Search Documents

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 O. G. Rivera, R. D. Moser, P. G. Allison, W. R. Whittington, P. Rivera-Soto, Z. McClelland, D. Francis

This research examined the evolving microstructure of quasi-static and dynamically loaded fully annealed metastable 301 austenitic stainless steel (SS). Experiments were performed to an interrupted strain value of 20% and to failure using a tension Kolsky bar (1000/s) and an electromechanical load frame (0.001/s). Electron Backscatter Diffraction (EBSD) identified the microstructural evolution from the as-received condition to the 20% strain level for the high and low rate interrupted samples. This material achieved over 60% elongation to failure with increasing strength as strain rate increased, as expected. Fractography analysis using SEM showed particles in the microstructure and a ductile failure mode. The 301 SS exhibited a greater amount of phase transformation from parent austenite to -martensite at the dynamic strain rate when compared to the quasi-static strain rate during the interrupted experiments. This result is indicative of the increased propensity for austenite to -martensite phase transformations at the high strain rate.

Jan 1, 2016

By Dominic T. Jordan, Quinn G. Reynolds, Christopher J. Hockaday, Ian J. Barker

A direct-current (DC) plasma arc furnace is a type of electric furnace used for metallurgical operations. The successful operation of DC furnaces depends to a large extent on gaining a fundamental understanding of the arc phenomenon itself, and ensuring its presence in the furnace at all times. A method for detection of the presence of the arc in a DC circuit is presented, along with discussion of why this may be of value for certain modes of furnace operation such as brush-arc. The theoretical development of the method is presented along with supporting experimental work conducted on large-scale pilot-plant facilities.

Jan 1, 2014

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 Hans Jürgen Maier, Gregory Gerstein, Florian Nürnberger

Microstructural analysis to support the development of material models provides valuable information to design complex forming operations. Damage models such as e.g. by Gurson consider spherical voids only. However, investigations of bcc steels by scanning electron microscopy reveal that voids exhibit an ellipsoidal shape with progressing deformation. The material’s weakening in the Gurson model is taken into account by the void volume fraction. Therefore, a three-dimensional characterization of the void shape offers important data for modelling. Thus, information on the anisotropy of the process of void evolution and accordingly, about the anisotropy of the deformation process is provided. Application of the information regarding the void shape anisotropy within the Gurson model is discussed.

Jan 1, 2016

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 Jiang Diao, Yong Qiao, Xuan Liu, Tao Zhang, Bing Xie

Adding CaO into the vanadium extraction converter is an effective way to decrease the dephosphorization burden in subsequent steelmaking process. The crystallisation process of spinel is one of the most decisive factors in the subsequent extraction. The theoretical calculation results show that the temperature of the peak total crystallization rate will decrease 5K with basicity increasing 0.1. The relation between cooling conditions and grain size of spinels is also discussed. It is found that low cooling rate and high basicity benefit spinel crystal growth. And the non-isothermal crystallization kinetics results indicated that the restriction factors of spinel growth is that solid crystals accept new components from liquid-solid interfacial. While the sample was cooled down to 1250 (1523K) at cooling rate of 5K/min, the crystal growth is consistent with Ostwald coarsening grew up law, and controlled by diffusion of particle.

Jan 1, 2016

By Shabnam Sabah, Geoffrey Brooks

In oxygen steelmaking, splashing and droplet formation play a key role in the kinetics of the process. Though splashing has been studied by previous investigators, there is only limited understanding of how different cavity modes affect splashing. Therefore, a cold model study (at various lance heights and gas flow rates) has been carried out focusing on the issue of cavity modes and how it affects splashing phenomenon. Analysis using Fast Fourier Transform (FFT) was carried out on cavity oscillation that showed that frequency and amplitude of oscillation was highest in penetrating mode. Measurements of splashing over a range of conditions showed splashing greatly reduced when cavities went from splashing to penetrating mode. The results were validated and compared with plant data and previous model investigations.

Jan 1, 2014

By Fuqiang Zheng, Feng Chen, Wenting Duan, Yufeng Guo, Tao Jiang

High-quality titanium-rich material is of significance in the development of titanium industry as it is the main raw material to produce sponge titanium and titanium white using chloride process. Activation roasting of titanium slag with high Ca and Mg contents as adding H3PO4 followed by acid leaching was investigated to prepare titanium-rich material. The effects of H3PO4 dosage, roasting temperature and time, hydrochloric acid quantity, acid leaching temperature and time on TiO2 grade and removal of impurities were studied. The results show that after the finely ground titanium slag roasted with 8% H3PO4 at 1000 for 2h, most Mg impurities in anosovite solid solution structure were converted into simple acid–soluble compounds. The impurities such as Ca and Mg obviously decreased when the hydrochloric acid concentration was 20%, leaching at 100 °C for 2h, from which a titanium-rich material containing 82.56% TiO2 and 1.15% (CaO+MgO) was obtained.

Jan 1, 2016

By He Zhi-jun, Ning Zhe, Pang Qing-hai, Zhang Jun-hong, Zhan Wen-long

The effect of microwave irradiation on grinding property of coal was studied by using Hardgrove grindability index tester. Superior grindability of coal was obtained to varying extent after microwave irradiation treatment. The variation in microstructure of pulverized coal during microwave irradiation was observed by utilizing scanning electronic microscope (SEM). The results indicated that the different microwave absorbance of minerals and carbon matrix led to cracks on their interface, by which coal particles were further pulverized and therefore the granularity of coal powder was reduced. Due to the different formation process of various coals, bituminite and anthracite are very different in physical and chemical properties. According to the content of coal pulverization, it can found that microwave irradiation has a stronger pulverizing effect on bituminite in comparison to anthracite.

Jan 1, 2016

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 Hong Yong Sohn

A novel flash ironmaking technology is under development at the University of Utah under the support of U.S. Department of Energy (DOE) and American Iron and Steel Institute (AISI). The history of the development from the conception of the idea to the current status will be discussed. The flash ironmaking process produces iron directly from fine iron ore concentrates without requiring cokemaking and pelletization/sintering, which will enable the technology to significantly reduce energy consumption and carbon dioxide emissions compared with blast furnace ironmaking. Unlike other gas-based ironmaking processes, this technology will not suffer from the problems of solid sticking and fusion. Current work is focused on the method of supplying the energy required to maintain the necessary temperature, as an intermediate step to determine the scalability for larger, industrial-scale pilot trials.

Jan 1, 2014

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 Zhigang Zak Fang, Michael L. Free, Jaehun Cho, Syamantak Roy, Amarchand Sathyapalan

Leaching characteristics of impurity removal from the Upgraded Titania Slag (UGS) using hydrochloric and boric acids has been investigated. Specifically, this study has focused on removal of iron oxides from the UGS that has been reduced by hydrogen gas and magnesium at 750oC for 5 hours. Reduced UGS is mainly composed of titanium hydride and impurities like iron oxides, silicon oxide, aluminum oxide, and magnesium oxide. The concentration of hydrochloric and boric acids and the leaching temperature have been chosen as the prime variables to identify the optimum conditions and leaching characteristics for removal of iron oxides. It was observed that under the constraint that 1 wt % of titanium hydride loss is the maximum amount tolerable, 0.1M HCl with 1M boric acid and 90oC are the most effective parameters for iron removal from the reduced UGS. Also, the overall rate of reaction seems to follow interfacial reaction controlled kinetics. The calculated activation energy of the reaction is 73.90kJ/mol.

Jan 1, 2016

By Yong Zhao, Yan-hui Sun

Behaviors and evolutions of MgO·Al2O3 in non-oriented silicon steel during calcium treatment were investigated by thermodynamic calculations and high-temperature experiments. MgO·Al2O3 inclusions were the main type of inclusions before calcium treatment, which is also confirmed by the stability diagram of MgO/MgO·Al2O3/Al2O3 from thermodynamic calculations. After calcium treatment, the majority of original MgO·Al2O3 inclusions were mainly modified to CaO-MgO-Al2O3 system inclusions, this would be beneficial to improve castability and product quality of silicon steel. But there was no modification happening to some MgO·Al2O3 spinels which were directly surrounded by CaS inclusions. The content of Al2O3 occasionally existed a sudden increase besides a common decrease in the product layer of CaO·MgO·Al2O3. Then the evolution mechanisms of MgO·Al2O3 inclusions were proposed in present work. Thus, Al/Mg atom ratio had a significant influence on the modification of MgO·Al2O3 spinel.

Jan 1, 2016

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 Yotamu Stephen Rainford Hara, Animesh Jha

The investigation focuses on a low temperature recovery of Cu and Co from a 40 wt% SiO2-(30 wt%Fe,6 wt%Al)2O3-10wt% CaO-7wt%CuO-7wt%CoO slag over a temperature range of 1173K to 1323K. The alloy phases containing Cu-Co and Fe-Co alloy formed via the carbothermic reduction of oxides: MO + C = M + CO(g), where M represents metallic copper, cobalt or iron. In the direct reduction of oxides, the recovery of metallic phase was well below 90% at 1323K, due to the kinetic barrier which was analysed and attributed to oxygen and metal-ion transport in the slag. This barrier was overcome by adding CaSO4 and carbon, which yields a matte (MS) phase via MO + CaSO4 + 4C = MS + CaO + 4CO reaction. Lime thus produced in situ participates in metal oxide/metal sulphide reduction reactions, which are analysed with the help of X-ray powder diffraction, scanning electron microscopy, and thermogravimetric analysis.

Jan 1, 2014