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Research into the Percolation Leaching of Copper and Silver from Stale Tailings 陈旧尾矿中铜、银的渗流浸出研究
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224700032
L. M. Karimova, Ye. T. Kairalapov, B. E. Mansurov

Silver extraction by percolation leaching on a pelletized sample of stale tailings with the organic binding agent Alcotac® CB6 is studied. A column 0.5 m high and 56 mm in internal diameter was used for laboratory tests on percolation leaching. Pelletization was carried out in a drum-type granulator with the Alcotac® CB6 reagent (BASF, Germany) consumption of 800 g/t; the moisture content of the granules was 8–10% with a size of 8–10 mm. The composition of the samples was determined based on the data of optical and electron microscopy, X-ray diffraction, local X-ray spectral, X-ray fluorescence, and mass spectrometry with inductively coupled plasma. Stale tailings of the Zhezkazgan enrichment plant (Ulytau region, Republic of Kazakhstan) were examined, in which the main part of copper is represented by oxidized minerals (78.47%); content of sulfide minerals is 21.53%. The results of physicochemical studies with the determination of the material composition of the sample and observations on the percolation leaching of copper and silver from the stale tailings of Zhezkazgan are presented. The copper leaching was studied in two stages using a sulfuric acid solution as a solvent. The next stage was the transfer of silver into the solution by cyanidation. Copper extraction into the solution was 88.55% with a sulfuric acid consumption of 80.0 kg/t of tailings, and that of silver was 75.31% with a sodium cyanide consumption of 0.55 kg/t. The studies of two-stage leaching showed the effectiveness of preliminary pelletizing of stale tailings with the Alcotac® CB6 reagent. In the process of leaching, the pelletized material features sufficient porosity and permeability and provides access of cyanide solutions to the surface of precious metals.

研究了有机结合剂Alcotac®CB6对陈旧尾矿球团样的渗滤提银。采用高0.5 m、内径56 mm的渗滤柱进行室内渗滤试验。在鼓式造粒机中进行制粒,Alcotac®CB6试剂(德国巴斯夫)用量为800 g/t;颗粒含水量为8-10%,粒径为8 - 10mm。根据光学和电子显微镜、x射线衍射、局部x射线光谱、x射线荧光和电感耦合等离子体质谱的数据确定样品的组成。对哈萨克斯坦乌里陶地区Zhezkazgan富集厂的陈旧尾矿进行了检测,其中铜的主要成分为氧化矿物(78.47%);硫化物矿物含量为21.53%。本文介绍了样品物质组成测定的物化研究结果和浙兹卡兹干废尾矿中铜、银的渗流浸出观察结果。以硫酸溶液为溶剂,分两阶段对铜浸出进行了研究。下一阶段是通过氰化将银转移到溶液中。铜浸出率为88.55%,尾矿硫酸用量为80.0 kg/t;银浸出率为75.31%,尾矿氰化钠用量为0.55 kg/t。两段浸出试验表明,采用Alcotac®CB6试剂对陈旧尾矿进行初步制粒是有效的。在浸出过程中,球团化物料具有足够的孔隙度和渗透性,为氰化物溶液进入贵金属表面提供了通道。
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引用次数: 0
Heat Treatment Effect on the Structure and Properties of Workpieces from Heat-Resistant Nickel Alloys Obtained by Additive Technologies 热处理对增材制造耐热镍合金工件组织和性能的影响
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224700056
A. V. Balyakin, E. A. Nosova, M. A. Oleinik

Both conventional technologies for obtaining workpieces and the additive technological process of direct energy and material feeding (direct energy deposition, DED) are employed for manufacturing bulky workpieces for gas turbine engine parts from heat-resistant nickel-based alloys. The DED technology allows managing a highly coordinated energy impact on the microvolume of the alloy, which ensures obtaining the material structure with higher working characteristics compared to castings. At present, application of nickel material in additive technologies is limited by the ultrafast crystallization processes that cause accumulation of significant internal stresses, which leads to formation of micro- and macrodefects. Heat treatment is recommended for residual stress reduction in the products after the DED process, but optimal modes of such processing of a workpiece are not specified. On the other hand, heat treatment implies obtaining high mechanical properties. For products fabricated by additive methods of surfacing powders with nonequilibrium structure, similar recommendations are insufficient. The place of heat treatment in the general cycle of manufacturing parts is set depending on the requirements for the properties of the product. In most cases, heat treatment is performed after mechanical post-treatment. This is associated with the requirements for high strength, hardness, and wear resistance of the product material. The article studies the effect of various heat treatment modes on the hardness, microstructure, and residual stresses of the samples made of the KhN50VMTYuB heat-resistant nickel-based alloy obtained by the DED technology. The DED technology of workpiece manufacturing from the KhN50VMTYuB alloy leads to a fairly high hardness of about 190 HB. It is well known that the growth of products from the highly alloyed powder of nonequilibrium structure proceeds by rapid cooling, which causes structural changes similar to the aging while heating by a laser beam. Heat treatment of the grown products may be aimed at increasing the machinability by cutting and reducing the warping of products, as a result of the redistribution of residual stresses. In this case, the decrease in hardness may be the criterion of goal achieving. The results of the presented study demonstrate that the most cost-efficient mode of heat treatment for the residual stress removal is the mode consisting in heating up to 1180°C and holding for 4 h with subsequent air cooling, which allows reducing hardness from 191 ± 1 HВ to 135 ± 1 HВ. The lowest hardness values of HB 128 ± 1 were obtained after heating to 1140°C, holding for 4 h, and cooling with a furnace. Air cooling allows obtaining the hardness of HB 130 ± 18. On one hand, this indicates slightly higher hardness values, but deviations are of a higher level, and the level of residual stresses in the annular samples herewith are of the lowest values, which follows from the results of change in the geometr

采用传统的工件获取技术和直接能量和材料进料的增材工艺(直接能量沉积,DED)制造燃气涡轮发动机耐热镍基合金零件的大块工件。DED技术允许在合金的微体积上管理高度协调的能量影响,从而确保获得比铸件具有更高工作特性的材料结构。目前,镍材料在增材技术中的应用受到了超快结晶过程的限制,该过程会导致显著的内应力积累,从而导致微观和宏观缺陷的形成。建议在DED工艺后对产品进行热处理,以减少残余应力,但没有规定对工件进行这种加工的最佳模式。另一方面,热处理意味着获得高的机械性能。对于用非平衡结构的表面粉末的添加剂方法制造的产品,类似的建议是不够的。热处理在制造零件一般周期中的位置是根据对产品性能的要求而定的。在大多数情况下,热处理在机械后处理之后进行。这与产品材料的高强度、硬度和耐磨性要求有关。本文研究了不同热处理方式对采用DED技术制备的KhN50VMTYuB耐热镍基合金试样硬度、显微组织和残余应力的影响。用KhN50VMTYuB合金制造工件的DED技术可获得相当高的硬度,约为190 HB。众所周知,非平衡结构的高合金粉末的生长是通过快速冷却进行的,这种快速冷却引起的结构变化类似于激光束加热时的时效。由于残余应力的重新分布,热处理的目的可能是通过切削和减少产品的翘曲来提高可加工性。在这种情况下,硬度的降低可能是达到目标的标准。研究结果表明,去除残余应力最经济有效的热处理方式是加热至1180°C并保持4小时,随后进行空气冷却,这可以将硬度从191±1 HВ降低到135±1 HВ。加热至1140℃,保温4 h,用电炉冷却后,HB 128±1的硬度值最低。风冷可获得HB 130±18的硬度。一方面,这表明硬度值略高,但偏差程度较高,环形试样的残余应力水平最低,这是切割后试样几何形状变化的结果。热处理结束时,加热至1100℃,保温4 h,空冷,硬度最高,为311±8 HB;然后加热至950℃,保温3.5 h,风冷;然后加热至800℃,保温7.5 h,并风冷;然后加热至700°C,保温14小时,空气冷却。长大试样的显微组织分析表明,经过各种热处理后,试样中形成了非等晶组织,沉积颗粒的层状组织特征丧失。
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引用次数: 0
Flow Behavior and Microstructure Characterization of an Ultrahigh-Alloyed Al–Zn–Mg–Cu Alloy 超高合金化Al-Zn-Mg-Cu合金的流动行为和微观组织表征
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224600807
Xiaorong Yang, Zhifa Wang, Xiongbo Yan, Yinyue Li, Zheming Zhang

Hot compression tests were conducted on an ultrahigh-alloyed Al–Zn–Mg–Cu alloy within a temperature range of 250 to 450°C and a strain rate range of 0.001 to 1 s–1. The effects of strain rate and temperature on the flow curves were analyzed, along with the relationship between flow stress and microstructural evolution. The results indicate that, except for a strain rate of 1 s–1 across all temperatures, the flow curves following the peak stress do not exhibit monotonic work hardening or dynamic softening. In contrast, continuous work hardening is observed at this strain rate. The diverse shapes of the flow curves are attributed to the various precipitates formed due to the high alloying element content. Dynamic recovery (DRV) is identified as the main flow softening mechanism for the ultrahigh-alloyed Al–Zn–Mg–Cu alloy. While dynamic recrystallization (DRX) contributes to flow softening at a strain rate of 0.001 s–1, the deformed microstructure becomes the predominant softening mechanism at lower temperatures and higher strain rates. Additionally, the low intensity of isotropic texture at higher temperatures and strain rates facilitates DRX, resulting in a decrease in peak stress.

对一种超高合金Al-Zn-Mg-Cu合金进行了热压缩试验,温度范围为250 ~ 450℃,应变速率范围为0.001 ~ 1 s-1。分析了应变速率和温度对流变曲线的影响,以及流变应力与微观组织演化的关系。结果表明,除了在所有温度下应变速率为1 s-1外,峰值应力后的流动曲线不表现为单调加工硬化或动态软化。相反,在此应变速率下,观察到连续的加工硬化。流动曲线的不同形状是由于合金元素含量高而形成的各种析出物所致。动态恢复(DRV)是超高合金Al-Zn-Mg-Cu合金的主要流变软化机制。在应变速率为0.001 s-1时,动态再结晶(DRX)有助于流动软化,而在较低温度和较高应变速率下,变形组织成为主要的软化机制。此外,在较高的温度和应变速率下,各向同性织构的低强度有利于DRX,导致峰值应力降低。
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引用次数: 0
Improving the Quality of Metallurgical-Grade Silicon by Acid Leaching 酸浸法提高冶金级硅的质量
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224700044
N. V. Nemchinova, A. A. Zaitseva

The aim is to conduct research in the field of hydrometallurgical refining of metallurgical silicon. The object of research was metallurgical silicon after oxidative refining from AO Kremnii, part of the United Company RUSAL (Shelekhov, Irkutsk oblast, Russia). The chemical composition of the obtained samples was studied by X-ray fluorescence analysis and X-ray spectral microanalysis. According to elemental analysis, metallurgical silicon contains (wt %) 0.53Al, 0.6094Fe, 0.0491Ti, 0.0628Ca, 0.0066V, 0.002Cr, 0.014Mn, 0.003Cu, 0.010P, 0.007Ba, 0.007Ni, 0.002Zn. It is shown that intermetallic compounds of the following composition were recorded in the studied samples: AlFeSi2 (with an admixture of Ca), FeSi2 (with an admixture of Al), FeSi2Ti (with an admixture of Zr). To reduce the content of impurities in silicon, we selected the following acids as solvents: 10% H2SO4, HCl, and HNO3, as well as 4% HF in various ratios. To study the possibility of reactions of interaction of intermetallic compounds with selected solvents, the values of the Gibbs energy change, which had negative values, were calculated. Experimental leaching of impurities was conducted on silicon samples with particle sizes of –200 μm under constant stirring using a magnetic stirrer. The process parameters included a temperature of 60°C, a liquid-to-solid ratio of 5 : 1, and a purification duration of 60 min. It was found that using a solvent mixture of sulfuric and hydrofluoric acids in a 1 : 1 ratio achieved the highest degree of silicon purification, with an impurity removal rate of 86.85%. It is shown that when using a mixture of sulfuric and hydrochloric acids in a ratio of 1 : 3, the degree of purification of metallurgical silicon was 41.48%. In this way, solvents that enable maximum purification of silicon from impurity elements were identified.

目的是开展冶金用硅湿法精炼领域的研究。研究对象是俄铝联合公司(俄罗斯伊尔库茨克州谢列霍夫)的一部分AO Kremnii氧化精炼后的冶金硅。用x射线荧光分析和x射线光谱微量分析研究了所得样品的化学成分。根据元素分析,冶金用硅含有(wt %) 0.53Al、0.6094Fe、0.0491Ti、0.0628Ca、0.0066V、0.002Cr、0.014Mn、0.003Cu、0.010P、0.007Ba、0.007Ni、0.002Zn。结果表明,在所研究的样品中记录了以下组成的金属间化合物:AlFeSi2(掺Ca), FeSi2(掺Al), FeSi2Ti(掺Zr)。为了减少硅中杂质的含量,我们选择了以下几种酸作为溶剂:10%的H2SO4、HCl、HNO3和4%不同比例的HF。为了研究金属间化合物与选定溶剂相互作用的可能性,计算了具有负值的吉布斯能变值。采用磁力搅拌器对粒径为-200 μm的硅样品进行了连续搅拌浸出实验。工艺参数为温度60℃,液固比为5:1,净化时间为60min。结果表明,使用硫酸和氢氟酸的溶剂混合物,以1:1的比例提纯硅的效果最好,杂质去除率为86.85%。结果表明,硫酸与盐酸的混合物以1:3的比例使用时,冶金用硅的净化度为41.48%。通过这种方法,确定了能够最大限度地从杂质元素中纯化硅的溶剂。
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引用次数: 0
Relationship between Anisotropy of Corrosion Properties of Extruded Alloys AZ31 and ZK60 with Crystallographic Texture and Volume Distribution of Second Phase Particles 挤压合金AZ31和ZK60腐蚀性能各向异性与晶体织构和第二相颗粒体积分布的关系
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224600832
E. D. Merson, V. A. Poluyanov, P. N. Myagkikh, A. A. Sergeev, D. L. Merson

Insufficient corrosion resistance of magnesium alloys limits their technical and medical applications. It is known that the corrosion rate of these materials depends, among other things, on the orientation of the samples relative to the workpieces, for example, rods or sheets obtained by thermomechanical processing. There is an opinion in the literature that this is primarily due to the influence of crystallographic texture. In this work, the corrosion resistance of samples cut from extruded rods of industrial alloys ZK60 and AZ31 along and across the extrusion direction was investigated. The corrosion rate was determined by the loss of weight and volume of the samples, as well as by the volume of hydrogen released when they were dissolved in a 0.9% NaCl solution. The microstructure and surface of the samples after corrosion tests were investigated using scanning electron microscopy, energy-dispersive X-ray microanalysis, and electron backscatter diffraction. It is shown that the rod has a pronounced basal texture, and therefore the crystallographic orientation of the grains to the lateral surface of the transverse and longitudinal samples is very different. It was found that samples of both alloys cut across the rod had higher corrosion resistance than longitudinal samples. According to published data, if the anisotropy of corrosion properties were caused by crystallographic texture, then longitudinal samples, on the contrary, should have a lower corrosion rate than transverse ones. Therefore, it is concluded that, in the case of medium- and high-alloy magnesium alloys, the anisotropy of corrosion properties is associated mainly with the nature of the volume distribution of second-phase particles, and not with the crystallographic texture. It is shown that the row arrangement of particles on the surface of longitudinal samples leads to deterioration of corrosion resistance.

镁合金的耐腐蚀性不足限制了其在技术和医疗上的应用。众所周知,这些材料的腐蚀速率,除其他因素外,取决于样品相对于工件的方向,例如,通过热机械加工获得的棒或片。文献中有一种观点认为,这主要是由于晶体结构的影响。本文研究了ZK60和AZ31工业合金挤压棒沿挤压方向和跨挤压方向的耐蚀性。腐蚀速率由试样的重量损失和体积损失以及在0.9% NaCl溶液中溶解时释放的氢的体积决定。采用扫描电子显微镜、能量色散x射线显微分析和电子背散射衍射对腐蚀试验后样品的微观结构和表面进行了研究。结果表明,该棒具有明显的基底织构,因此,横向和纵向样品的晶粒向侧面的晶体取向是非常不同的。结果表明,两种合金的横切试样均比纵向试样具有更高的耐蚀性。根据已发表的数据,如果腐蚀性能的各向异性是由晶体织构引起的,那么纵向样品的腐蚀速率应该低于横向样品。因此,在中、高合金镁合金中,腐蚀性能的各向异性主要与第二相颗粒的体积分布性质有关,而与晶体织构无关。结果表明,纵向试样表面颗粒的排状排列导致其耐蚀性下降。
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引用次数: 0
Processing and Microstructure Characterization of Bio-Waste Induced Closed-Cell Aluminium/SiCp Composite Foams 生物垃圾诱导闭孔铝/SiCp复合泡沫材料的制备及微观结构表征
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224600777
Thulasikanth Vaddi, Aditi Manthripragada, Padmanabhan Raghupathy

Aluminium closed-cell foams are valued for their low density, high stiffness, corrosion resistance, and recyclability, making them suitable for aerospace, marine, and automotive applications. The quality of these foams depends on raw materials and processing methods. Therefore, employing an efficient and cost-effective processing method and raw materials is vital for ensuring that the foam’s properties are not compromised. This work investigates the use of bio-waste chicken eggshell powder and recycled aluminium alloy as a foaming agent for closed-cell aluminium/SiCp composite foams. The foams produced are examined for micro & macrostructure and its characteristic mechanical behavior. The influence of SiCp concentration on foam expansion and stability are investigated. Eggshell powder enabled the aluminium alloy to expand and form foam, further adding SiCp resulted in the homogeneous distribution of pores with negligible metal drainage.

铝闭孔泡沫因其低密度、高刚度、耐腐蚀性和可回收性而受到重视,适用于航空航天、船舶和汽车应用。这些泡沫的质量取决于原材料和加工方法。因此,采用高效且具有成本效益的加工方法和原材料对于确保泡沫的性能不受损害至关重要。本研究以生物废鸡蛋壳粉和再生铝合金为发泡剂制备闭孔铝/SiCp复合泡沫材料。对所产生的泡沫进行了微;宏观结构及其特性力学行为。研究了SiCp浓度对泡沫膨胀和稳定性的影响。蛋壳粉使铝合金膨胀形成泡沫,再加入SiCp,气孔分布均匀,金属流通量可忽略不计。
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引用次数: 0
Modeling of Axial Compression of Aluminum Matrix Composite V95/10% SiC under Nonstationary Thermomechanical Conditions 非稳态热力学条件下V95/10% SiC铝基复合材料轴向压缩模型
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2025-02-22 DOI: 10.1134/S1067821224700020
D. I. Kryuchkov, A. V. Nesterenko, A. G. Zalazinsky

To obtain products made of aluminum-matrix composite materials (AMCM) with the required level of mechanical properties, processing by means of intense deformation is necessary. To model the deformation behavior in nonstationary conditions of thermal deformation treatment, the identification of the AMCM model remains an urgent task. One of the approaches to the description of material fluidity is the use of the Johnson–Cook plasticity model. In the proposed work, the object of research is an AMCM made of granulated high-strength aluminum alloy V95 of the Al–Zn–Mg–Cu system, reinforced with 10 wt % SiC particles. The aim of the work is to determine the influence of nonstationary thermomechanical (pressure on the workpiece and heating temperature) deformation conditions on the true deformation and deformation rate of the composite material, as well as to identify the material model and verify its application to study the processes of shape change in the studied pressure and temperature range. An experimental study of the precipitation process under uniaxial compression of sintered cylindrical samples of AMCM in the range of initial pressures of 5.65–7.81 MPa when heated to 510, 530, and 550°C is conducted. In this range, the dependences of the degree of deformation and the average deformation rate for the process are obtained. Identification of the rheological model of the material was carried out. A mode of preliminary thermomechanical processing is proposed and a prototype is manufactured at an initial pressure of 6.7 MPa on the workpiece and heated to 550°C in 84 min. The above mode provided relatively uniform filling of the stamp cavities with composite material. To confirm the possibility of applying the results of parametric identification of the material model, simulation modeling of the technological process of manufacturing a prototype was carried out.

为了使铝基复合材料(AMCM)制造的产品具有所要求的机械性能水平,必须通过强烈变形的方式进行加工。为了模拟非平稳条件下热变形处理的变形行为,AMCM模型的识别仍然是一个紧迫的任务。描述材料流动性的方法之一是使用Johnson-Cook塑性模型。本文的研究对象是由Al-Zn-Mg-Cu体系的粒状高强铝合金V95制成的AMCM,并用10% wt %的SiC颗粒增强。本工作的目的是确定非稳态热力学(工件压力和加热温度)变形条件对复合材料真实变形和变形速率的影响,并确定材料模型并验证其应用于研究所研究的压力和温度范围内的形状变化过程。在初始压力5.65 ~ 7.81 MPa范围内,加热至510、530、550℃,对烧结后的AMCM圆柱形试样在单轴压缩下的析出过程进行了实验研究。在这个范围内,得到了变形程度和平均变形速率的依赖关系。对材料流变模型进行了识别。提出了一种初步的热机械加工模式,并在工件上施加6.7 MPa的初始压力,在84 min内加热到550℃,制造出了原型。该模式提供了复合材料相对均匀地填充冲压腔。为了验证材料模型参数识别结果应用的可能性,对原型制造工艺过程进行了仿真建模。
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引用次数: 0
Process Research and Mechanism Analysis of Pellet Roasting and Monazite Decomposition 颗粒焙烧和独居石分解的工艺研究与机理分析
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-19 DOI: 10.1134/S1067821224600121
Jianfei Li, Yubo Xu, Zhisheng Dong, Ruifeng Ma, Xiaowei Zhang, Ligang Wen, Qing Wang, Xiaoyan Hao, Wenbin Xin, Zhaogang Liu

The concentrated sulfuric acid roasting method and caustic soda method, as the main processes for treating Bayan Obo mixed rare earth concentrate, have been operating normally for decades. However, due to their serious pollution, high cost, and waste of accompanying resources, relevant rare earth enterprises are facing severe environmental and cost pressures. The sodium carbonate roasting method is a clean method for treating rare earth minerals, but due to the phenomenon of “ring formation” in the rotary kiln during the reaction process, this process has not been widely promoted. Based on the above facts, this article proposes a decomposition method for sodium pelletizing to decompose monazite, which effectively alleviates the related technical problems caused by the “ring formation” problem. Moreover, the rare earth leaching rate is 86.87%, and the recovery rates of F, P, and Th are 98.64, 13.87, and 88.96%. It is a potential rare earth mineral cleaning production process and can provide certain technical references for relevant rare earth enterprises.

浓硫酸焙烧法和烧碱法作为处理巴彦奥博混合稀土精矿的主要工艺,几十年来一直正常运行。然而,由于其污染严重、成本高昂、伴生资源浪费等问题,相关稀土企业正面临着严峻的环保和成本压力。碳酸钠焙烧法是一种清洁的稀土矿物处理方法,但由于在反应过程中回转窑内存在 "结圈 "现象,该工艺一直未得到广泛推广。基于上述事实,本文提出了一种钠法造粒分解独居石的方法,有效缓解了 "成环 "问题带来的相关技术难题。此外,稀土浸出率为 86.87%,F、P、Th 的回收率分别为 98.64%、13.87%、88.96%。这是一种有潜力的稀土矿物净化生产工艺,可为相关稀土企业提供一定的技术参考。
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引用次数: 0
Exothermic Synthesis of Binary Solid Solutions Based on Hafnium and Zirconium Carbides 基于碳化铪和碳化锆的二元固溶体的放热合成
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-19 DOI: 10.1134/S106782122460025X
V. A. Shcherbakov, A. N. Gryadunov, M. I. Alymov

The paper presents the results of an experimental study into the possibility of producing ultrahigh temperature ceramics constituting solid solutions of HfC and ZrC carbides by the single-stage electrothermal explosion (ETE) method under pressure. Adiabatic flame temperature and phase composition of the equilibrium final product were calculated on the basis of thermodynamic data. It was shown that, when the ZrC content in the final product is less than 20 wt %, the adiabatic flame temperature reaches 3800–3900 K, and the combustion product contains hafnium and zirconium carbides. The effect of mechanical activation modes in an AGO-2 planetary centrifugal mill used for a reaction mixture containing Hf, Zr, and C powders on its properties, phase composition formation, and the microstructure of carbide solid solutions was studied. It was shown that high-energy mixing in hexane leads to the destruction of the crystal structure of Hf and Zr particles and the formation of amorphous composite particles. The synthesized samples of ultrahigh temperature ceramics were studied by X-ray diffraction and microstructure analyses. It was shown that exothermic synthesis leads to the formation of single-phase solid solutions of HfC and ZrC carbides with the average particle size of 1.5–0.2 µm. The residual porosity of the binary carbides obtained is 10–12%. It was found that, despite the high temperature of sample heating during ETE under pressure, the particle size of the resulting solid solutions is significantly (by an order of magnitude) smaller than the particle size of similar complex carbides (20–50 µm) obtained by other methods (SPS and hot pressing). This is associated with the rapidity of the exothermic interaction of the reagents (10–50 ms) during ETE.

本文介绍了一项实验研究的结果,即在压力下通过单级电热爆炸(ETE)法生产由 HfC 和 ZrC 碳化物固溶体构成的超高温陶瓷的可能性。根据热力学数据计算了平衡最终产物的绝热火焰温度和相组成。结果表明,当最终产物中的碳化锆含量小于 20 wt % 时,绝热火焰温度达到 3800-3900 K,燃烧产物中含有碳化铪和碳化锆。研究了用于含 Hf、Zr 和 C 粉末反应混合物的 AGO-2 行星离心研磨机中的机械活化模式对其性质、相组成形成和碳化物固溶体微观结构的影响。结果表明,正己烷中的高能混合会导致 Hf 和 Zr 颗粒晶体结构的破坏,并形成无定形的复合颗粒。通过 X 射线衍射和微观结构分析研究了合成的超高温陶瓷样品。结果表明,放热合成导致形成平均粒径为 1.5-0.2 微米的 HfC 和 ZrC 碳化物单相固溶体。获得的二元碳化物的残余孔隙率为 10-12%。研究发现,尽管在加压下进行 ETE 时样品加热温度很高,但所得到的固溶体的粒度明显(小一个数量级)小于通过其他方法(SPS 和热压)得到的类似复合碳化物的粒度(20-50 µm)。这与 ETE 期间试剂的快速放热作用(10-50 毫秒)有关。
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引用次数: 0
Tungsten Carbide by Electrothermal Explosion under Pressure: Accompanying Phase Transformations 碳化钨在压力下的电热爆炸:伴随的相变
IF 0.6 4区 材料科学 Q4 METALLURGY & METALLURGICAL ENGINEERING Pub Date : 2024-10-19 DOI: 10.1134/S1067821224600273
V. T. Telepa, M. I. Alymov, A. V. Shcherbakov

Phase transformations taking place during synthesis of WC by electrothermal explosion (ETE) were investigated within the following range of process parameters: T = 293–3700 K, 49.8–50.2 at % C, P = 96 MPa, V = 10 V, I = 20 МА/m2, sample diameter of 20 mm. The thermogram of the ETE process was subdivided into four stages (I–IV). Stage I, warmup, temperature range of 293–563 K, endothermic reaction (isothermic plateau), input electric energy Q = 2.96 kJ, specific input energy Е = 111.6 kJ/mol. Low-temperature stage II, 563–1190 K, ignition, Q = 5.46 kJ, Еа = 109.2 kJ/mol. High-temperature stage III, 1190–2695 K, eutectoid decay, order–disorder transformation, Q = 14.25 kJ, Еа = 424 kJ/mol. Stage IV, melting, 2695–3695 K, Q = 14.31 kJ, Еа = 143.2 kJ/mol. The rate of ETE reaction is highly sensitive to applied pressure, concentration of reagents, sample shape, oxide film, etc. Variation in E affords facile control of the ETE process.

研究了电热爆炸(ETE)合成碳化钨过程中在以下工艺参数范围内发生的相变:T = 293-3700 K,49.8-50.2 % C,P = 96 MPa,V = 10 V,I = 20 МА/m2,样品直径 20 mm。ETE 过程的热图细分为四个阶段(I-IV)。第一阶段,预热,温度范围为 293-563 K,内热反应(等温平台),输入电能 Q = 2.96 kJ,输入比能量 Е = 111.6 kJ/mol。低温阶段 II,563-1190 K,点火,Q = 5.46 kJ,Еа = 109.2 kJ/mol。高温阶段 III,1190-2695 K,共晶衰变,有序-无序转变,Q = 14.25 kJ,Еа = 424 kJ/mol。第四阶段,熔化,2695-3695 K,Q = 14.31 kJ,Еа = 143.2 kJ/mol。ETE 反应的速率对施加的压力、试剂浓度、样品形状、氧化膜等非常敏感。E 的变化可以方便地控制 ETE 过程。
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Russian Journal of Non-Ferrous Metals
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