机械活化对Nb2O5微波碳热还原的影响

利用高能球磨机和微波烧结炉研究机械活化对Nb₂O₅微波碳热还原的影响,对不同球磨时间、不同加热温度下Nb₂O₅的还原情况进行分析。使用电子显微镜(SEM)、能量色散谱仪(EDS)、X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)和失重率等手段研究了Nb₂O₅的还原情况和微观组织形貌。结果表明,在相同的烧结温度下,Nb₂O₅的失重率随球磨时间的延长而增加;在球磨20 h,1200℃微波烧结时,可将大部分Nb₂O₅还原成NbC,并在球磨30 h,1400℃微波烧结时,成功制得金属铌。机械活化可以加快Nb₂O₅微波碳热还原的进程,降低反应温度。     

钒钛矿转底炉直接还原炉底上涨成因及对策

针对钒钛磁铁矿转底炉直接还原过程中炉底上涨的原因进行了分析研究,并在实验室开展了相关试验。通过分析黏结物化学组成和物相组成,得出转底炉炉底上涨为玻璃质液相黏结高熔点橄榄石和铁氧化物累积导致炉底上涨;通过实验室试验研究表明,物料粒度是影响转底炉炉底上涨的关键因素,其次是还原温度和还原时间。根据上述研究结果,结合资源综合利用中试线现场条件,优化了原料转底炉系统的工艺参数,改进了干球技术指标,转底炉炉底上涨基本得到抑制,实现了试验生产顺行。     

鲕状赤铁矿微波加热还原提铁脱磷机制

采用微波加热还原鲕状赤铁矿内配碳球团,考察了还原温度、碱度及添加剂用量对球团含磷组元迁移的影响,对微波碳热还原提铁脱磷机制进行了分析。结果表明,随着还原温度的升高含磷组元逐渐被还原,当还原温度达到1 150℃以上时含磷矿物被大量还原,并且富集到还原铁中造成还原铁粉磷含量过高。在较低还原温度下,通过选择合适的碱度和脱磷剂用量,能有效地抑制含磷组元的还原,促进铁氧化物的还原和聚集。实验采用原矿粒度0.8 mm、碱度0.8、碳氧摩尔比1.0、钠盐添加剂用量20%(质量分数)、还原温度为950℃保温10 min的条件对物料进行还原,将还原物料研磨到0.074 mm在65 mT的场强下进行磁选可得到全铁质量分数82.79%、回收率86.49%、P质量分数0.34%的指标,所得到的还原铁粉杂质较少,而含磷物质主要以磷酸盐的形式存在于磁选渣中。     

高温球磨对氧化铝碳热还原反应的影响

研究了高温球磨对氧化铝碳热还原反应的作用。发现在６００℃高温球磨过程中发生了碳热还原反应,产物相为ＡｌＩＮ相;粉末经高温球磨后,再进行碳热还原氮化反应,与室温球磨及原始粉末相比,高温球磨后的反应率提高,即高温球磨促进了碳热还原反应的进行。     

低温固相反应法制备碱式碳酸锆

采用氧氯化锆和碳酸钠为原料进行低温固相反应,得到碱式碳酸锆钠前驱物,前驱物经过加稀盐酸和除杂后得到碱式碳酸锆.对碱式碳酸锆进行了红外光谱分析,并通过条件实验,研究了球磨时间、球磨转速对产物粒度和调酸pH对产物杂质含量的影响.结果表明:在对原料采用锆珠球磨、球磨转速150 r/min、球磨时间为2 h,对前驱物调酸除杂pH值稳定在3.9~4.1的最佳工艺条件下,制备的碱式碳酸锆产品平均粒度大约11μm,粒度分布均匀、分散性好、活性强、纯度高.     

低温还原制取超细铁粉的研究

探索了超细氧化铁粉低温还原制取超细铁粉的研究.采用高能球磨,制得不同粒度的超细氧化铁粉末,然后,分别在不同还原温度和还原时间下,进行氢气还原.对还原后的粉末进行氧含量的测定,并计算出氧化铁粉末的还原率,对还原铁粉进行粒度和粒度分布的分析,通过扫描电子显微镜,观察还原铁粉的形貌.找出超细氧化铁粉粒度、还原温度、还原时间等参数对氧化铁粉还原率、铁粉粒度、粒度分布和铁粉形貌等的影响.由于采用了高能球磨的方式破碎粉末,显著地增加了氧化铁粉末的比表面积、表面能及提高了粉末的活性.研究结果表明,较大地降低了还原温度,即使在280℃温度下,仍然可以被氢气还原.由于还原反应是在很低的温度下进行,粉末颗粒长大的动力被极大降低,所以能够制得超细铁粉.采用0.35μm氧化铁粉,在400℃的还原温度下,可以制取到粒度小于0.4 μm的超细铁粉,并且还原率接近100%.     

氧化还原—机械活化对攀西钛铁矿浸出行为的影响

研究了"氧化还原—机械活化—盐酸浸出"的方法对钛铁矿中主要杂质离子铁离子浸出行为的影响,并采用XRD、SEM/EDS对处理前后的矿物结构进行分析。结果表明:经过氧化还原—活化处理,钛铁矿的物相明显发生改变,铁迁移至表面,形成了富铁的新表面,表面变得疏松、凹凸不平,出现了大量的微裂缝,铁浸出率有了显著的提高。     

Fe-Cr-W复合氧化物粉末共还原工艺研究

通过H2-CO共还原法对Fe-18Cr-9W复合氧化物粉末进行还原，控制还原工艺的参数制得纳米级Fe-18Cr-9W复合粉末。采用XRD对粉末进行物相分析，并计算晶粒尺寸；采用高倍SEM观察粉末形貌；对复合粉末的费氏粒度、比表面面积、氧含量等进行测定与分析，研究还原温度和还原时间对粉末性能的影响。结果表明：当还原温度高于650℃时制得的复合粉末由Fe和Fe-（Cr，W）两相组成；粉末颗粒呈球形或近球形：还原温度和还原时间都对Fe-18Cr-9复合粉末的性能有显著影响，当还原温度为700℃，还原时间为90min时。制备的颗粒为平均费氏粒度低于0．58μm。平均BET粒度小于80nm，晶粒粒径小于50nm，粉末氧含量小于0．14％的纳米级Fe-18Cr-9复合粉末。     

铜渣还原磁选工艺实验研究

以浮选铜渣的尾渣为原料,对其配碳还原和磁选分离工艺进行实验研究.探究碱度、温度对铜渣还原的影响,并研究在相应条件下不同粒度对磁选产物的影响.对铜渣进行矿相分析可知铁主要以Fe3O4和铁橄榄石形式存在;焙烧温度为1 175℃、配碳量为wC/wO=1.2、碱度为R=0.4、粉碎粒度小于42μm时经还原和磁选,可得铁品位74.7%的磁性物质;对还原产物进行矿相分析后发现金属铁颗粒弥散分布在还原产物中,铜元素以冰铜的形式嵌布在金属铁颗粒中.     

喷雾转换法制备纳米WC-6Co复合粉的工艺研究

以偏钨酸铵、醋酸钴、有机碳为原料,去离子水为溶剂,采用喷雾干燥-煅烧-球磨-连续还原碳化新工艺制备纳米WC-6Co复合粉。采用氮气吸附法测定粉末比表面积,XRD、SEM分别分析粉末物相和形貌,研究球磨工艺对钨钴复合氧化物粉末性能的影响以及连续还原碳化过程中粉末比表面积的变化。结果表明,在连续还原碳化前进行球磨,可有效破碎粉末;适当增大球料比或延长球磨时间,可使粉末破碎效果更好,粒度分布更均匀,当球料比为10∶1、球磨时间为240min时,粉末破碎、分散效果最佳,比表面积为11.62m2/g;球磨后的钨钴复合氧化物粉末在连续还原碳化过程中发生团聚烧结、预合金化,生成平均粒度为80nm的WC-6Co复合粉。     

Mechanically activated carbothermic reduction of ilmenite

A systematic study of the effect of milling conditions on the low-temperature carbothermic reduction of the mineral ilmenite has been carried out. It was found that after ball milling of an ilmenite-carbon mixture at room temperature, the ilmenite was reduced to rutile and metallic iron during subsequent low-temperature annealing (760 °C for 30 minutes). A longer milling time results in a lower reduction temperature and a higher reduction rate. Higher milling intensity also leads to a lower reduction temperature. This enhanced reduction reaction induced by ball milling mainly results from the intimate mixing and large contact area between milled ilmenite and carbon particles.     

Effect of Temperature on Carbothermic Reduction of Ilmenite

The reduction of ilmenite (FeTiO3) 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, Ti3O5 and carbon.     

A Study of the Effect of Aluminium on the Mechanochemical Reduction of Hematite by Graphite

The effect of addition of small amounts of aluminium on mechano‐chemical reduction of hematite by graphite was studied. Various amounts of aluminium (0 to 10%) were added to a hematite‐graphite mixture, in which C/O ratio was 1:1. The hematite‐graphite‐aluminium mixtures were then subjected to ball milling followed by heating up reduction. The heating up reduction was carried out in Ar atmosphere, using TG‐DTA device. In TG‐DTA experiments, samples were heated by a constant heating rate of 10 °C/min from room temperature up to 1100 °C and maintained for 30 minutes at this temperature. To clarify the reactions which took place during milling and heating up reduction, the samples were subjected to XRD examinations. It was found that the heat generated during exothermic reaction of aluminothermic reduction of hematite promoted the endothermic reaction of carbothermic reduction. In the course of heating up reduction, the carbothermic reaction occurred just after aluminothermic reaction. Increasing of aluminum content from 0 to 10% in 2 hours ball milled samples decreased the temperature of carbothermic reaction from 1020 °C to about 860 °C. The further ball milling of the samples up to 5 and 10 hours, for the samples containing 10 and 5% aluminium respectively, caused the decrease of the temperature of aluminothermic and carbothermic reactions to around the melting point of aluminium.     

热酸球磨浸出攀枝花钛铁矿

在工业矿酸比条件下,研究攀枝花钛铁矿热酸球磨快速浸出的可行性,着重考察了搅拌球磨的转速、球料比、硫酸浓度以及反应温度等因素对酸解的影响。结果表明,与未实施球磨的浸出相比(其它试验条件相同、磨浸60 min),钛的浸出率可提高64%,这是由于搅拌球磨导致钛铁矿晶格畸变以及颗粒显著细化所致。获得了磨浸的优化工艺条件为:搅拌磨的转速700 r/min,球料比5∶1,矿酸比1∶1.6,硫酸浓度70%以及温度120℃。在此条件下磨浸60 min钛的酸解率达到81%,所得钛液稳定性≥550 mL,表明70%硫酸可直接液相酸解钛铁矿,为实现水解废酸循环利用提供了一条可行途径。     

外包法直接还原钛铁矿过程的动力学研究

采用外包还原剂的方法对钛铁矿进行直接还原试验,研究了直接还原钛铁矿的动力学。结果表明,半焦粉直接还原钛铁矿分为两个阶段,第一阶段是升温阶段和恒温的初始阶段,受界面化学反应控制,表观活化能为113.14kJ/mol;第二阶段为恒温阶段,受固相中气体的内扩散控制,表观活化能为180.13kJ/mol。温度对还原度和还原速率的影响显著。随着温度的升高,还原度随之升高,反应速率加快;延长恒温时间也可以提高还原度,但恒温阶段反应速率增加缓慢     

球磨参数对机械合金化制备Al_2O_3/Mo_5Si_3复合粉体特性的影响

以MoO3粉、Mo粉、Si粉及Al粉为原料,采用机械化学还原法制备了Al2O3/Mo5Si3复合粉体。利用XRD、SEM等对复合粉体在球磨过程中的物相转变和形貌进行表征,并对球磨参数对机械合金化过程的影响进行探讨。结果表明,原料粉体球磨10 h后转变为Al2O3/Mo5Si3复合粉体,反应较完全。随球磨时间延长,复合粉体细小均化,粉体粒度较小,球磨20h后粉体粒度在3~5μm之间,随球磨转速的提高,球磨时间延长,球磨提供能量提高,反应开始时间变短。     

制备工艺对无钴AB5型贮氢合金的相结构和电化学性能的影响

用真空熔炼、快淬工艺以及球磨工艺制备稀土基无钴AB5型La（NiMnAlFe）5贮氢合金，用XRD测试了合金的相结构，并测试了不同制备工艺下合金的电化学性能。研究了制备工艺对无钴合金的相结构和电化学性能的影响。结果表明，由真空熔炼和快淬工艺制备的合金为CaCu5型单相结构，球磨合金由CaCu5型相和游离Ni相组成，并出现了非晶化趋势。快淬和球磨均使合金的放电容量降低，循环稳定性提高，但球磨工艺的影响更为显著，主要原因是球磨后合金中出现非晶化趋势。     

Effect of Different Production Methods on the Mechanical and Microstructural Properties of Hypereutectic Al-Si Alloys

In this study, the effects of different production methods like melt spinning, high-energy ball milling, and combined melt spinning and high-energy ball milling on the mechanical and microstructural properties of hypereutectic Al-20Si-5Fe alloys were investigated. While microstructural and spectroscopic analyses were performed using scanning electron microscopy and X-ray diffractometry, mechanical properties were measured using a depth-sensing indentation instrument with a Berkovich tip. Microstructural and spectroscopic analyses demonstrate that high-energy ball milling process applied on the melt-spun Al-20-Si-5Fe alloy for 10 minutes brings about a reduction in the size of silicon particles and intermetallic compounds. However, further increase in milling time does not yield any significant reduction in size. High-energy ball milling for 10 minutes on the starting powders is not enough to form any intermetallic phase. According to the depth-sensing indentation experiments, high-energy milling of melt-spun Al-20Si-5Fe alloys shows an incremental behavior in terms of hardness values. For the Al-20Si-5Fe alloys investigated in this study, the production technique remarkably influences their elastic–plastic response to the indentation process in terms of both magnitude and shape of P-h curves.     

钛铁矿的还原技术研究现状

在简要分析当前钛铁矿还原富集技术中存在的问题的基础上,阐述了钛铁矿的非碳热还原及常规碳热还原技术的国内外研究现状。结合微波加热的特点,重点阐述了钛铁矿的微波碳热还原的国内外研究现状。指出,微波加热应用于钛铁矿的碳热还原,能明显提高炭的还原能力,提高还原速率,缩短反应时间,大幅度降低能耗,显示出良好的经济价值和潜在的工业化前景,同时也指出了钛铁矿微波碳热还原技术中需要解决的问题。     

Preparation of synthetic rutile by hydrochloric acid leaching of mechanically activated Panzhihua ilmenite

Dissolution of mechanically activated Panzhihua ilmenite in hydrochloric acid for the preparation of synthetic rutile was investigated. Both the dissolution and its coupled titanium hydrolysis were greatly enhanced by the mechanical pretreatment. Increases in the lattice strain and surface area of ilmenite induced by energetic ball milling were responsible for the enhanced dissolution. The rapid hydrolysis led to formation of quantities of the nanosized primary particles, giving rise to a solid/liquid separation problem. The 15 min milled ilmenite, however, yielded an easy-to-filter hydrolysate due to formation of porous, micron-sized, secondary particles during the dissolution. The crystallization and aggregation behaviour of the primary particles were probably related to both the surface property of the un-reacted solid and the ferric ion concentration in solution. The technology for preparation of synthetic rutile was systematically investigated. The optimum milling and dissolution conditions were as follows: milling in air for 15 min, hydrochloric acid concentration 20%, initial reaction temperature 100 °C, ilmenite/20% acid mass ratio 1 g:5.5 g, reaction time ≥ 6 h. The synthetic rutile prepared under the optimum conditions contained 92% TiO₂ and 2.1% Fe₂O₃ as well as combined CaO and MgO of 0.28%. The results demonstrate that the mechanical pretreatment can take the place of the traditional high temperature pretreatment of ilmenite and avoid the dissolution being conducted under pressurized condition.