Minerals ◽  
1992 ◽  
Vol 27 (4) ◽  
pp. 413-421 ◽  
Author(s):  
M. Soma ◽  
G. J. Churchman ◽  
B. K. G. Theng

AbstractThe surface composition of some halloysites with different particle morphology has been investigated by X-ray photoelectron spectroscopy (XPS) before and after removal of external Fe. The Fe(III) 2p3/2 binding energy of external Fe is appreciably smaller than that of structural Fe. Particle morphology is influenced by structural Fe content. The long-tubular halloysite has very little surface Fe, and its concentration tends to increase with the proportion of non-tubular particles in the samples. The spheroidal sample contains the most structural Fe which, however, does not appear to influence particle shape directly. Study by XPS indicates that Fe substitutes for Al in octahedral positions in approximately 1 : 2 proportion. As a result, an increase in octahedral vacancies and cation exchange capacity would be predicted. Further, halloysite layers within a crystal are generally inhomogeneous in composition. Built up like “onion skins”, the surface layers would either be enriched or depleted in Fe depending on the chemical environment in which crystal growth occurs.


2010 ◽  
Vol 1259 ◽  
Author(s):  
Srikanth Raghavan ◽  
Timothy C. Nelson ◽  
Tobias Denig ◽  
C D Stinespring

AbstractHalogen based (CF4 and Cl2) inductively coupled reactive ion etching (ICP-RIE) has been used to selectively etch silicon from 6H-SiC to produce a controlled number of carbon layers. After annealing at temperatures in the range of 550 °C to 1100 °C to reconstruct the near surface layers, x-ray photoelectron spectroscopy has been used to characterize the composition of the films. For the Cl2 based ICP-RIE, two carbon species are observed. One is due to carbon bound as SiC in the substrate and a second which can be attributed to graphene. In the case of CF4 based etching the situation is similar except the second peak is most closely aligned with p-type graphene. This is most likely due to electron transfer from the graphene to the trace levels of fluorine remaining on the surface after annealing.


Materials ◽  
2020 ◽  
Vol 13 (7) ◽  
pp. 1740 ◽  
Author(s):  
Darja Steiner Petrovič ◽  
Djordje Mandrino ◽  
Božidar Šarler ◽  
Jelena Horky ◽  
Andrea Ojdanic ◽  
...  

Two binary biodegradable Mg-alloys and one ternary biodegradable Mg-alloy (Mg-0.3Ca, Mg-5Zn and Mg-5Zn-0.3Ca, all in wt%) were investigated. Surface-sensitive X-ray photoelectron spectroscopy analyses (XPS) of the alloy surfaces before and after immersion in simulated body fluid (SBF) were performed. The XPS analysis of the samples before the immersion in SBF revealed that the top layer of the alloy might have a non-homogeneous composition relative to the bulk. Degradation during the SBF immersion testing was monitored by measuring the evolution of H2. It was possible to evaluate the thickness of the sample degradation layers after the SBF immersion based on scanning electron microscopy (SEM) of the tilted sample. The thickness was in the order of 10–100 µm. The typical bio-corrosion products of all of the investigated alloys consisted of Mg, Ca, P and O, which suggests the formation of apatite (calcium phosphate hydroxide), magnesium hydrogen phosphate hydrate and magnesium hydroxide. The bioapplicability of the analyzed alloys with regard to surface composition and degradation kinetics is discussed.


2005 ◽  
Vol 119 (1-3) ◽  
pp. 213-217 ◽  
Author(s):  
A OHKI ◽  
T NAKAJIMA ◽  
Y SAKAGUCHI ◽  
A IWASHITA ◽  
H TAKANASHI

Metals ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 1684
Author(s):  
Andrei Shoppert ◽  
Dmitry Valeev ◽  
Irina Loginova ◽  
Leonid Chaikin

One of the potential sources of alumina and mesoporous silica is the coal-fired thermal plants waste known as the coal fly ash (CFA). The studies of the alumina extraction from CFA are often focused on the preliminary desilication, but the efficiency of the alkali desilication is low due to formation of the desilication product—Na6[Al6Si6O24]·Na2X (DSP). This research is focused on the possibility of CFA desilication without formation of DSP using a leaching process with higher liquid to solid ratios (L/S) and alkali concentrations. The experimental data were analyzed using an artificial neural network (ANN) machine learning method and a shrinking core model (SCM). The investigation of the CFA morphology, chemical and phase composition before and after leaching were carried out by scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray diffraction (XRD). The present work shows that it is possible to avoid formation of DSP if using the L/S ratio >20 and concentration of Na2O—400 g/L during CFA leaching. The kinetics analysis by SCM showed that the process is limited by the surface chemical reaction at T <100 °C, and by diffusion through the product layer at T >100 °C, respectively. The SEM images of the solid residue after NaOH leaching under conditions that prevent the DSP formation show mullite particles with an acicular structure.


Author(s):  
Замир Валериевич Шомахов ◽  
Светлана Сергеевна Налимова ◽  
Рустам Мухамедович Калмыков ◽  
Кирилл Аубекеров ◽  
Вячеслав Алексеевич Мошников

Слои диоксида олова синтезированы гидротермальным методом из водного раствора SnF. Наночастицы серебра осаждены на поверхность полученных слоев методом фотовосстановления. Проведено исследование морфологии поверхности образцов методом атомно-силовой микроскопии. Размер наночастиц серебра зависит от концентрации раствора AgNO, используемого для проведения реакции фотовосстановления. При синтезе из раствора с концентрацией 0,02 М размер полученных наночастиц составляет варьируется от 10 до 100 нм, при увеличении концентрации раствора в два раза размер наночастиц составляет порядка 100 нм. С помощью рентгеновской фотоэлектронной спектроскопии изучен состав поверхности слоев до и после осаждения наночастиц серебра. При выбранных условиях синтеза формируется слой диоксида олова без посторонних включений, и происходит осаждение металлического серебра. Химический сдвиг пиков олова и кислорода после осаждения наночастиц серебра свидетельствует об обмене электронами между оловом и серебром. Полученные слои представляют интерес для применения в области полупроводниковых адсорбционных газовых сенсоров. Tin dioxide layers were synthesized by hydrothermal method from an aqueous solution of SnF. Silver nanoparticles were deposited on the surface of the obtained layers by the photoreduction method. The surface morphology of the samples was studied by atomic force microscopy. The size of the silver nanoparticles depends on the concentration of the AgNO solution used for the photoreduction reaction. When synthesized from 0,02 M solution with a concentration of, the size of the nanoparticles varies from 10 to 100 nm, when the concentration of the solution is doubled, the size of the nanoparticles is about 100 nm. The surface composition of the layers before and after the deposition of silver nanoparticles was studied using the X-ray photoelectron spectroscopy. It was shown that a layer of the tin dioxide is formed without external inclusions, and metallic silver is deposited. The chemical shift of the peaks of tin and oxygen after the deposition of silver nanoparticles indicates the exchange of electrons between tin and silver. The synthesized layers are of interest for application in the field of semiconductor adsorption gas sensors.


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