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By Florian Kongoli

Slags and fluxes are important interchangeable dimensions of pyrometallurgical processes. They can increase the efficiency of the smelting, converting and refining processes and improve the quality of the final products. A good slag should have appropriate physicochemical properties such as low liquidus temperature, optimal viscosity, maximum ability to attract undesirable elements, minimum potential of attracting valuable elements, etc .. A good flux, on the other hand, when properly used, can considerably improve the physicochemical properties of the slag since by modifYing its chemical composition it could decrease the liquidus temperature, improve viscosity etc.. Consequently, the choice of a good slag and the corresponding fluxing strategies has become indispensable in most of industrial processes. However, the properties of multi component slags as well as the effect of several fluxes are known only empirically and confusion exists in the literature and in the industrial practice. In today's reality of frequent changes in the composition of raw materials and that of the fluxes themselves, in the existing or new developing technologies, the quantification of the thermophysicochemical properties of multicomponent slags and the effect of fluxes becomes indispensable. This paper reviews some of the work carried out by the author's group during the last ten years on the quantification of the thermophysicochemical properties of multicomponent slags and on the effect of fluxes in several smelting and converting processes in close relation to their individual characteristics. Several examples have been given in order to demonstrate the fact that when taken outside the context some fluxes can become in fact anti-fluxes.

Jan 1, 2003

By Florian Kongoli

Slags and fluxes are important interchangeable dimensions of pyrometallurgical processes. They can increase the efficiency of the smelting, converting and refining processes and improve the quality of the final products. A good slag should have appropriate physicochemical properties such as low liquidus temperature, optimal viscosity, maximum ability to attract undesirable elements, minimum potential of attracting valuable elements, etc .. A good flux, on the other hand, when properly used, can considerably improve the physicochemical properties of the slag since by modifying its chemical composition it could decrease the liquidus temperature, improve viscosity etc.. Consequently, the choice of a good slag and the corresponding fluxing strategies has become indispensable in most of industrial processes. However, the properties of multicomponent slags as well as the effect of several fluxes are known only empirically and confusion exists in the literature and in the industrial practice. In today's reality of frequent changes in the composition of raw materials and that of the fluxes themselves, in the existing or new developing technologies, the quantification of the thermophysicochemical properties of multicomponent slags and the effect of fluxes becomes indispensable. This paper reviews some of the work carried out by the author's group during the last ten years on the quantification of the thermophysicochemical properties of multicomponent slags and on the effect of fluxes in several smelting and converting processes in close relation to their individual characteristics. Several examples have been given in order to demonstrate the fact that when taken outside the context some fluxes can become in fact anti-fluxes.

Jan 1, 2003

By Alex I. Kociubczyk, Wilky Desrosin, Lucía Mabel Boycho, Alicia E. Ares, Carlos E. Schvezov

In the present research, commercially pure Sn and Zn, and Sn-Zn alloys (Sn-1wt.%Zn, Sn- 2wt.%Zn, Sn-4wt.%Zn, Sn-8wt.%Zn and Sn-8.9wt.%Zn, weight percent) were obtained by a horizontal directional solidification process with two opposite senses and heat extraction. The solidification process was realized using a horizontal furnace with two heat extraction systems at both ends. The temperature was measured using eight K-type thermocouples and an electronic recorder of temperature data. The resulting structures were analyzed using optical microscopy. From the solidification process the thermal and metallographic parameters were determined in all samples. The presence of defects in the solidified pieces was observed. Internal defects pretended to be dependent not only on the composition of the alloys under consideration but also on the size of the structures formed, also, on the velocities and accelerations of interphases, and on the variation of thermal gradients. A model of the phenomenon from the first principles is presented.

Jan 1, 2015

By Chengyi Ding, Xuewei Lv, Changyang Ji, Rende Zhang, Xiangwei Zheng

Inexpensive and high-quality sinter has an extraordinary position in iron making, and there are many factors influencing the sintering. This research takes the basicity and coal dosage as research subjects to do the experiments based on cost analysis with sinter pot experiment system. Linear program is taken to make the schemes of ore blending. During the experiments of changing basicity from 1.6 to 2.3, the properties and microstructures of the sinter are studied. It comes to a conclusion that increasing the basicity is beneficial to sinter quality but leads to higher cost. To further ascertain the cost of sinter and the potential of saving coke, the work of improving coal dosage is taken on the basis of experiments of changing basicity. Through analyzing the results, a formula (Y=1849+261.1R-130.6C) is proposed which indicates the relation among the cost, basicity and fixed carbon content. And it works well for actual production.

Jan 1, 2015

By H. Y. Sohn, M. Y. Mohassab-Ahmed

"As part of research to develop a novel flash ironmaking process using reduction of iron ore concentrate by natural gas or hydrogen, sulfur and phosphorus distribution ratios between MgOsaturated slag and iron were determined in the temperature range 1550-1650°C under three different gas atmospheres: H2/H2O, H2/H2O/CO/CO2, and CO/CO2. The distribution coefficients of sulfur (Ls) were 4.0, 2.0, and 0.8, respectively, under these atmospheres. The distribution coefficients of phosphorus (Lp) were, respectively, 8, 17, and 20 under these atmospheres. In the flash process over -25 wt% P and S volatilize during ore concentrate downward flight in the reactor shaft in addition to avoiding coke. Therefore, iron produced by the flash ironmaking process would have much lower sulfur contents than the typical hot metal produced by the BF.IntroductionGiven the issues related to large carbon dioxide emissions and energy consumption in the existing ironmaking technologies, a novel flash ironmaking technology was conceived by Sohn [1-3] at the University of Utah. This technology is the first ironmaking process that will convert iron ore concentrate directly to metallic iron in-flight. This process will produce iron directly from concentrate without requiring pelletization or sintering and avoid the need for coke. In addition, this process concept takes full advantage of the fine particle size of concentrate with a large surface area, which permits rapid reduction by a gas. In this novel ironmaking process, potential reductants and fuels are H2, natural gas, and coal gas. Therefore, an iron-slag bath is expected to be at equilibrium with gas atmospheres of mainly H2/H2O or CO/CO2/H2/H2O, respectively, corresponding to the use of H2 or natural gas/coal gas. Since the effects of an H2O- containing atmosphere on slag properties have not been studied before, it is critical for the development of the novel flash process to determine these effects. In H2-H2O-CO-CO2 gas mixtures under ironmaking conditions, H20 was found to have the most pronounced effect on the slag chemistry [ 4, 5]. In addition, it was found in this laboratory that water in the gas atmosphere affected the distribution of Mn between slag and molten iron [6]. Most previous work used CO/CO2 gas mixture to control oxygen partial pressure (p02) [7, 8]. Others used only inert atmospheres [9], although Kor and Richardson [10] used a mixture of C02/H2 to control p02. For phosphorus, previous research focused on Ar [11], Ar-CO mixture [12], CO [13], CO/CO2 [14] or N2/CO [15]. Therefore, it was necessary to investigate the effect of water vapor content in H2-H2O-CO-CO2 mixtures on the equilibrium distribution of sulfur and phosphorus between CaO-MgOsatSiO2-Al2O3-FeO- MnO (0.2-0.8 wt%)-P2O5 (0.1-0.9 wt%) slag and molten iron as part of the development of the novel flash ironmaking technology."

Jan 1, 2014

By Donghai Li, Cheng Pan, Xuewei Lv, Mei Liu, Enguang Guo

"Phosphorite is the main raw material for the production of phosphorus in chemical industry. More attentions have been drawn to the phosphorite concentrate beneficiated from low-grade phosphorite due to the decrease of high-grade phosphorite. For another, the agglomeration process is necessary for the phosphorite concentrate after beneficiation process. The mineralogy and sintering process of the phosphorite from Leshan, China were studied in this work. The result shows that the main phases in the phosphorite are fluorapatite (Ca3(P04)3F), hydroxylapatite (Cas(P04)3(0H)), quartz (Si02) and dolomite (CaMg(C03)2). The yield of the sinter increases with increasing the carbon dosage to 7%, and then decreases when it continuously increases. Similar regularities were found for the strength and the content of P20s of the sinter. The best strength of the sinter as well as its P205 content were discovered when the carbon dosage is 7%. Fluorapatite ((Ca5(P04)3)F) is the main phase in the sinter while fuggerite (Ca2MgSiz01) is the main binder phase.IntroductionPhosphorus is an important foundation industrial raw material of national defense industry, food industry and chemical industry, where it is used to produce red phosphorus, phosphonium hydroxide, phosphorus pentasulfide and phosphoric anhydride[l-2]."

Jan 1, 2013

By M. Z. Sukiennik

A static method for vapor pressure measurement up to 1450 K and above 1 hPa is presented. The method is designed for equilibrium and kinetic studies of metallic systems, including those with a chemical reaction. Application examples are given for determination of activities in condensed phases, and heterogeneous reaction rates and equilibrium constants.

Jan 1, 1993

By Florian Kongoli

"Lime ferrite" slag with limited silica content has proven to be a valuable choice in the modem processes of copper smelting and converting due to several advantages that this slag offers compared to classical silicate slags. Nevertheless the liquidus surface of this slag has been experimentally measured only at low oxygen potentials such as in equilibrium with iron or hear it and in air. Although most of the smelting and converting processes that use this slag occur at intermediate oxygen potentials, the liquidus surface of this slag is not known at these conditions and the effect of oxygen potential and silica has not been correctly understood. This has brought some confusion in literature as well as in the industrial practice. In this work the liquidus surface of the calcium ferrite slags has been quantified by the means of a new thermophysicochemical model and a new type of liquidus surface diagrams which are very convenient for any industrial process that uses calcium ferrite slags. These diagrams can be easily used to select the lowest liquidus temperature of calcium ferrite slags at a minimum cost and can help design several fluxing strategies in copper smelting and converting processes. The effect of the oxygen potential and silica is also quantified and important industrially related conclusions are drawn.

Jan 1, 2003

By Florian Kongoli

"Lime ferrite" slag with limited silica content has proven to be a valuable choice in the modem processes of copper smelting and converting due to several advantages that this slag offers compared to classical silicate slags. Nevertheless the liquidus surface of this slag has been experimentally measured only at low oxygen potentials such as in equilibrium with iron or near it and in air. Although most of the smelting and converting processes that use this slag occur at intermediate oxygen potentials, the liquidus surface of this slag is not known at these conditions and the effect of oxygen potential and silica has not been correctly understood. This has brought some confusion in literature as well as in the industrial practice. In this work the liquidus surface of the calcium ferrite slags has been quantified by the means of a new thermophysicochemical model and a new type of liquidus surface diagrams which are very convenient for any industrial process that uses calcium ferrite slags. These diagrams can be easily used to select the lowest liquidus temperature of calcium ferrite slags at a minimum cost and can help design several fluxing strategies in copper smelting and converting processes. The effect of the oxygen potential and silica is also quantified and important industrially related conclusions are drawn.

Jan 1, 2003

By Lin Li, Wen Shi, Hua Wang

"Specimens of the ultra-low carbon bake hardening steel were soaked for 1 min to 5 min, and then cooled by water quenching. The internal friction experiments were carried out to detect the spectra of the specimens. Results show that Snoek peaks are present in all the specimens, however, an obvious Snoek-Koster peak is found only in the 5 min-annealed specimen. Besides, tensile results indicate that the bake hardening values increase with the annealing time prolonging from 1 min to 3 min, but decrease as the annealing time prolongs further to 5 min. The solute distributions in the specimens were characterized by three dimensional atom probe. Some segregated C and V are found in the 1 min-annealed specimen, and the C and V contents decrease as annealing time prolongs to 5 min.1. IntroductionAs an excellent member of automotive body panel materials, various types of bake hardening (BH) steels have been developed since 1980s. Bake hardening property, as one of the most important mechanical properties, has been studied by many researchers [ 1-5]. As is known, BH phenomenon is generally controlled by the interaction between solute C and dislocations. The Snoek peak of internal friction (IF) is very popular in the investigation of solute C [6-9]. However, result of internal friction cannot suggest the distribution pattern of solute C as well as its influence on BH phenomenon.Three dimensional atom probe (3DAP) can diagnose solute element atoms as well as nano-sized precipitates, and it is the only instrument that currently can identify the identities of individual atoms in a material and measure their spatial coordinates with the resolution close to 0.3 nm [10]. There have been a number of studies about using 3DAP to detect solute elements as well as nanometer sized precipitates [11-19]. For example, Hono et al. [16] used 3DAP to determine the solute elements in an age-hardened Mg-Ca-Zn alloy, and they also obtained the distribution patterns of the observed elements."

Jan 1, 2011

By Guo Chen, Yifeng Shi, Xiaobiao Shang, Nanshang Shen, Bangqi Zhang, Jinhui Peng, Junruo Chen

"The energy is introduced directly into the volume of the honeycomb ceramic regenerator due to the complex interaction of microwaves with minerals in microwave gas heating system. A three-dimensional numerical model is developed to simulate the electromagnetic field by solving Maxwell's equations using finite-difference time-domain method. Computational result is presented for the microwave power absorption of the regenerator. Effects of the dielectric constant and the effective loss factor on the microwave power absorption in the regenerator are studied as well. Numerical results show that the heating pattern strongly depends on the dielectric property of the regenerator. The demonstration of the model of electromagnetic field distribution can be applied effectively and efficiently to optimize the fundamental parameters in the microwave heating processing.IntroductionIn recent years, microwave energy has been utilized in many fields, such as food processing, chemical engineering and mineral processing [l]. In contrast to conventional heating, where heat is transferred from a surface to the interior, microwave energy is introduced directly into the volume of minerals due to the complex interaction of the microwave with the mineral. Based on volumetric heating effects, microwave heating has several advantages such as pollution free, rapid heating technique, internal heating, high efficiency over conventional heating [ 1-4]."

Jan 1, 2013

By Vaughan R. Voller

"Over the last ten years an increasing number of heat and mass transfer models of solidification processes have been presented in the literature. A key component in these models is the coupling between thermal and solute fields. This is achieved by developing relationships based on the behavior at the microscopic scale in the casting (typically a secondary dendrite arm space). An important class of models in this respect are models that describe the local scale redistribution of solute alloy components-collectively referred to as microsegregation models. This paper explores this class of models.IntroductionModeling takes a key role in processing materials for properties. This is particularly time in solidification processes where current computer techniques allow for a detailed treatment of the critical macroscopic phenomena. Typically these macro scale models consist ·of three main coupled components.1. A model of flow in the melt and solid + liquid mushy region.2. A model of heat transfer.3. A model of solute transport.The focus of this paper is the solute transport component, in particular the manner in which process scale transport is coupled to transport ·at the local scale of the solid-liquid interface. This step requires a modeling of the redistribution of solutes at the scale of the secondary arm spaces in the dendritic mushy region-a process referred to as microsegregation. Basic microsegregation models use the limit assumptions of no mass diffusion in the solid (Gulliver-Scheil [l]) or complete diffusion in the solid (equilibrium lever rule) in a fixed and space. Recently, however, more sophisticated microsegregation models that account for finite mass diffusion and coarsening of the arm space have been developed [2-19]. In this paper governing equations for a general microsegregation model for a multi-component alloy in a coarsening and spacing _are introduced. From these general equations various models for a binary system are developed and tested"

Jan 1, 2000

By George P. Demopoulos

n this study we have sought to highlight the critical linkage between individual reaction kinetic parameters (usually determined in small bench scale experiments) and large continuous reactor performance by focusing on the industrially significant zinc pressure leach process. To this end a comprehensive mathematical model previously developed for the description of this process was employed. In this paper we have examined in particular how small variations in key kinetic parameters impact on the autoclave&apos;s performance, i.e. attainment of autogenous steady-state temperature, zinc conversion and solution chemistry. The reaction parameters studied were: (i) stoichiometry of the marmatite leaching reaction; (ii) the activation energy of the same reaction, E,; (iii) the rate constant of the ferrous to ferric oxidation reaction, k,; and (iv) the apparent equilibrium constant for ferric precipitation, K,. This parameter sensitivity analysis was done under no oxygen mass transfer control limitations. Model predictions were found to be more sensitive to the kinetic parameters under certain conditions than others. The most dramatic finding was the one related to the small amount of sulfate produced during marmatite leaching. In connection to this it was found that the small percentage (< 5 %) of sulfate produced enhances the autothermal operational stability of the autoclave. The need for accurate kinetic parameter determination under conditions similar to those encountered in industrial zinc pressure leaching was demonstrated.

Jan 1, 1999

By Katri Avarmaa

Aluminum and copper are large volume metals in electronic appliances, while tin and indium exist as common minor elements. All of these non-ferrous metals are aimed to be separated and recycled from the end-of-life electronics into non-ferrous scrap fraction(s), and further through pyrometallurgical and/or hydrometallurgical processes to pure metals. Depending on the mechanical pre-treatment processes, aluminum and copper liberation from each other varies. This study focuses on the influence of alumina on indium and tin distributions between copper alloy and iron silicate slags with 0, 9 and ∼16 wt% of Al2O3. The experiments were executed with an equilibration-quenching-EPMA technique in an oxygen pressure range of 10−10–10−5 atm at 1300 °C. The metal-slag distribution coefficient of indium remains constant as a function of alumina in slag, while that of tin increases. Therefore, aluminum in feed or alumina addition to the slag improves the recovery of tin into copper. Nevertheless, oxygen pressure has clearly more significant influence on the behavior of both the metals in the smelting conditions.

By Zhang Chuanfu, Tan Pengfu

"A thermodynamic model is developed to simulate nickel flash smelting process. In the nickel flash furnace, oxidation of concentrate occurs at one end, and reduction of slag occurs at the other. The model makes use two zones, namely the reaction shaft/settler zone and the appendage zone and accounts for 6 phases (matte, slag, silica, magnetite, Cu-Ni alloy and gaseous phase), 13 elements (Ni, Co, Cu, Fe, S, 0, N, C, H, Si, Al, Mg and Ca) and 33 chemical components in nickel flash smelting system. The compositions of matte, slag and gaseous phases in equilibrium are calculated by using the data of free energies of formation and activity coefficients of components. Two nickel sulfide species are used to allow for the modeling of sulfur-deficient mattes. The model predictions are compared with the known industrail data from Kalgoorlie Nickel Smelter, and excellent agreement is obtained. The model can be a very useful tool for monitoring and optimizing the actual industrial operations of nickel smelting process. The distribution behaviors of Ni, Co, Cu, Fe, S and 0 in the nickel smelting furnace depend on the process parameters such as smelting temperature, volumes of air, the content of the elements~ charge and oil.1. IntroductionThe nickel flash smelting furnace essentially consists of a reaction shaft where nickel sulfide concentrate is partially oxidized with air, a settle zone where matte and slag are allowed to separate, and a slag cleaning end where coke is added to provide for the reduction of the oxidized nickel from slag, and electrodes are used to provide heat.The theoretical model to consider a mass balance for copper flash furnace is developed by S. Goto and R. Shimpo[1][2J. However, this can not be true for nickel flash furnace as a whole since oxidation of concentrate occurs at one end (in the reaction shaft/settler), and reduction of slag occurs at the other (in the appendage). Despite these limitations, an acceptable pseudo-thermodynamic description of the furnace can be achieved using essentially two zones, namely the reaction shaft/settler zone and the appendage zone. Compositions of gas, slag and matte in two zones are calculated."

Jan 1, 1998

By Jilai Xue, Jun Zhu, Baisong Li

"TiB2-C/C Function Gradient Materials (FGM) is used in cathode materials to improve aluminum wettability and melt penetration in aluminum electrolysis. In this investigation, FGM was tested for use as part of the cathode materials, where a 10 mm thick TiB2-rich layer was on the top as an Al-wettable surface, the TiB2-C layers in the middle as a gradient layer and the carbon on the bottom as a base. Electrical resistances ofFGM were determined in the temperature range of25- 9600C in argon atmosphere. The results show that the present of TiB2-C gradient layer can reduce the open porosity and the electrical resistance of the cathodes materials at elevated temperatures. The cathode samples after aluminum electrolysis usually demonstrates an increase in electrical resistance, but the application of FGM layer can compensate such an increase for certain extend due to less variation in porosity and lower the level of melts penetration.IntroductionCarbon is still used for aluminum reduction cathodes dominantly, but it has a poor wetting properties by liquid aluminum and the anode-cathode distance has to be kept about 4-5cm with an additional 1.3-2.0 V voltage drop [l]. TiB2 has better wettability by liquid aluminum with higher electrical conductivity and stronger chemical resistance to the electrolyte attack. And the wettability ofTiB2-C composites cathode on liquid aluminum can be also improved, while liquid aluminum can completely wet the cathode surface ifTiB2 content exceeds 27% [2-4]. However, during the process of TiB2-C composites cathodes preparation and aluminum electrolysis, the deformation by temperature variation or sodium penetration are great disparity between TiB2 and carbon due to their physical properties difference. This will accelerate the cathodes cracking and deterioration."

Jan 1, 2013

By Zhucheng Huang, Ronghai ZHONG, Tao Jiang, Jun ZOU

The method of reduction roasting and magnetic separation of low-grade, micro- fine disseminated refractory iron ore following granulation with coal produced unexpected success. Pellets of iron ore with diameter between 3 and 8mm were granulated with coal, bentonite and water. The raw pellets and reduction products were analyzed by scanning electron microscopy and x-ray diffraction. Results show uniformly distributed coal powders inside the pellets improved the kinetics of the reduction process and accelerated the reduction rate. Reduction time was higher at temperatures below 890℃, which resulted in the formation of substantial amounts of fayalite. When temperature was increased, micro- fine hematite was then quickly reduced to iron metal and the amount of fayalite decreased sharply. When pellets were reduced at 950℃ for 25min, reduction products with 56.73% metallization rate were obtained. After grinding and magnetic separation, a concentrate with 72.18% Fetot was obtained.

Jan 1, 2015

By N. Ono, H. Fujiwara, S. Otsuka-Yao-Matsuo, T. Omata

"The electrical conductivity and the oxygen release and uptake of sintered indium tin oxide (ITO) upon heating and cooling under the condition that P(O2)/P*=4.9X10-4 (P* = atmospheric pressure), :when P(O2) was approximately 50Pa, were simultaneously measured by using a closed-system oxygen-gas analyzer. A large increasing in -the electrical conductivity - upon the· oxygen release detected in 1130<T<1273K was observed. Quantitative relationship between the number of oxygen atom released from ITO and the conduction electron density in ITO was studied. The release of one oxygen atom agreed with the generation of two conduction electrons, i.e., the efficiency-carrier-generation for the oxygen release from the ITO was almost one. The oxygen atom released must be originally at the quasi-anion site in the C-type rare-earth lattice, i.e., the 16c site in the space group of Ia3, as an interstitial excess oxygen, Oi"". It was concluded that the mechanism of conduction carrier generation and compensation upon SnO2 doping into In2O3 can be expressed by the defect equation, 2SnO2-2Sn1n +2(1-z)e'+zOi""+3O0 x+(l-z)/2O2, and that the oxygen release bringing the increase in the electrical · conductivity can be expressed by the equation, Oi""-1/2O2+2e'.IntroductionThin films of SnO2-doped In2O 3 (generally designated as ITO, for indium tin oxide), which have high optical transparency for visible light and high electrical conductivity, have been used as transparent electrodes for liquid crystal and electrochromic displays. It is well known that the electrical conductivity of ITO depends on the content of SnOi-dopant and oxygen. However, a reliable relationship between electrical conductivity and the absolute oxygen content in ITO has yet to be reported. The elucidation of such a relationship is one of the important clues for realizing extremely highly conductive ITO electrodes."

Jan 1, 2000

By D. Silva-Galvan, R. D. Morales, S. Gonzáelez-López, A. Romero-Serrano, G. Plascencia-Barrera, F. Chavez-Alcala

This work is focussed on lead decopperising by two techniques: conventional top addition of sulfur and injection of sulfur powder. It is found that the first method proceeds under equilibrium conditions and the second one depends on kinetic considerations. Experiments were carried out using 15 kg lead baths at two temperatures, 340°C and 380°C. The carrying gas used for the injection trials was nitrogen at flow rates of 6.3 and 18.6 L min- 1• The results show that 'decopperising process is more efficient at temperatures close to the melting point of lead for the sulfur top addition process, whereas high temperatures produce better copper removal for the injection of sulfur powder. Besides, the sulfur injection with the higher nitrogen flow rate (18.6 L min-1) produced higher decopperising rates. Thermodynamic and kinetic models are used to simulate this lead refining process.

Jan 1, 2000

By Gervais Soucy, François Quesnel, Pierre Hovington, Wen Zhu, Karim Zaghib, Jocelyn Veilleux

The properties of lithium titanates anodes in Li-ion batteries are highly dependent on their secondary constituents. While their main phase is usually constituted of Li4Ti5O12, significant quantity of lithium titanates compounds of various stoichiometry are often present, due to either the processing, usage or aging of the material. These may go underreported, as many of these spectrums overlap or display low signal in X-ray diffraction (XRD). Samples of nanosized lithium titanates synthetized by inductive plasma were characterized by XRD and scanning electron microscopy (SEM), as they provide a regular yet typical crystallite size and shape including multiple phases. A Rietveld refinement was developed to extract the composition of these samples. Mass balance through further annealing and differential scanning calorimetry (DSC) enthalpy measurements from phase transformations were also used as identification and validation techniques.

Jan 1, 2015