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By Jian Li, P. Liu, R. Zhang and J. Lo

In the past decades, focused ion beam (FIB) has evolved into a powerful microscope that provides capabilities that no other microscopes can offer. The combination of high-resolution imaging and stress-free ion beam cross sectioning provides valuable microstructure information both at the specimen surface and beneath. FIB techniques are also the preferred method to prepare site-specific transmission electron microscope (TEM) specimens. CanmetMATERIALS owns a world-class microscopy facility, where advanced microscopy work provides strong supports to research programs that cover a wide range of subject areas. This paper is aimed to provide a few practical examples of FIB applications in microstructure characterizations that include cross-sectioning and imaging, serial sectioning, and advanced TEM specimen preparation in materials research at CanmetMATERIALS.

Jan 1, 2015

By Xiaojie Gao, Jingshe Li, Chengsong Liu, Haiyan Tang

In order to clarify the reaction between MnO-SiO2 oxides with low FeO content and Fe-Mn-Si alloy, two diffusion couples were produced by the new method using confocal scanning laser microscopy (CSLM). The interface of the alloy and oxide, content of Mn and Si in the alloy near the interface, size distribution and composition of the particles which precipitated in the alloy were observed and analyzed using the electron probe microanalysis (EPMA). Results show that though the FeO content in the oxides decrease to 1% which is lower than the equilibrium with the molten steel at 1873K, the diffusion of oxygen from oxide to alloy still exists during the heat treatment at 1473K and causes shorter Particle Precipitated Zone (PPZ) and Manganese Depleted Zone (MDZ) normally for the reduction of diffusion flux of oxygen.

Jan 1, 2015

By Fuming Wang, Lifu Hu, Changrong Li, Ruipeng Pang

The solidification structure of 430 ferritic stainless steel has been calculated in the solidification process by using 3D-CAFE model under the condition of water cooling. The calculated results consistent with those obtained from experiment. Under watercooling condition, the solidification structure consists of chilled layer, columnar grain zone, transition zone and equiaxed grain zone

Jan 1, 2015

By Xiao-hui Fan, Xu-ling Chen, Zhi-yuan Yu1, Guanghui Li, Min Gan, Yun-song Huang, Tao Jiang

Compared with the traditional de-NOx processes by cleaning the waste gas, a new approach for reducing the formation of NOx during sintering process is proposed. Since more than 90vol% of NOx comes from the fuel combustion, the influence of sintering coke breeze pretreated by CO(NH2)2 additive on the NOx emission is researched. As adding CO(NH2)2, the reduction agents (NHi) are generated during the pyrolysis of CO(NH2)2, which reinforce the NOx reduction, And the appropriate content of CO(NH2)2 is 1.0 mass% of coke breeze.

Jan 1, 2015

By Thenepalli Thriveni, Ch. Ramakrishna, Yujin Jegal, Ji Whan Ahn, Jyothi Rajesh Kumar

In alumina production or alumina refining, bauxite is converted to alumina (aluminium oxide) The rare-earth elements (REEs) are a group of 17 chemically similar metallic elements (15 lanthanides, including scandium and yttrium). Rare earth elements play a key role in many industrial applications, petroleum refining, clean energy, automobile, electronics, and defense applications. These rare earths are essential to the success of green technologies. China today controls more than 95 percent of the rare-earth supplies and nearly all rare-earth refining and after 2009 year rare earths crisis raises due to China’s export restrictions and growing internal demand for rare earth elements. The extraction of gallium and yttrium from Korean red mud (KC red mud) by selective acid leaching was explored. The recovery of gallium and yttrium from a leach solution of the Korean red mud using solvent extraction was studied. A number of extractants were investigated for the extraction of those mentioned two rare earth elements and also we proposed a flow sheet of rare earth elements respectively. The toxic heavy metals presented in KC red mud were removed by CO2 stabilization.

Jan 1, 2015

By Warren J. Bruckard, Mark I. Pownceby, Sazzad Ahmad, M. Akbar Rhamdhani

Rutile is the preferred feedstock for producing high-grade TiO2 pigment but due to decreasing resources, alternative materials such as ilmenite is now used to produce a synthetic rutile (SR) feedstock. This requires removal of impurities (e.g. Fe, Mg, Mn) which, for a primary ilmenite is straightforward process. Processing of weathered ilmenite however, is complex, especially when chrome-bearing impurities are present since minor chromium downgrades the SR market value as it imparts color to the final TiO2 pigment, Chrome-bearing spinels are a problem in weathered ilmenites from the Murray Basin, Australia as their physical and chemical properties overlap with ilmenite making separation difficult. In this paper, different sulfidation process routes for weathered ilmenites are analyzed for their applicability to Murray Basin deposits as a mean of remove chrome spinel impurities. Thermodynamic and experimental studies indicated that selective sulfidation of chrome-bearing spinel can be achieved under controlled pO2 and pS2 processing conditions thereby making them amenable to separation.

Jan 1, 2015

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

By Hans Jürgen Maier, Hans-Bernward Besserer, Gregory Gerstein, Florian Nürnberger

The formation and development of voids in both the single-phase ferritic steel DC04 and the dual-phase ferritic-martensitic steel DP600 are discussed. Various mechanisms and kinetics of void formation are considered regarding the influence of dislocation glide, precipitates and other parameters. Different characteristic locations in the microstructure are investigated at which strain concentrations during plastic deformation can occur and cause the formation of voids and microcracks. For the specimen preparation ion slope cutting is applied. Voids and cracks revealing ductile damage are analyzed by Scanning Electron Microscopy (SEM). Stress concentrations in consequence of plastic deformation could be shown by extinction contours on images recorded by Transmission Electron Microscopy (TEM).

Jan 1, 2015

By Duclerc Fernandes Parra, Washington Luiz Oliani, Christiano Gianesi Bastos Andrade, Ademar Benevolo Lugão, Danilo Marin Fermino, Francisco R. Valenzuela Diaz

This work concerns the study of the effect of discarded bond paper on the mechanical behavior of polypropylene/organophilic clay nanocomposites. A brown polycationic bentonite from the state of Paraíba, Brazil, was treated with sodium carbonate to transform it into a bentonite that swells in water and then treated with hexadecyltrimethylammonium ammonium chloride to transform it into a bentonite that swells in organic liquids. Polypropylene with 3 % polypropylene graft compatibilizer (PP-g-AM) was mixed with 1 % and 2 % by weight of discarded bond paper and with 1% and 2% by weight of organophilic clay using a twin-screw extruder. The specimens were prepared by the injection process. The clay as received and after organophilization was characterized by XRD, SEM, and capacity of swelling in water and in organic solvents. The nanocomposite specimens were characterized by XRD and thermal analysis. The mechanical behavior of the injected specimens was evaluated by strength, flexural and impact tests. The nanocomposites showed improved mechanical properties compared with the polymer without filler.

Jan 1, 2015

By Jie Li, Shu Yang, Zhongliang Tian, Xun Hu, Yanqing Lai, Shaolong Ye

The electrolyte with high solubility for Sc2O3 is very important to realize the preparation of Al-Sc master alloy by the molten salt electrolysis. The solubility of Sc2O3 in K3AlF6- Na3AlF6-AlF3 melts is determined with an isothermal saturation method. The effects of KR (ratio of K3AlF6 to K3AlF6+Na3AlF6), the concentration of Al2O3 and the temperature on the solubility of Sc2O3 are also investigated. The results indicate that the solubility of Sc2O3 in K3AlF6-Na3AlF6-AlF3 melts increases and then decreases with KR increasing. The solubility of Sc2O3 is 8.698 wt.% in (K3AlF6-Na3AlF6)(KR25%)-18 wt.%AlF3 melts at 940℃. The effect of temperature on the solubility is little, and the values are 8.575 wt.% and 8.762 wt.% respectively when the temperatures are 930℃ and 960℃. The solubility decreases from 8.809 wt.% to 7.058 wt.% as the concentration of Al2O3 increases from 1.5 wt.% to 5.0 wt.% at 950℃.

Jan 1, 2015

By Halvor Dalaker, Alain Marc Ferber, Thor Anders Aarhaug, Pål Tetlie

Off-gas monitoring of experimental reactors give little information about intermediate reaction products and reflect chemical equilibria at reduced gas temperatures. A reactor design with optical access was designed and tested in order to be able to qualify and quantify gaseous species from their emission spectra. By use of a sequence of sapphire, UV fused silica and IR transparent sapphire and CaF2 windows and lenses optical access to a hot, maximum 1800 °C, reaction zone was gained. A cooled area behind the reaction zone was used as a background in order to avoid signal saturation from reactor walls. In addition to molecular emission spectra, atomic emission lines are used to characterize stable gas constituents and radicals. The setup has been designed for the study of methane dehydrogenation experiments in order to investigate the carbon activity of reduction of oxide with methane, but has also been used to monitor gaseous silicon suboxide.

Jan 1, 2015

By Xu Zhang, Xuewei Lv, Guibao Qiu

Slag foaming phenomenon is of vital importance to the mass and energy transfer in metallurgical processes. A considerable extensively studies carried out via out-gas in the past cannot simulate well the foaming phenomenon formed in the blast furnace where high TiO2 iron ore is used. A gas reaction was designed in the water-glycerol system to simulate the inner-gas system. This study investigated the influences of solution viscosity, particle concentration and particle size on foaming caused by endogenetic gas. The results show that the foaming height decreases with the increase of solution viscosity, which means reduced foaming ability, more difficult foaming elimination process and prolonged time for natural defoaming. With increasing the solid particle content, the foam height presents a trend which increases firstly and then decreases. Under a certain solid particle content, foaming height decreases with the increase of solid particle size, indicating a weak foaming ability.

Jan 1, 2015

By Yuanbo Zhang, Zhixiong You, FENG ZHOU, Guanghui Li, Zhengwei Yu, Zhiwei Peng

Reduction disintegration of sinter significantly affects the coke consumption and productivity of blast furnace smelting. As we know, the reduction disintegration index (RDI+3.15) of sinter obtained from titanomagnetite concentrate is relatively worse than those from ordinary iron ores. In this study, the effect of sintering parameters, mainly involving coke breeze dosage and basicity on sintering indexes was investigated using titanomagnetite concentrate as raw material in an experimental-scale pot. Subsequently, RDI+3.15 of the sinter was detected according to the Chinese standard of GB/T13242-91. The results show that RDI+3.15 rises with the increase of coke breeze dosage, while it decreases with increasing basicity from 0.5 to 2.0 and then increases in the basicity range of 2.0-3.0. Finally, the microstructure of sinter before and after reduction was studied. And the mechanism of reduction disintegration was preliminary revealed by analyzing the morphologies and distributions of minerals in the sinter.

Jan 1, 2015

By Cui Wang, Bing Dai, Haibin Zuo, Jianliang Zhang

The damage mechanism of ductile cast iron cooling stave applied to No.4 blast furnace of Guofeng steel was analyzed through damage investigation in details, the damage causes: hightemperature gas flow erosion, wear of burden, high-temperature ablation, carburizing damage, improper operation on blast furnace, etc. were given out both in macroscopic and microscopic views. It can be obtained from metallographic diagrams that the diameter of graphite nodules increases, the number per unit area reduces, and roundness declines, successively, from cold to hot surface, which are not conducive to stave longevity. In summary, the material for staves manufacture should be better in comprehensive mechanical properties to prolong the service life, thus making blast furnace long campaign.

Jan 1, 2015

By Jiao Li, WenhuiMa, KuixianWei, YongnianDai, Cong Zhang

The paper studied the diffusion process of nitrogen and characteristic distribution of iron impurities in the bottom of cast crystalline silicon ingot along the direction of crystal growth. According to the dynamics analysis of the decomposition of Si3N4 coating, the diffusion process of nitrogen into multicrystalline silicon ingot during casting process should be divided into three steps. The diffusion length of nitrogen in multicrystalline silicon ingot is 700 μm. The results of EDS analysis indicate that the distribution characteristic of iron in multicrystalline silicon ingot is concerned with the diffusion process of nitrogen in this length. Based on the above research results, the distribution model of iron in casting multicrystalline silicon ingot was established and verified by the experimental results.

Jan 1, 2015

By Yong-ming Chen, Chao-bo Tang, Yun Li, Long-gang Ye, Sheng-hai Yang, Hao-tian Xue

In order to achieve high recovery of Cu and Co during cobalt-bearing copper sulphide ore smelting process, reducing agent (coke) and sulphidizing agent (pyrite) were added into molten smelter slag for reducing-sulphidizing smelting to product Cu-Co matte. Effects of reductive atmosphere, pyrite dosage, smelting temperature and smelting duration on Cu, Co, Fe distribution behaviours were investigated. The results show that the distributions of Cu and Co are mainly enriched in Cu-Co matte, and the distribution ratio, LCu and LCo, improve with increasing of coke amount or pyrite addition, whereas above 6 wt.% coke or 20 wt.% pyrite, Cu and Co tend to transfer from matte to cleaned slag. A properly high temperature(1300) and smelting duration(3h) are beneficial to the enhancement of the distribution ratio of valuable metals, and under the given set of conditions, LCu > LCo generally. However, an undesired high Fe contents in matte limit further increase of LCu and LCo.

Jan 1, 2015

By Kexin Jiao, Huichang Song, Zhijia Zhang, Jianliang Zhang, Zhengjian Liu

A clear understanding of iron carburization reaction occurring between molten iron and carbonaceous materials is of great importance in blast furnace, and it is one of the hot spots that ironmaking workers pay close attention to. Although carburization rates between iron and coke have been studied, the factors directly controlling it have not been clearly identified. This study focused on the kinetics analysis of iron carburization reaction. Sulfur content was determined as having positive influence on graphite carburizing reaction rate in the range of 0.02% - 0.06%. The values of apparent activation energy calculated by the experiment are consistent with the existing literature, which in turn proved the reliability of the experimental data.

Jan 1, 2015

By M. GONZALES-FERNANDES M

Natural rubber/organophilic clay nanocomposites were prepared and characterized. A brown bentonite from Paraiba’s State, Brazil was modified with a sodium salt and treated with quaternary ammonium salt hexadecyltrimethyl ammonium chloride. The clay in its natural state, after cation exchange with sodium and after organophilization was characterized by XRD, IR, SEM, thermal analysis. Nanocomposite samples were prepared containing 10 resin percent of organophilic clay. The vulcanized samples were analyzed by XRD, SEM. The nanocomposites obtained showed improvement in their mechanical properties in comparison with samples without clay.

Jan 1, 2015

By Enrui Dai, Weibing Chen, Bin Yang, Wenhui Ma, Haisheng Fang, Hui Wang

LiMn0.8Fe0.2PO4/C composite was prepared by an improved solid-state method and the effect of calcination temperature on properties of the obtained materials was investigated. The results showed that increasing calcination temperature from 600 to 700 oC improved the performance of the LiMn0.8Fe0.2PO4/C due to enhanced crystallinity and increased conductivity, but further increase in calcination temperature to 800 oC led to degraded performance due to particle growth and decrease in porosity. Therefore, the LiMn0.8Fe0.2PO4/C composite prepared at 700 oC exhibited the best electrochemical performance, and could deliver a high capacity of 152 mAh g−1 at 0.1 C, 147 mAh g−1 at 1 C and 114 mAh g−1 at 10 C. In addition, the performance of the LiMn0.8Fe0.2PO4/C and LiMn0.8Fe0.19Mg0.01PO4/C was compared when they were obtained at the optimum calcination temperature.

Jan 1, 2015

By Yongqi Sun, Zuotai Zhang

Our study investigated the influence of P2O5 and B2O3 on the viscosity and crystallization behavior of Ti-bearing blast furnace (Ti-BF) slags for the purpose of Ti extraction. The investigation of the crystallization behaviors were carried out using a single hot thermocouple technique (SHTT) and the viscosity was obtained by rotating cylinder method. For the viscosity, the results showed that P2O5 substantially increased the slag viscosity. P2O5 is a network-forming oxide, which increased the degree of polymerization of slags and accordingly increased the slag viscosity. However, both of slag viscosity and apparent activation energy for viscous flow remarkably decreased with B2O3 addition. As a typical network forming oxide, B2O3 was introduced into the network and existed dominantly as 2-D structure, BO3 triangular, which caused a simpler structure and a decreasing slag viscosity. As for the crystallization behaviors of Ti-BF slags, both P2O5 and B2O3 enhanced the crystallization trend of rod-shape rutile and suppressed the crystallization trend of dendrite CaTiO3. Therefore the added P2O5 and B2O3 caused the primary phase change from CaTiO3 to rutile. Additionally, it was found that the rod-shape rutile showed a 1-D growth, whereas the dendrite CaTiO3 showed a 3-D growth style.

Jan 1, 2015