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By Juan Hernández Ávila

This work studies the Molybdenum effect on the microestructure, mechanical properties of an as-cast ductile iron. For this study five ductile irons with different amounts of Molybdenum each were made in an induction furnace. In this material nodule count and nodularity is affected by the Molybdenum additions; The iron´s matrix, nodules and the phase were analyzed using scanning electron microscopy detecting Molybdenum only in the matrix. Mechanical properties such as hardness, microhardness, tensile strength and yield strength show increments as the Molybdenum amount is increased. In the same way, ferrite and pearlite phases display a variation in their percentage as the contents of the alloy element increase. This element has a marked influence on the pearlite interlaminar spacing. From the obtained results we conclude that Molybdenum in these quantities dissolves in solid ferrite solution during the solidification process, improving the material´s mechanical properties.

Jan 1, 2009

By R. Venugopal, V. K. Saxena, Veerendra Singh

"Ore morphology plays a vital role during the milling and liberation of minerals. This study was carried out to understand the role of mineral crystallography and mineral interfaces on the milling and liberation processes. Data related to mineral crystallography, Vickers Hardness Number and beneficiation processes were collected from literature, and detailed statistical analysis was conducted to relate these parameters. Review of the crystallographic information of minerals present in ores indicates that molecular weight and cell parameters significantly affect milling and liberation characteristics. Mineral interfaces were classified into the three categories of coherent crystals, semi-coherent and incoherent crystals, and breakage behaviors were studied. The studied cases revealed that these material interfaces control the micropore properties that play a vital role in the initiation of intergranular and intercrystalline fractures which occur in siliceous manganese ores and dolomite as a result of thermal treatment. In contrast, banded hematite jasper and coal exhibited a much more complex fracture pattern due to their coherent interfaces and finer physical associations. This study explains the effect of the various types of interfaces on milling, and the approach can be helpful in developing a methodology to enhance mineral liberation with minimum energy consumption.IntroductionComminution is a vital unit operation in the mineralprocessing, cement-making, power-generation and pharmaceutical industries. Its importance in mineral beneficiation operations is increasing every year as a result of the growing need to exploit lower-grade ore bodies and process reject materials (Blazy et al., 1994; DOE, 2005). Low-grade ores require significant energy during grinding to liberate the valuable minerals, which are further separated from the gangues by various beneficiation methods. Various attempts have been made to enhance mineral liberation during grinding to minimize energy consumption. Most of these studies focused on the analyses of the compression mechanism, chemical additives, thermal treatment, microwave treatment and electric disintegration (Klimpel and Austin, 1982; Norgate and Weller, 1994; Bearman et al., 1997; Kumar et al., 2010; Wang et al., 2011; Singh et al., 2012). However, many of these efforts had limited success, and there is a need to see the problem from a fresh perspective."

Jan 1, 2015

By Jingyuan Wang, Hengyi Zhang, Peng Lan, Ruitian Zhang, Jiaquan Zhang, Yang Li

"For the determination of mould taper and wall thickness, a 3-D numerical model of ingot-mould-hot top system has been made to evaluate the related ingot solidification process and the final soundness. The effect of mould wall thickness and the taper of its hot faces on the thermal history and the as cast structure of steel ingot has been revealed through the numerical simulation. It is shown that the ingot soundness can be improved remarkably by increasing the mould wall thickness, which is possibly beneficial to the mould life as well owning to an improved mould thermal state. The mould taper is vital to the ingot soundness but much less coherent to the mould temperature profiles. Under given casting situations, a larger mould taper can lead to a less intensity of the shrinkage porosities at the top part of ingot.IntroductionIngot casting is still one of important processes for steel production, which is adopted especially for the supply of large-sized semi-products of high quality special steels. The understanding to the solidification process is vital to both the yield improvement of casting production and the quality control of steel ingots, such as their soundness and homogeneity.The ingot processing and service performance are closely related to its defects, such as porosities and pipes[1,2], which are the most common but serious defects during ingots casting. In the late 1960s, Mahadevan and Murthy et al.[3], Irani and Kondic[4] began to analyze criteria for the prediction of shrinkage porosities in light metal casting. In 1980s, Niyama and Uchida[5], Hansen and Sahm[6,7] et al have successfully presented some related porosities and pipes criteria for steel casting. At the same time, numerical solidification simulation was well developed and applied to ingot quality studies[8-10]. However, due to the quick development of continuous casting, less emphasis has been given to the further study on ingot casting process. There leaves much work to be made for the comprehensive understanding to ingot quality improvement and the mould design by the aid of modern solidification technology[11, 12]. In this paper, the effects of mould taper and wall thickness on its thermal history, ingot solidification and the final soundness are numerically studied through solidification simulation, which has been adopted in mould design and industrial production of both the mould and its steel ingot."

Jan 1, 2012

By D J. Williams, C Zhang, F E. Herrera Cabrera

Farming on bauxite residue using screw propelled equipment (SPE) has been commonly practised to accelerate dewatering and as it promotes consolidation and enhances storage capacity. However, it is unclear when and how often farming should be conducted during the transition of bauxite residue from slurry to dry solids and how deep each slurry deposition should be. To address this issue, three desiccation tanks were established in the laboratory to investigate how much farming could enhance the desiccation and consolidation of tailings. The cuboid tanks, of 350 mm in height and 300 mm in width and length and with an opening on the top, were placed on load cells to monitor the water loss during desiccation and were instrumented with moisture and suction sensors designed and developed at the University of Queensland to measure the water content profile of the residue. The bauxite residue, composed of silt-size particles with low plasticity, was hydraulically deposited in the tanks as a slurry at 27% solid content, resulting in 100 mm depth of solid material settling. Evaporation was enhanced by placing two identical electrical fans above the tanks. Two phases were conducted. In the first phase, the two tanks were left untouched for evaluating non farmed conditions and for calibrating sensors, while in the second phase, three tanks were subjected to atemporal farming using purpose-built screw propelled equipment. The experiment was terminated when the residue was completely desiccated. This paper reports on the instrumented tank set-up and the results obtained to date.

Jul 1, 2021

We describe a new method of characterising the effect of dissolved materials on the rate of coalescence of bubbles in aqueous media. Single bubbles were allowed to rise to meet the surface of an aqueous solution, and the time of persistence between arrival and bursting of bubble was measured as a function of solute concentration. A laser beam was placed just above the surface of the liquid, with a detector in the light path, so that any disturbance at the surface could be seen as a break in the beam. The arrival of a bubble at the surface could be detected from the behaviour of the trace on an oscilloscope, and when the bubble broke, another significant change in the signal could easily be seen. The time between disruptions was reported as the persistence time. The effect of a homologous series of n-alcohols (C1 to C8) on the persistence time was measured, in aqueous solution. It was found that with increasing concentration of a particular solute, the persistence time increased up to a point, and then declined. However the magnitude of the persistence time was found to increase with increasing numbers of carbon atoms in the molecule. Bubbles of 1, 2 and 3 mm diameter were used. Persistence time increased with increasing bubble diameter, the maximum values observed being of order 100 secs. For a given solute, the persistence (drainage) time increased with increasing bubble diameter. The concentration Cmax at which the maximum persistence time was observed, was found to be independent of the bubble size. It decreased uniformly as the carbon number increased, and was well correlated by the function y1/2 (dy /dc) -2 I dc)-2 . There was no apparent correlation with the surface excess at maximum persistence time.

Jan 1, 2006

By Nadia H. Rafat, Iman S. El-Mahallawi, Hussein Badr, N. Khattab, Ahmed A. Abdel-Rehim

The basic part of solar water heaters is the collector and the main functional part of the collector is the absorber layer. In this work, a commercial locally available black painting (PACEN code 10382 colour 890), used for swimming pools solar heating, was modified by adding nano-graphite dispersion. The effect of nano-graphite particles percentage on the spectral absorbance of the material was examined on samples containing two values of 1.5 and 2.5% nano-graphite particles by weight. Fourier transform spectroscopy (FTIR) analysis was also used to identify the functional groups in the developed material. A simple experimental setup was designed to evaluate the performance of the developed nanodispersed selective coating polymeric based material, by measuring the increase in temperature of circulating water. It was shown that adding 1.5–2.5% nano-graphite particles to a polymer based black coating causes an increase in the optical absorptance, and an increase in the circulating water temperature.

Mar 1, 2018

By M. Fan

Coal has in general a wide range of density from minus 1.3 to plus 2.0 g/cm3 because of its variations in purity, rank, and porosity, etc. The coal density has great impact on froth flotation performance, but much less attention has been paid to particle density than particle size. Our previous research results demonstrated that cavitation-generated nanobubbles around 700 nm in diameter can significantly improve coal and phosphate flotation performance over a wide particle size range. In this study, the effect of nanobubble on the flotation performances of different density fractions (minus 1.3, 1.3-1.4, 1.4-1.5, 1.5-1.6, 1.6-1.8, 1.8-2.0, 2.2-2.2, and plus 2.2 g/cm3) of coal was investigated using a bank of 10-liter flotation cells, a specially designed 50-mm-inside-diameter column, and a 152-mm-inside-diameter column. It was found that nanobubble has the biggest impact on the flotation performance of 1.4-1.8 g/cm3 medium-density coal particles.

Feb 23, 2014

By Yuemin Zhao, Daniel Tao, Rick Honaker, Maoming Fan

"Froth flotation is the most widely used method of separating fine coal, especially coal with coking properties. However, froth flotation is not efficient for treating ultrafine coal and coarse coal particles. Our previous fundamental test results demonstrated that cavitation-generated nanobubbles around 700 nm in diameter can significantly improve coal and phosphate flotation performance over a wide particle size range. In this study, the effect of nanobubbles on the flotation performance of different particle size fractions of coal was investigated using a bank of 10-L flotation cells, a specially designed 50-mm inside diameter column and a 152-mm inside diameter column. It was found that nanobubbles that were either directly formed on or subsequently attached to the surface of coal particles during the froth flotation process improved flotation efficiency. The use of nanobubbles in a bank of mechanical cells flotation and column flotation significantly increased the flotation recovery at a given product grade. Nanobubbles increased the flotation rate constants of different coal particle sizes. The presence of nanobubbles in flotation slurry could extend the lower and the upper particle size limits for effective coal flotation.IntroductionFor minus 0.6 mm fine coal or minus 0.15 mm ultrafine coal particles, froth flotation is known to be the most efficient and the most cost-effective separation technique. However, flotation efficiency decreases sharply with ultrafine and relatively coarse coal particles. Studies have shown that the low flotation efficiency of ultrafine particles is mainly due to the low probability of bubble-particle collision (Yoon et al., 1989; Ralston and Dukhin, 1999). Enhanced flotation of fine and ultrafine coal can be achieved by increasing collision and attachment probabilities.The top size of particles that can be recovered by flotation depends on the combination of mineral properties and flotation devices. Turbulence in flotation devices is an important factor that affects the stability of bubble-particle aggregates. Even in the flotation of fine particles, bubble-particle detachment can significantly influence the kinetics of flotation taking place in mechanical cells, which provide intensive turbulent agitation (Deglon et al., 1999). Coarse particle flotation is more difficult, because increased agitation is required to maintain particles in suspension and coarse particles are more likely to detach under turbulent conditions (Mankosa and Kohmuench, 2002; Soto and Barbery, 1991). More efficient attachment of particles and improved flotation rate has been observed when tiny bubbles coexist with conventional-sized flotation bubbles (Attalla et al., 2000; Tao et al., 2010; Fan et al., 2010a, b, c, d; Fan et al., 2012)."

Jan 1, 2015

By M. O. Pekguleryuz, D. S. Aydin

The high temperature oxidation and ignition resistance of Mg-(0-6) wt% Nd alloys have been investigated via isothermal and continuous heating experiments conducted in air atmosphere. Alloy composition is observed to be effective in low levels (~ 0.5 %) in the ignition temperature (Ti) of the alloys; the Ti of pure Mg increased from 630 °C to 770 °C with 0.5 wt% Nd addition. However, no noteworthy improvement was achieved with further additions up to 6 wt% Nd. The initial microstructure was observed to determine the oxide structure on the surface due to the differing oxidation behavior of the phases (a-Mg + Mg12Nd intermetallics). It has been found that the formation of a Nd-depleted region at the subsurface due to extensive Nd oxidation at the oxide/intermetallic interface lowers the protective ability of the oxide scale.

Jan 1, 2015

By S. J. Moema, M. G. Maruma, L. A. Mampuru, M. E. Maja

"The most commonly used high-chromium white cast iron (HCWCI) is the hypoeutectic white cast iron that contains 2–3.5 wt.% C and 10–30% Cr. This type of material relies on hard, brittle M7C3 carbides to impart good wear resistance. Due to its good wear resistance, this material has found application in the mining industry and cement industry. However, it has low fracture strength and this challenge led to research aimed at refining the microstructure. This was done by the addition of niobium in the range between 0.1 and 0.6 wt.%. In the as-cast condition, the addition of niobium was found to increase the fracture strength due to the finer eutectic microstructure. The hardness was also found to have increased slightly compared to the reference alloy with no niobium additions. Low fracture strength after heat treatment was observed in the Nb-added HCWCI, which is believed to have been caused by the precipitation of secondary carbides and the transformation of the matrix from austenite to martensitic. IntroductionFor the past few years Mintek has been involved in a project in which a number of alloys have been identified for grinding media applications. The high-chromium white cast iron (HCWCI) alloys were among the alloys researched for this application. The knowledge acquired from the grinding ball media research has now been extended to mill liners, which have traditionally been made of manganese-, chromium- and chrome-molybdenum steels. The replacement of worn mill liners costs the mining industry a significant amount of money and this has led to a need for continuous research to prolong the life of the liners. During milling operations, liner wear has an adverse effect on the capacity of the mill, the energy efficiency and milling efficiency and finally leads to relining, to replace worn liners."

Jan 1, 2016

By Raj P. Singh Gaur

Due to high concentration of NaOH in the digested slurry after scheelite digestion, it is diluted to about 4N before filtration to separate sodium tungstate solution from the sludge (residue). However, in practice there may be deviations in the normality of NaOH present in the slurry. There may also be variations in the temperature of the slurry and filtration time. Slight variations in these parameters could cause tungsten losses in the sludge via the back reaction: Ca(OH)2 + Na2WO4? CaWO4 + 2NaOH This paper pertains to the effect of normality, temperature and time on the tungsten losses in the sludge that is separated from ?diluted-scheelite-slurry-in-NaOH? via filtration. Results indicated that tungsten losses in the filtered residue (sludge) were quite significant when the slurry temperature was kept at 70°C or higher. The effect of high temperature was less significant at the slurry normality of 3.6 or higher. Combination of low slurry normality (<3.6) and high temperature (>60°C) resulted into large W-losses in the sludge.

Jan 1, 2006

By David Whalen

Mobile equipment in oil sand mining operations experience more maintenance problems than similar equipment in other surface mines, due to soft underfoot conditions. Oil sand properties are known to vary with temperature, bitumen content and previous loading cycles. One of the challenges is the widely variable underfoot pressure which supports shovels and trucks. In the case of a heavy hauler driving on in-pit roads, each tire is supported by a different ground stiffness resulting in an apparent uneven surface. Driving over uneven ground causes twist in the truck frame, which is transmitted to the dump body. Through a finite element analysis of a haul truck dump body, it was shown that slight frame twists produce localized stresses in the intersections of the floor stiffeners. These stresses are at times greater than those resulting from the maximum ore weight and are primarily responsible for cracking in these intersections. Syncrude maintains high quality haul roads, which are constructed of gravel, and makes every effort to keep the shovel pit roads as smooth as possible. This problem cannot be avoided through operational practices only and must also be accounted for in the design of haul truck bodies.

May 1, 2003

By Diler Katircioglu-Bayel, Oner Yusuf Toraman, Safak Gokhan Ozkan

Calcite has found many applications in the industrialized countries recently, such as filler for paper, paint, plastics, rubber and food. Furthermore, calcite separates many toxic elements, and thus it is used in water treatment, and it is also used to raise the pH of drinking water. Due to its special features, calcite has been characterized as a useful coating and reinforcement filler for applications. Finer particle size of calcite has been determined to provide improved features for all of these applications. For submicron particle production, wet milling is selected over dry milling to produce finer particle sizes. Wet stirred media mills are also used in many industries. For that reason, this study investigated the effects of operating parameters on particle size reduction in the wet grinding process. The knowledge acquired by this study will allow the finding of optimal operating parameters for a stirred media mill to optimize specific energy consumption and reduce particle size.

By Diler Katircioglu-Bayel, Oner Yusuf Toraman, Safak Gokhan Ozkan

One of the most energy-intensive processes for producing submicron range calcite is stirred media mill. In the present work, numerous operating parameters such as solid mass fraction, grinding media size, media filling ratio, and grinding time have been investigated using a vertical type stirred media mill. The results are evaluated on the basis of mean particle size, specific surface area, and specific energy consumption. After conducting this study, optimum experimental conditions found to be as 70% media filling ratio, 25% solid mass fraction, 1 mm grinding media size, and 120 min grinding time. Besides, energy savings up to 22% were achieved with the choice of proper media size.

By Sunil Koppalkar, A. R. Laplante

"A Pilot Plant was installed in one of the grinding circuits of the Dome Mill, Ontario, Canada. Tests were conducted on a KCCD12 Knelson Concentrator to systematically analyze the effect of operating variables on the performance. The main objective of this test work was to explore the effect of very coarse (6 mm) feed size on GRG recovery and performance of the Knelson concentrator. Preliminary results have shown that coarse feed size is deleterious to maximizing recovery. Size-by-size GRG recoveries have shown an unusual trend in the sense that recoveries do not decrease monotonically with decreasing gold particle size. Similar trend observed in one other full-scale unit has been compared. The observed trend is probably linked to the feed size distribution and top size.INTRODUCTIONKnelson Concentrators are the most widely used semi-continues centrifuge gravity separation units for the recovery of gold and platinum group minerals (Xiao and Laplante 2004). The main advantages over the competing centrifugal gravity units are their design, operating simplicity and good separation efficiency that make them the most common choice for gravity circuit. Despite some characterization at bench scale and a limited characterization at full scale, there is a lack of a comprehensive study of impact of operating variables on efficiency that reflects realistic full scale operating practice. GRG characterization studies, at bench scale, on these units provide information about the occurrence of gold in ore samples but fail to provide adequate information about the effect of operating variables for full-scale units. It is well known fact that such work is difficult to undertake on full-scale units owing to the difficulties involved in sampling and systematic variation of operating parameters. To tackle these problems, a pilot facility consisting of a 12-in CD Knelson Concentrator, a feed screen and tailing pump was installed in one of the grinding circuits of Dome Mill. This paper describes the work carried out and the results.Porcupine Joint Venture (PJV)Porcupine Joint Venture was formed in 2002 between Placer Dome Inc. and Kinross Gold Corporation. The JV utilizes the milling capacity of the Dome Mill to process ore from Placer Dome and Kinross mines. The Dome Mill circuit has gravity concentration, cyanidation and CIP circuits to recover gold. Gravity recovery has been used at Dome Mill since inception to recover gold: first by using conventional jigs, which were eventually replaced by two Knelson Concentrators in 1993, one in each of the grinding circuits. Three more Knelsons joined the circuit in 2002 to improve gravity recovery. An Acacia Intensive Leach Reactor was also added in 2002 to process gold concentrates replacing shaking tables (Chong et al 2004)."

Jan 1, 2007

By Y. F. Liang

Fe-6.5wt.%Si alloy has excellent soft magnetic properties compared with conventional silicon steel. It is very brittle at room temperature due to appearance of ordered phases, like B2 and DO3. In this paper, we investigate the effect of ordering on cold workability of this alloy. Methods of rapid quenching and hot rolling were utilized. It is found that rapid quenching and proper heat treatment of the hot rolled sheet could decrease the degree of order due to the very high solidification rate and high cooling rate. The rapid quenched sheet and hot rolled sheet after proper heat treatment could be cold rolled without crack. Microstructure, phase ordering, micro hardness, and cold rolling properties were investigated by Optical Microscope, X-ray Diffraction, Micro Hardness Indenter and Four-high Mill.

Jan 1, 2009

By T. V. Jayaraman

Fe-Ga alloys, with compositions around 27.5 at % Ga, can be heat treated to obtain ? (ordered bcc), DO19 (ordered hexagonal), and L12 (ordered fcc) ordered structures. Our earlier work using polycrystalline samples had shown that magnetostriction is strongly influenced by ordering in this alloy. Here more detailed study of the correlation between ordering and magnetostriction using single crystals of Fe 27.5 at. % Ga alloys is reported. Single crystals of Fe 27.5 at % Ga were grown using Bridgman single crystal growth technique. X-ray and electron diffraction were used to study the ordering in this alloy. Magnetostriction measurements were carried out at no load conditions. Elastic constants were measured using Resonant Ultrasound Spectroscopy.

Jan 1, 2006

By Tony Lipiec, Ian Orford

"A key part of plant design is the selection of the design tonnage which is the hourly tonnage target that the equipment selection is based on. Its selection is critical for ensuring that the nominal tonnage which is critical to the financial performance of the project will be met. With deposits being developed at lower grades, higher tonnages and a higher degree of hardness variability, it is essential to ensure that the design process selects the comminution equipment which will be able to deal with the impact of this ore quality variation.Ore hardness and its variance are key factors to be taken into consideration for the selection of the design tonnage. It is well accepted that for the nominal or name plate tonnage to be consistently achieved, it is necessary to base the design tonnage on a hardness value greater than the average ore hardness of the deposit to be mined. The question is how much greater should this design value be to ensure that the nominal tonnage is met to the satisfaction of the project financial model. Standard industry practice is to set the design tonnage by:1. Select an ore hardness percentile that is greater than the average ore hardness to be the basis of the nominal tonnage. Typically either the 75th or 80th percentile value from the data set will be selected.2. Selection of a design factor to multiply by for determining the design tonnage, i.e. the design tonnage = tonnage (based on the average ore hardness) multiplied by design factor.This paper discusses the selection of the design ore hardness through the use of modelling or the use of a design factor. It further shows the impact of ore hardness variance on the capacity of the process and its ability to meet the nominal tonnage. Insight is provided as to what ore hardness percentile value should be selected balancing the shortfalls of tonnage for ores harder than the design value versus the above target production achieved for ores softer than the design ore hardness."

Jan 1, 2016

By N. H. J. Freire, D. Majuste

In this paper, the effects of some organic compounds on the current efficiency, cell voltage and specific energy consumption during nickel electrowinning, and on the deposit features (morphology, crystallographic orientation and nanohardness) were described. The organics tested here (extractant, diluent, flocculant, lubricating oil and acid mist suppressant) are currently used in industrial plants. The results indicated that only the flocculant and acid mist suppressant exhibit relevant negative impacts on the current efficiency and energy consumption. The current efficiency dropped from 93.6 % (organic-free solutions) to 86.0 % and to 92.8% in electrolytes containing 100 mg.L-1 of acid mist suppressant and flocculant, respectively. At this concentration, their addition to the electrolyte led to increases of the specific energy consumption in the order of 18 % (acid mist supressant) and 2 % (flocculant). Cyclic voltammetry showed that Ni nucleation occurs at more negative potentials at 50 and 100 mg.L-1 of these organics in the electrolyte, thus indicating an inhibition of the deposition process. The deposit quality decreased at the higher concentration of all organics, when more hydrogen pitting was observed. The acid mist suppressant caused delamination of the Ni deposit at 50 and 100 mg.L-1. The addition of 100 mg.L-1 of flocculant and acid mist suppressant to the electrolyte increased the nanohardness of the deposit around 31 and 72%, respectively. The increase in Ni deposit hardness may lead to a decrease in the material ductility, thereby affecting the stripping and cutting of Ni sheets. Our findings may be helpful since strong adverse effect of some organics that may be present in the electrolyte were identified, thus the industry can control and optimize the organic´s dosage in the corresponding operations.

Jan 1, 2016

By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Paolo Ciambelli, Lenore Rainey

"The evolution during oxidation of the internal structure of soot and carbon black particles was studied using high-resolution transmission electron microscopy (HRTEM) and an image analysis system. Increasing ordering to the carbon structure with increasing oxidation is observed. Measures of the increased order are increases in the fractional coverage of a cross section of the particles with a layered structure, a decrease in the mean interlayer spacing, and a decrease in the spread of the interlayer spacing. The changing structure of the carbon black impacts its properties, such as the rate of oxidation.There is considerable interest in the study of the structural changes of carbonaceous materials as a function of oxidation. Davis et al.1 measured the variation of carbon dioxide surface area of various coals as a function of residence time in a flow reactor. HRTEM measurements revealed that crystallite dimensions and interlayer spacings are altered by combustion. Ishiguro et al.2 showed that oxidation alters the structure of diesel soot. The aim of our current research is to develop a better understanding of the microstructural reordering of carbon blacks with implications to their properties. The carbon blacks used in this research have already been studied and their reactivities as a function of oxidation measured.3The methodology used in this work has already been described in detail elsewhere.4 This paper presents an application to quantify the structural changes of carbon black particles as a function of oxidation and graphitization. The technique used is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, chars, etc., possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure. The carbon structure has been variously described as turbostratic5 or as crumpled sheets6 to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as the composition of the source of the carbonaceous material. The value of electron micros¬copy in studying the morphology of such materials has been well established,2,7,8 although only a few attempts toward quantification have been made.The sample observed was carbon black CB330 from De¬gussa. One set of carbon black samples were oxidized in a thermo-gravimetric analyzer (TGA) in air at 575 0C, so that the conversion varied from 0 to 96%. Another set of carbon black samples were graphitized (Graphpac-GB by ALLTECH) and then oxidized in the TGA at 680 °C until 92% burnout was reached. The latter samples are called GB 0% and GB 92%, respectively.For the HRTEM observation a small portion of each sample was ultrasonically dispersed in ethanol. The suspension was deposited dropwise on a copper TEM grid coated with a lacey carbon film. The examination of the samples was carried out on areas that extend over the holes in the supporting film in order to avoid interference from the amorphous carbon background film An oriented gold crystal was used as a calibration standard and subjected to the same techniques as the carbon black samples."

Jan 1, 1998