Thermal expansivity of geikielite and ilmenite utilizing in-situ synchrotron X-ray diffraction at high temperature

The unit-cell parameters and volumes of geikielite(MgTiO_(3))and ilmenite(FeTiO_(3))were investigated at high temperatures up to 700 K and ambient pressure,using in-situ angle-dispersive synchrotron X-ray diffraction.No phase transition was detected over the experimental temperature range.Using(Berman in J Petrol29:445-522,1988.10.1093/petrology/29.2.445)equations to fit the temperature-volume data,the volumetric thermal expansion coefficients at ambient conditions(α_(V0))of MgTiO_(3) and FeTiO_(3) were obtained as follows:2.55(6)×10^(-5)K^(-1)and 2.82(10)×10^(-5)K^(-1),respectively.We infer that the larger effective ionic radius of Fe^(2+)(Ⅵ)(0.78 A)than that of Mg^(2+)(Ⅵ)(0.72?)renders FeTiO_(3)has a larger volumetric thermal expansivity than MgTiO_(3).Simultaneously,the refined axial thermal expansion coefficients under ambient conditions areα_(a0)=0.74(3)×10^(-5)K^(-1)andα_(c0)=1.08(5)×10^(-5)K^(-1)for the aaxis and c-axis of MgTiO_(3),respectively,andα_(a0)=0.95(5)×10^(-5)K^(-1)andα_(c0)=0.92(12)×10^(-5)K^(-1)for the aaxis and c-axis of FeTiO_(3),respectively.The axial thermal expansivity of MgTiO_(3) is anisotropic,but that of FeTiO_(3) is nearly isotropic.We infer that the main reason for the different axial thermal expansivity between MgTiO_(3) and FeTiO_(3) is that the thermal expansion mode of the Mg-O bond in MgTiO_(3) is different from that of the Fe-O bonds in FeTiO_(3).

Effect of surface dissolution on flotation separation of fine ilmenite from titanaugite

The influence of surface dissolution on flotation separation of fine ilmenite from titanaugite was investigated through infrared spectroscopic （FT-IR） analysis and X-ray photoelectron spectroscopy （XPS） test. The results show that surface dissolution in weak acid solution is helpful to enlarge the floatability difference between ilmenite and titanaugite. In weak acidic solution, as sodium oleate mainly interacts with Fe which results in ilmenite flotation, and surface dissolution is beneficial to its oxidation, the floatability of ilmenite after surface dissolution is increased; meanwhile, sodium oleate interacts with Ca and Mg which results in titanangite flotation, and the quantities of Ca and Mg on the surface of titanautite are decreased due to the surface dissolution, so the floatability of titanaugite after surface dissolution is depressed. For an ilmenite ore obtained from Panzhihua with TiO2 grade of 8.41%, flotation after surface dissolution treatment could increase TiO2 grade of rough concentrate from 26.7% to 31.73 %.

Microwave drying characteristics and kinetics of ilmenite

The microwave drying of ilmenite was investigated.The effects of power levels and sample mass on drying characteristics of moisture content,drying rate,moisture ratio were studied,with microwave power ranging from 119 W to 700 W and sample mass from 5 g to 25 g.The drying processes were completed within 2-8 min at different conditions.The moisture content and drying rates are found to be dramatically affected by microwave power density.For all drying processes the prior microwave absorption of moisture produces an accelerating peak on the drying rate curves in the initial stage.For the sample mass of 25 g and power of 385 W,the drying kinetics were studied.The experimental results fit better to the Henderson-Pabis index model rather than the Page＇s semi-empirical model;the drying rate constant k is increased with the increase of microwave power and decrease of sample mass.

Microwave assisted grinding of ilmenite ore

The influence of microwave heating on the grinding of Panzhihua ilmenite ore was investigated. Factors that influence the processing are： the microwave exposure time, power density and sample mass. 40 g sample was microwave heated for 30 s with 1 kW of microwave power and followed by water quenching. SEM analysis indicated that intergranular fractures occurred between ores and gangues other than transgranular fractures after microwave treatment, which would liberate minerals from each other effectively. The subsequently magnetic separation trials provided evidence that the recovery rate increased from 44% for raw ore to 72% by microwave treatment.

Effect of temperature on dielectric property and microwave heating behavior of low grade Panzhihua ilmenite ore

The permittivity of low grade Panzhuhua ilmenite ore at 2.45 GHz in the temperatures from 20 ℃ up to 100 ℃ was measured using the technology of open-ended coaxial sensor combined with theoretical computation. The results show that both the real （ε′） and imaginary （ε′） part of complex permittivity （ε′-jε′） of the ilmenite significantly increase with temperature. The loss tangent （tanδ） is a quadratic function of temperature, and the penetration depth of ilmenite decreases with temperature increase from 20 ℃to 100 ℃ The increase of the sample temperature under microwave radiation displays a nonlinear relationship between the temperature （T） and microwave heating time （t）. The positive feedback interaction between complex permittivity and sample temperature amplifies the interaction between ilmenite and the microwave radiation. The optimum dimensions for uniform heat deposition vary from 10 cm to 5 cm （about two power penetration depths） in a sample being irradiated from both sides in a 2.45 GHz microwave field when temperature increases from room temperature to 100 ℃

Phase transitions, micro-morphology and its oxidation mechanism in oxidation of ilmenite (FeTiO_3) powder

Phase transitions, morphology changes, and oxidation mechanism of the ilmenite oxidation process were investigated. FeTi03 transforms to hematite and rutile when oxidation at 700-800 ℃, and pseudobrookite is formed when the oxidation temperature reaches 900 ℃. The initial ilmenite powder exhibits paramagnetism; however, after being oxidized at the intermediate temperature （800-850 ℃）, the oxidation product exhibits weak ferromagnetism. The oxidation mechanism was discussed. The microstructure observations show that a lot of micro-pores emerge on the surfaces of ilmenite particles at the intermediate temperature, which is deemed to be caoable ofenhancin~ the mass transfer ofoxgen during oxidation.

TiO_2 nanoparticles prepared by hydrochloric acid leaching of mechanically activated and carbothermic reduced ilmenite

A new combination method consisting of ball milling, carbothermic reduction and hydrochloric acid leaching was proposed for the preparation of nanosized synthetic rutile from natural ilmenite. The ball milling was employed to grind ilmenite into small particles. The carbothermic reduction was carried out to yield a high titanium slag, which would be easily purified by subsequent leaching procedure. Factors affecting the hydrochloric acid process, namely the leaching time, temperature, and acid concentration, were studied. After leaching and calcining the milled and annealed mixture of FeTiO3/C under the optimal conditions, the TiO2 nanoparticles with size of 10-200 nm and purity〉98.0% were obtained.

Effects of mechanical activation and oxidation-reduction on hydrochloric acid leaching of Panxi ilmenite concentration

The effects of oxidation-reduction treatment and mechanical activation on the hydrochloric acid leaching performance of Panxi ilmenite concentration were investigated.The results show that both of oxidation-reduction treatment and mechanical activation significantly accelerate the extraction of Fe,Ca and Mg from Panxi ilmenite concentration;however,the CaO and MgO contents of the calcined residues obtained from oxidized-reduced ilmenite concentration are higher than the standard values required by chlorination process.The Ca and Mg in oxidized-reduced ilmenite concentration can be leached much faster after mechanical activation,yielding a synthetic rutile which meets the requirements of chlorination process containing 90.50% TiO2 and 1.37% total iron as well as combined CaO and MgO of 1.00%.The optimum oxidation and reduction conditions are as follows：oxidization at 900 ℃ in the presence of oxygen for 15 min and reduction at 750 ℃ by hydrogen for 30 min.

Effect of milling time on carbothermic reduction of ilmenite

A systematic investigation on the effect of milling time on carbothermic reduction of ilmenite was carried out by a combination of thermal analysis, X-ray diffraction（XRD）, scanning electron microscopy（SEM） and particle size analysis. It was shown that the graphite crystalline structure was easily destroyed along the（002） crystal plane during milling process. The particle size of ilmenite/graphite mixture was largely decreased and a fully mixed composite structure was obtained after milling for 4 h at high milling intensity. Milling exerts positive effect on the decreasing temperatures of ilmenite reduction and gradual deoxidizing of titanium oxides was completed.

Reductive kinetics of Panzhihua ilmenite with hydrogen

The hydrogen reduction of Panzhihua ilmenite concentrate in the temperature range of 900?1050 °C was systematicallyinvestigated by thermogravimetric analysis (TG), X-ray diffraction (XRD) and scanning electron microscopy (SEM) methods. It wasshown that the products of the Panzhihua ilmenite reduced at 900 °C were metallic iron and rutile. Above 1000 °C, ferrouspseudobrookite solid solution was generated. During the reduction process, element Mg gradually concentrated to form Mg-rich zonewhich can influence the metallization process. The reduction reaction proceeded topochemically and its related reduction kineticswere also discussed. The kinetics of the reduction indicated that the rate-controlling step was the diffusion process. The apparentactivation energy of the hydrogen reduction of Panzhihua ilmenite was calculated to be 117.56 kJ/mol, which was larger than that ofsynthetic ilmenite under the same reduction condition.

An in situ ATR-FTIR study of mixed collectors BHA/DDA adsorption in ilmenite-titanaugite flotation system

This paper researched the enhanced flotation separation performance of ilmenite and titanaugite using the mixed collector benzhydroxamic acid/dodecylamine(BHA/DDA).The interface assembly mechanism was mainly investigated through in situ attenuated total reflectance Fourier transform infrared(ATRFTIR)spectroscopy combined with the two-dimensional correlation spectroscopy(2D-COS)and X-ray photoelectron spectroscopy(XPS).It has been found that BHA/DDA mixed collectors successfully separate ilmenite from titanaugite at a molar ratio of 8:1.Zeta potential experiments suggested that,in the presence of mixed collector system,the BHA-DDA complex adsorbed on the ilmenite surface via the chemically adsorbed BHA and the electrostatically adsorbed DDA,however,the complex adsorbed on the surface of titanaugite unstably.According to in situ ATR-FTIR combined with 2D-COS and XPS results,the interface assembly mechanism of BHA/DDA is summarized as:the function group of BHA molecules first binds to the metal sites on minerals to form bidentate ligand,then DDA co-adsorbed with BHA on the surface of minerals through hydrogen bonding.DDA may change the adsorption modes of some BHA on the ilmenite surface from four-membered ring to five-membered ring,while the modes on the titanaugite surface is true opposite.Finally,recommended adsorption configurations of the BHA/DDA complex on the two mineral surfaces are proposed.

Phase transformation and reduction kinetics during the hydrogen reduction of ilmenite concentrate

The reduction of ilmenite concentrate by hydrogen gas was investigated in the temperature range of 500 to 1200℃. The microstructure and phase transition of the reduction products were studied by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, and optical microscopy （OM）. It was found that the weight loss and iron metallization rate increased with the increase of reduction temperature and reaction time. The iron metallization rate could reach 87.5% when the sample was reduced at 1150℃ for 80 min. The final phase constituents mainly consist of Fe, M305 solid solution phase （M=Mg, Ti, and Fe）, and few titanium oxide. Microstructure analysis shows that the surfaces of the reduction products have many holes and cracks and the reactions take place from the exterior of the grain to its interior. The kinetics of reduction indicates that the rate-controlling step is diffusion process control with the activation energy of 89 kJ.mo1-1.

Mossbauer Spectrum Study on Hydrogen Reduction of Preoxidized Ilmenite

Reduction behavior of preoxidized synthetic ilmenite was studied by means of Mossbauer spectra. In the course of reduction, iron component in the samples is reduced in stepwise: Fe 3+ →Fe 2+ →Fe 0, and some intermediate compounds, such as Fe 3O 4, Fe 2TiO 4 etc . and their solid solution may be generated besides Fe 2O 3 and FeTiO 3. If the reduction temperature is higher than 1173 K, the metallization needs only half time of the case when the temperature is lower than 1073 K.

Beneficiation of Titanium Oxides From Ilmenite by Self-Reduction of Coal Bearing Pellets

The study on the beneficiation of titanium oxides from Panzhihua ilmenites by reduction of coal bearing pellets was carried out. The iron oxides in pellets were efficiently reduced to metal iron, and titanium oxide slag beneficiated was separated from metal iron. The effect of temperature, flux and coal blending ratio on the reduction and separation was investigated, and rational parameters were determined. A new process for the beneficiation of titanium oxides by rotary hearth furnace （RHF） was proposed.

Reagent types and action mechanisms in ilmenite flotation:A review

Ilmenite is an essential mineral for the extraction of titanium.Conventional physical separation methods have difficulty recovering fine ilmenite,and dressing plants have begun applying flotation to recover ilmenite.The interaction of reagent groups with Ti and Fe sites on the ilmenite surface dramatically influences the ilmenite flotation.However,the investigation on Fe sites has received more attention because the activity of Ti is lower than that of Fe.For the activators on ilmenite flotation,most are metal ions but typically lead ions.The metal ions of activators promote ilmenite flotation by increasing the active sites on the ilmenite surface.Combined reagents have a better selective separation of ilmenite than single reagents due to their synergistic effect.Combining the lead ion(Pb^(2+))and the benzyl hydroxamic acid(BHA)into a Pb-BHA complex has a marked effect on ilmenite flotation,which puts forward a new idea of developing combined reagents for ilmenite flotation.This review considers reagent types and action mechanisms in ilmenite flotation.On the basis of the analysis of previous research,a brief future outlook of reagent types and action mechanisms in ilmenite flotation is also proposed in this study.

Removal of iron from ilmenite by KOH leaching-oxalate leaching method

Oxalic acid was used for the removal of iron from the intermediates of ilmenite leached by KOH liquor. Various parameters, such as pH, temperature, initial oxalate concentration, and illumination were investigated. Meanwhile, it was found that orthorhombic crystal Ti2O2（OH）2（C2O4）-H2O formed as the leaching proceeded. Scanning electronic microscope （SEM） images implied that the formation of Ti2O2（OH）2（C2O4）.H2O with good crystallinity proceeded through three stages. Calcining Ti2O2（OH）2（C2O4）·H2O, anatase （350℃） or mtile （550℃） type TiO2 was obtained, respectively. Element analysis found that the calcined product contained 94.9% TiO2 and 2.5% iron oxide, but only about 1600 ppm dissolvable iron oxide was left, which indicates that oxalic acid was comparatively effective on iron oxide removal from the intermediates. Finally, an improved route was proposed for the upgrading of ilmenite into mtile.

Comparison of wear behaviour of LM13 Al−Si alloy based composites reinforced with synthetic(B_(4)C)and natural(ilmenite)ceramic particles

Dry sliding wear behaviour of stir-cast aluminium matrix composites(AMCs)containing LM13 alloy as matrix and ceramic particles as reinforcement was investigated.Two different ceramic particle reinforcements were used separately:synthetic ceramic particles(B_(4)C),and natural ceramic particles(ilmenite).Optical micrographs showed uniform dispersion of reinforced particles in the matrix material.Reinforced particles refined the grain size of eutectic silicon and changed its morphology to globular type.B_(4)C reinforced composites(BRCs)showed maximum improvement in hardness of AMCs.Ilmenite reinforced composites(IRCs)showed maximum reduction in coefficient of friction values due to strong matrix−reinforcement interfacial bonding caused by the formation of interfacial compounds.Dry sliding wear behaviour of composites was significantly improved as compared to base alloy.The low density and high hardness of B_(4)C particles resulted in high dislocation density around filler particles in BRCs.On the other hand,the low thermal conductivity of ilmenite particles resulted in early oxidation and formation of a tribo-layer on surface of IRCs.So,both types of reinforcements led to the improvement in wear properties of AMCs,though the mechanisms involved were very different.Thus,the low-cost ilmenite particles can be used as alternative fillers to the high-cost B_(4)C particles for processing of wear resistant composites.

MICROWAVE-ASSISTED CARBOTHERMIC REDUCTION OF ILMENITE

The microwave-assisted carbothermic reduction of ilmenite was investigated by thermogravimetric analysis under argon atmosphere. A comparison between microwave assisted reduction and the conventional one was made. It was demonstrated that the instantaneously volumetric heating of microwaves could significantly enhance the overall reduction process. By microwave application, the reduction could take place at much lower temperatures and the activation energy for the process could be lowered.The mechanism of the reduction was discussed according to the experimental data.

Effect of Temperature on Carbothermic Reduction of Ilmenite

The reduction of ilmenite (FeTiO_3) has been studied extensively. Temperature for the carbothermic reduction of ilmenite ranges from 900 ℃ to 1 400 ℃, and the reduction degree of Panzhihua ilmenite increases with increasing temperature. X-ray diffraction analysis and SEM analysis were used to identify the phase before and after reduction, and to identify the morphology of reduced samples respectively. It is found that the reaction initiates at about 860 ℃. The reaction rate varies with temperature simultaneously. Impurities in Panzhihua ilmenite decrease the reduction degree. Magnesium and calcium oxide-rich zone is formed preventing complete reduction of Fe 2+. In general, the reaction products are iron, Ti_3O_5 and carbon.

Direct carbothermic reduction of ilmenite concentrates by adding high dosage of Na_(2)CO_(3) in microwave field

A clean and efficient route for the utilization of ilmenite concentrates was proposed by direct carbothermic reduction in microwave field.High dosage of Na_(2)CO_(3),which can be recycled,was added to accelerate the reduction reaction of ilmenite concentrates.After microwave heating in the temperature range of 1073−1123 K for 20 min,the main products were Na_(2)TiO_(3) and metallic Fe with the metallization ratios being as high as 92.67%−93.21%.The reduction products were processed by water leaching,ball-milling in CO2 atmosphere and magnetic separation in turn.The final products after magnetic separation were Fe-rich materials and Ti-rich materials(90.04 wt.%TiO2),which can be used to produce iron and TiCl4 or TiO2.The optimized heating temperature was 1123 K in terms of metallization ratios,magnetic separation and caking property of the reduction products.Besides,the reduction mechanism of ilmenite concentrates with the addition of Na_(2)CO_(3) in microwave field was also proposed.