New process for treating boron-bearing iron ore by flash reduction coupled with magnetic separation

Boron is an important industrial raw material often sourced from minerals containing different compounds that cocrystallize,which makes it difficult to separate the mineral phases through conventional beneficiation.This study proposed a new treatment called flash reduction-melting separation(FRMS)for boron-bearing iron concentrates.In this method,the concentrates were first flash-reduced at the temperature under which the particles melt,and the slag and the reduced iron phases disengaged at the particle scale.Good reduc-tion and melting effects were achieved above 1550℃.The B_(2)O_(3) content in the separated slag was over 18wt%,and the B content in the iron was less than 0.03wt%.The proposed FRMS method was tested to investigate the effects of factors such as ore particle size and tem-perature on the reduction and melting steps with and without pre-reducing the raw concentrate.The mineral phase transformation and morphology evolution in the ore particles during FRMS were also comprehensively analyzed.

Preparation of ZrB_(2)-ZrO_(2)-SiC Composite Powder by Carbothermal Reduction from Zircon

Using zircon,boric acid and carbon black as starting materials,ZrB_(2)-ZrO_(2)-SiC composite powder was synthesized by calcining at 1500℃in flowing argon atmosphere.The effects of the soaking time(3,6 and 9 h)and the addition of additive AlF_(3)(0,0.5%,1.0%,1.5%,2.0%and 2.5%,by mass)on the phase composition and the microstructure of the synthesized products were investigated.The results show that:(1)ZrB_(2)-ZrO_(2)-SiC composite powder can be synthesized by carbothermal reduction at 1500℃in flowing argon atmosphere;ZrB_(2) and ZrO_(2) are granular-like,and SiC crystals are fiberous;(2)with the soaking time increasing,the amount of ZrB_(2) increases,the amounts of m-ZrO_(2) and SiC decrease,and the total amount of non-oxides ZrB_(2),SiC and ZrC gradually increases;the optimal soaking time is 3 h;(3)compared with the sample without AlF_(3),the sample with 0.5% AlF_(3) has decreased m-ZrO_(2)amount,noticeably increased ZrB_(2) amount but decreased SiC amount;however,when the addition of AlF_(3) increases from 0.5%to 2.5%,the m-ZrO_(2) amount increases,the ZrB_(2)amount decreases,and the SiC amount changes slightly;the optimum AlF_(3)addition is 0.5%.

Investigation of β-Ga_(2)O_(3) thick films grown on c-plane sapphire via carbothermal reduction

We investigated the influence of the growth temperature, O_(2) flow, molar ratio between Ga_(2)O_(3) powder and graphite powder on the structure and morphology of the films grown on the c-plane sapphire(0001) substrates by a carbothermal reduction method. Experimental results for the heteroepitaxial growth of β-Ga_(2)O_(3) illustrate that β-Ga_(2)O_(3) growth by the carbothermal reduction method can be controlled. The optimal result was obtained at a growth temperature of 1050 °C. The fastest growth rate of β-Ga_(2)O_(3) films was produced when the O_(2) flow was 20 sccm. To guarantee that β-Ga_(2)O_(3) films with both high-quality crystal and morphology properties, the ideal molar ratio between graphite powder and Ga_(2)O_(3) powder should be set at 10 : 1.

Preparation of TiC powders by carbothermal reduction method in vacuum

The preparation of fine TiC powders by carbothermal reduction of TiO2 in vacuum was investigated by XRD,SEM,XRF and laser particle sizer.Thermodynamic analysis indicates that it is easy to prepare TiC in vacuum and the formation sequence of products are Ti4O7（Magneli phase）,Ti3O5,Ti2O3,TiCxO1-x and TiC with the increase of reaction temperature.Experimental results demonstrate that TiC powders with single phase are obtained with molar ratio of TiO2 to C ranging from 1：3.2 to 1：6 at 1 550 ℃ for 4 h when the system pressure is 50 Pa,and TiC1.0 is gained when the molar ratio of TiO2 to C is 1：4 and 1：5.In addition,fine TiC1.0 powders（D50 equals 3.04 μm） with single phase and low impurities are obtained when the molar ratio of TiO2 to C is 1：4.SEM observation shows that uniform shape,low agglomeration,and loose structure are observed on the surface of block product.

Synthesis of Al_2OC Compound by Carbothermal Reduction Process with Boron Oxide Additive

The synthesis method of Al2OC by adding B2O3 was studied to modulate the traditional synthesis process.The mixtures of active carbon,alumina and boron oxide with different carbon contents were heated at 1 700 ℃ for 2 h in flowing argon atmosphere to get the Al2OC product.The results indicate that the addition of B203 promotes the formation of Al2OC,which is dependent on the addition of B2 O3,and the Al2 OC content in the products increases with the increase of carbon.By systematically exploring the ratio of active carbon,alumina and boron oxide,the best formulation and the corresponding reaction mechanism were determined.

Thermodynamics and kinetics of carbothermal reduction of zinc ferrite by microwave heating

The kinetics of carbon reduction of ZnFe2O4 in the temperature range of 550-950 °C was investigated in a microwave tank-type reactor. The mechanism of formation of ZnO and Fe3O4/FeO by the decomposition of ZnFe2O4 was detailed using the equilibrium calculations and thermodynamics analysis by HSC chemistry software 6.0. In addition, the effects of decomposition temperature, the C/ZnFe2O4 ratio, the particle size and the microwave power were assessed on the kinetics of decomposition. Zn recovery as high as 97.93%could be achieved at a decomposition temperature of 750 °C with C/ZnFe2O4 ratio of 1：3, particle size of 61-74 μm and microwave power of 1200 W. The kinetics of decomposition was tested with different kinetic models and carbon gasification control mechanism was identified to be the appropriate mechanism. The activation energy for the carbon gasification reaction was estimated to be 38.21 kJ/mol.

Modified carbothermal reduction method for synthesis of LiFePO_4/C composite

With LiAc-2H2O as Li precursor,pure olivine phase LiFePO4/C was synthesized at a relatively low temperature（650 ℃） and short sintering period（4 h） by molten salt carbothermal reduction method.Scanning electron micrograph shows that particle size of the product is about 1μm,smaller than that of the sample synthesized with Li2CO3 as Li precursor.Electrochemical measurements prove that LiFePO4/C obtained from LiAc-2H2O shows high capacity.The initial discharge capacities are 148 mA-h/g at 0.5C rate and 115 mA-h/g at 5C rate,respectively.After 50 cycles,the capacity retention ratios are 93% and 89% at 0.5C rate and 5C rate,respectively.

Mineralogy and carbothermal reduction behaviour of vanadium-bearing titaniferous magnetite ore in Eastern India

Vanadium-beaxing titaniferous magnetite bands hosted by Precambrian gabbro-norite-anorthositic rocks or their metamorphic equivalents were discovered in some parts of Eastern Indian Shield, containing 48%-49% Fe （total）, 10%-25% TiO2, and 0.3%-2.20% V2O5 by mass. Mineralogical and petrological study, composition, and characterization of the vanadium-bearing titaniferous magnetite ore were carried out by scanning electron microscopy-energy dispersive X-ray （SEM-EDX）, wave length X-ray florescence （WDXRF）, inductively coupled plasma-atomic emission spectroscopy （ICP-AES）, X-ray diffraction （XRD）, etc. Chemical beneficiation for valuable metals, such as Fe, Ti, andV, was performed by reduction roasting. The direct and indirect reduction were investigated by mixing the lump ore with solid activated charcoal in a closed reactor and purging the reducing gas mixture in standard reducibility index apparatus at different temperatures and time intervals. The reduction roasting parameters were optimized. Finally, the reduced samples were crushed and upgraded by magnetic separation. The results show that, the maximum mass fractions of magnetic and nonmagnetic parts achieved axe 69.36% and 30.64%, respectively, which contain 10.6% TiO2 and 0.84% V205 in the magnetic part and 36.5% TiO2 and 0.22% V205 in the nonmagnetic part.

Preparation of titanium oxycarbide from various titanium raw materials:Part I.Carbothermal reduction

Carbothermal reduction was performed at temperatures up to 1600°C for vanadium-bearing titanomagnetite,ilmenite concentrate,and high titania slag.The possibility of selective carbothermal reduction was discussed in detail from the viewpoint of thermodynamics,and also tested.The products were analyzed by X-ray diffraction,scanning electron microscopy,and chemical analysis.The results show that it is possible to reduce all iron oxide to metallic iron,and titania to oxycarbide（TiCxOy）,without the reduction of other oxides like silica and magnesia.

Carbothermic reduction characteristics of ludwigite and boron–iron magnetic separation

Ludwigite is a kind of complex iron ore containing boron, iron, and magnesium, and it is the most promising boron resource in China. Selective reduction of iron oxide is the key step for the comprehensive utilization of ludwigite. In the present work, the reduction mechanism of ludwigite was investigated. The thermogravimetry and differential scanning calorimetry analysis and isothermal reduction of ludwigite/coal composite pellet were performed. Ludwigite yielded a lower reduction starting temperature and a higher final reduction degree compared with the traditional iron concentrates. Higher specific surface area and more fine cracks might be the main reasons for the better reducibility of ludwigite. Reducing temperature highly affected the reaction fraction and microstructure of the reduced pellets, which are closely related to the separation degree of boron and iron. Increasing reducing temperature benefited the boron and iron magnetic separation. Optimum magnetic separation results could be obtained when the pellet was reduced at 1300°C. The separated boron-rich non-magnetic concentrate presented poor crystalline structure, and its extraction efficiency for boron reached 64.3%. The obtained experimental results can provide reference for the determination of the comprehensive utilization flow sheet of ludwigite.

Carbothermal reduction process of the Fe-Cr-O system

Understanding the reduction behaviors and characteristics of the end products of Fe-Cr-O systems is very important not only for maximizing the recovery of metals from stainless steel dust but also for the subsequent reuse in metallurgical process. The present work first predicted the possible products thermodynamically when FeCr204 was reduced by C. The reduction behaviors by graphite of three kinds of Fe-Cr-O systems, i.e., FeCr204, Fe203q-Cr203, and Feq-Cr203, were then investigated in 1350-1550℃. Further, the microstructures of final products and element distribution conditions were examined. The results suggest that, thermodynamically, the mass of products for the carbothermal reduction of FeCr204 is a strong function of temperature, and the initial carbon content is used. More Fe-Cr-C solution and less residual carbon content are obtained at higher temperatures and lower no：no ratios （the initial molar ratio of C to O in the sample）. Experimental data show that the sample amount tends to affect the reduction rate, and the residual carbon content strongly depends on nc：no. With regard to the phases present in products during the reaction process, metal carbides tend to form in the initial stage, whereas Fe-Cr-C solution forms when the degree of reduction is sufficiently high.

Carbothermal reduction-chlorination-disproportionation of alumina in vacuum

The carbothermal reduction-chlorination-disproportionation of alumina in vacuum was investigated by XRD and thermodynamic analysis. The experiments on alumina and graphite at 1643-1843 K in vacuum were carried out. The results demonstrate that AlCl3（g） reacts with Al2O（g） or Al（g） generated from the carbothermal reduction of alumina to form AlCl（g）, and the AlCl（g） disproportionates to aluminum and AlCl3（g） at a lower temperature and the reaction rate of AlCl（g） reaches 90% at 980 K and 100 Pa. The aluminum can absorb CO to catalyze its disproportionation to C and CO2, and react backward with CO to form Al4C3, Al2O3, C and CO2, resulting in the aluminum product containing C, Al4C3 and Al2O3. The impurities in the aluminum product decrease as the AlCl（g） disproportionation temperature decreases. AlCl3 condenses at a temperature approximated to the room temperature.

Production of magnesium during carbothermal reduction of magnesium oxide by differential condensation of magnesium and alkali vapours

Most of researchers believed that the developments on the condensation of magnesium produced by carbothermic reduction just concentrated on two process routes:the“quench”route and the“solvent”route.But this paper will briefly analyzes the major challenges in magnesium vapor condensation during the vacuum carbothermic reduction of calcined dolomite,on equipment upgrade,heat transfers alter,to achieve condensation control and production collection.Solutions are then proposed using theoretical calculations and experiment results.Comparative analysis of the experiment results shows that the burning and even explosion of condensation products during the vacuum carbothermic reduction of calcined dolomite are mainly due to the burning of crystallized powder magnesium,which results from the self-ignition of alkali metals.Finally,this paper proposes a multistage condensation solution to improve traditional vacuum condensation equipment.And result show that the condensation equipment can effectively mitigate the burning and loss during condensation,also the morphology of the condensation products clearly improved,the grain size increased,and the oxidation rate decreased.The potassium/sodium vapor and the magnesium vapor were separately condensed.

Effects of Technological Parameters on Carbothermal Reduction and Nitridation of Zircon

Carbothermal reduction and nitridation （CRN） of zircon （ ZrSiO4 ） permits obtaining diffbrent composites of oxides and nitrides such as ZrO2 -Si2N2O and ZrN - Si3N4. The effects tf technological parameters （ carbon source, reaction temperature, and carbon con.tent ） on the reaction rate and product phase composition of CRN of zircon were investigated by TGA and XRD. The resuhs show that： （1） carbon source is an important factor for a rapid reaction, and actiwtted carbon is chosen as the carbon source considering the expect products and reaction rate ; （ 2 ） reaction tetnperature has vital effect on reaction rate and product. In, case of carbon content above 20% , the zircon phase and m-ZrO2 phase decrease with increasing temperature, while the ZF7N8O4 phase increases firstly and then decreases, and the ZrN phase increases continually; （3） different carbon contents result in different reaction products. The higher the carbon content, the lower the starting temperature for the CRN of zircon.

Synthesis of titanium oxycarbonitride by carbothermal reduction and nitridation of ilmenite with recycling of polyethylene terephthalate (PET)

An innovative and sustainable carbothermal reduction and nitridation(CTRN) process of ilmenite(FeTiO_3) using a mixture of polyethylene terephthalate(PET) and coal as the primary reductant under an H_2–N_2 atmosphere was proposed. The use of PET as an alternative source of carbon not only enhances the porosity of the pellets but also results in the separation of Fe from titanium oxycarbonitride(TiOxCyNz) particles because of the differences in surface tension. The experiments were carried out at 1250°C for 3 h using four different PET contents ranging from 25wt% to 100wt% in the reductant. X-ray diffraction(XRD),scanning electron microscopy(SEM) in conjunction with energy-dispersive X-ray spectroscopy(EDX),and LECO elemental analysis were used to study the phases and microstructures of the reduced samples. In the case of 75wt% PET,iron distinctly separated from the synthesized Ti OxCyNz phase. With increasing PET content in the sample,the reduction and nitridation rates substantially increased. The synthesis of an oxycarbonitride with stoichiometry of TiO_(0.02)C_(0.13)N_(0.85) with minimal intermediate titanium sub-oxides was achieved. The results also showed that the iron particles formed from CTRN of FeTiO_3 exhibited a spherical morphology,which is conducive for Fe removal via the Becher process.

SYNTHESIS OF TiN BY MICROWAVE CARBOTHERMAL REDUCTION OF TiO_2

Titanium nitride powder was synthesized by microwave carbothermal reduction of titanium oxide. The mechanism and thermal dynamics of the reaction process were studied. The results show that the microwave carbothermal reduction technology has unique advantages over the conventional reduction methods. It can not only lower the reaction temperature, shorten the synthesis cycle, but also refine the product particles,as well as improving the reactivity of the powder.

Comparative evaluation of energy and resource consumption for vacuum carbothermal reduction and Pidgeon process used in magnesium production

With the fast development of the application of magnesium based alloys,the demand for primary magnesium is increasing dramatically all over the world.The Pidgeon process is the most widely used process for producing magnesium in China,but suffers from problems such as high energy,resource consumption and environmental pollution.While the process of vacuum carbothermal reduction to produce magnesium(VCTRM)has attracted more and more attention as its advantages,but it has not been well-practiced in industrial applications and there also is no comprehensive and quantitative analysis of this process.This study quantified the flows of resource and energy for the Pidgeon process and the VCTRM process,then compared and analyzed these two processes with each other from three aspects.The VCTRM process results in 63.14%and 69.16%lower of non-renewable mineral resources and energy consumptions when compared to the Pidgeon process,respectively.Moreover,the low energy consumption(2.675 tce vs.8.681 tce)and material to magnesium ratio(2.953:1 vs.6.429:1)of the VCTRM process,which lead to lower greenhouse gas(GHG)emissions(8.777 t vs.26.337 t)and solid waste generation(0.522 t vs.5.465 t)with a decrease of 66.67%and 90.45%,respectively.Results indicate that the VCTRM process is a more environmentally friendly process for magnesium production with high efficiency but low cost and low pollution,and it shows a good potential to be industrialized in the future after solving the bottleneck problem of the reverse reaction.

Response Surface Optimization for Process Parameters of LiFePO_4/C Preparation by Carbothermal Reduction Technology

A statistically based optimization strategy is used to optimize the carbothermal reduction technology for the synthesis of LiFePO4/C using LiOH,FePO4 and sucrose as raw materials.The experimental data for fitting the response are collected by the central composite rotatable design(CCD).A second order model for the discharge ca-pacity of LiFePO4/C is expressed as a function of sintering temperature,sintering time and carbon content.The ef-fects of individual variables and their interactions are studied by a statistical analysis(ANOVA).The results show that the linear effects and the quadratic effects of sintering temperature,carbon content and the interactions among these variables are statistically significant,while those effects of sintering time are insignificant.Response surface plots for spatial representation of the model illustrate that the discharge capacity depends on sintering temperature and carbon content more than sintering time.The model obtained gives the optimized reaction parameters of sinter-ing temperature at 652.0 ℃,carbon content of 34.33 g?mol-1 and 8.48 h sintering time,corresponding to a dis-charge capacity of 150.8 mA·h·g-1.The confirmatory test with these optimum parameters gives the discharge ca-pacity of 147.2 and 105.1 mA·h·g-1 at 0.5 and 5 C,respectively.

Synthesis of ZrO_2-SiC Composite by Carbothermal Reduction of Zircon

Zircon （mesh size ≤ 44μm ） and carbon black （mesh size ≤30μm ） were used as the starting materials, weighed with re（zircon） ： re（carbon black） of 100 ： 20 and mixed fully. The specimens with the diameter of 20ram and length of 5ram were prepared by pressing at 100 MPa, then dried at 120℃ for 12h, put into a furnace with 1. 5L ·min^-1 argon gas and fired at 1450℃, 1500℃, 1550℃, 1600℃ and 1650℃ for 4h, respectively. The chemical composition, phase composition and microstructure of the specimens were studied by chemical analysis, X-ray diffraction and scanning electronic microscope, and the carbothermal reduction reaction process was discussed by thermodynamic analysis. The results showed that the ZrO2-SiC composite could be synthesized by carbothermal reduction reaction using zircon and carbon black as the starting materials in argon atmosphere. The composite with different composition was obtained by controlling the firing temperature and partial pressure of CO gas. The proper temperature to synthesize ZrO2-SiC composite was 1600℃ in this experiment.

Preparation of ZrB_2-SiC Powders via Carbothermal Reduction of Zircon and Prediction of Product Composition by Back-Propagation Artificial Neural Network

Phase pure ZrB2-SiC composite powders were prepared after 1 450℃/3 h via carbothermal reduction route,by using ZrSiO4,B2O3 and carbon as the raw materials.The influences of firing temperature as well as the type and amount of additive on the phase composition of final products were detailedly investigated.The results indicated that the onset formation temperature of ZrB2-SiC was reduced to 1 400℃by the present conditions,and oxide additive（including CoSO4·7H2O,Y2O3 and TiO2）was effective in enhancing the decomposition of raw ZrSiO4,therefore accelerating the synthesis of ZrB2-SiC.Moreover,microstructural observation showed that the as-prepared ZrB2 and SiC respectively had well-defined hexagonal columnar and fibrous morphology.Furthermore,the methodology of back-propagation artificial neural networks（BP-ANNs）was adopted to establish a model for predicting the reaction extent（e g,the content of ZrB2-SiC in final product）in terms of various processing conditions.The results predicted by the as-established BP-ANNs model matched well with that of testing experiment（with a mean square error in 10^（-3） degree）,verifying good effectiveness of the proposed strategy.