钙化-酸浸提钒沉钒母液中锰的回收

对钙化?酸浸提钒沉钒母液中锰资源的回收，一方面可以提升提钒工艺的经济效益，另一方面可避免母液循环时锰浓度不断累积而影响氧化钒产品质量，从而有助于实现母液闭路循环而提升全流程的环境效益。本工作提出了采用草酸沉淀法高效回收沉钒母液中的Mn2+，考察溶液体系pH值、草酸加量系数、反应温度和时间对锰回收率及沉淀产物物相组成的影响，以及草酸沉淀分离锰后母液的循环次数对钒浸出过程的影响。结果表明，草酸沉淀法可高效分离沉钒母液中的Mn2+，在溶液体系pH=4.0、草酸加量系数为1.5、反应温度为50℃、反应时间为60 min的条件下，锰回收率达94.33%，所得产物为纯度大于98%的水合草酸锰，为片状晶体，并呈花簇状生长。将脱锰后的沉钒母液循环至酸浸段，对钒浸出率及浸出液中锰的浓度没有明显影响，表明该方法有助于实现钙化?酸浸提钒中废水的闭路循环。     

Al-Er-Zr合金的热变形行为及动态析出

通过对Al-0.04Er-0.08Zr合金进行200°C 到450°C 范围内的热压缩测试对该合金的热变形行为进行了研究，在这个过程中利用Arrhenius-type方程进行线性拟合从而分析应力-应变曲线，之后通过透射电镜来观察研究变形组织。结果表明对于固溶态以及时效态合金来讲，在热压缩过程中动态回复是使合金软化的一个主要机制。高温以及低应变速率的热变形会诱导固溶态合金快速析出。动态析出会明显增加固溶态合金在热压缩过程中其表面的流变应力，但是却不能有效提高变形合金的硬度。动态析出还会导致应力-应变曲线拟合出现Arrhenius型偏差。     

白云鄂博矿焙烧浸出-萃取沉淀分离稀土及钍的试验研究

采用焙烧浸出-萃取沉淀法从白云鄂博稀土精矿中分离稀土和钍,得到最佳焙烧浸出条件为: 矿酸比1∶1.5、焙烧时间1 h、焙烧温度200 ℃、水浸液固比8∶1、水浸时间4 h、水浸温度50 ℃,最佳条件下CeO₂、La₂O₃、Nd₂O₃、Pr₆O₁₁、Sm₂O₃和ThO₂浸出率分别为80.77%、69.24%、95.71%、76.82%、93.31% 和98.13%。采用羧酸类萃取-沉淀剂从浸液中萃取分离稀土和钍,在萃取-沉淀剂皂化度70%、料液pH=3.1、萃取-沉淀剂和钍的摩尔比4∶1的最佳条件下,稀土和钍萃取-沉淀率分别为19%和90%,实现了稀土和钍的有效分离。     

Coherency strain induced hardening in bulk polycrystalline ceramics: A case study with MgO-based “ceramic alloys”

The role of coherency strain at the matrix/precipitate interface toward hardening of bulk polycrystalline “ceramic alloys” has been established here. Formation of “near ideal” bulk polycrystalline ceramic microstructure characterized by the presence of uniformly distributed coherent “ultra-fine” MgCr₂O₄ particles (size: ~25 nm) within matrix (MgO) grains was achieved via solid-state precipitation during aging treatment of bulk supersaturated MgO–Cr₂O₃ solid solutions (formed during pressureless sintering in air, followed by fast cooling). The as-aged MgO–MgCr₂O₄ “ceramic alloys” exhibited hardness increment by ~73% over that of phase pure bulk MgO upon aging for just 10 hours at 1000°C in air. Evidences toward the presence of significant coherency strains across the MgO/MgCr₂O₄ coherent interfaces were obtained with transmission electron microscopy. Analysis based on hardening mechanisms and comparisons with MgO–MgFe₂O₄ system, having lesser hardening due to lower misfit strain at MgO/MgFe₂O₄ coherent interfaces (despite greater content of second-phase particles), confirm the dominant role of coherency strains toward hardness enhancement in “ceramic alloys.”     

Single-phase and binary phase nanogranular ferrites for magnetic hyperthermia application

The study demonstrates the performance of heating efficiency in single-phase and binary phase spinel ferrite nanosystems. Ferrimagnetic cobalt ferrite (CoFe₂O₄) (CFO) and superparamagnetic copper ferrite/copper oxide (CuFe₂O₄/CuO) (CuF) nanosystems of different particle sizes were synthesized through a microwave-assisted coprecipitation method. The heating behavior was observed in range of both field amplitudes (8-24 kA/m at 516 kHz) and frequencies (325-973 kHz at 12 kA/m). The heating efficiency was analyzed and compared by means of particle size, magnetization, effective anisotropy constant, and Néel relaxation mechanism. Indeed, the heating rate was maximized in larger ferrite particles with low effective anisotropy constant. Moreover, though the magnetization and effective anisotropy constant of single-phase CoFe₂O₄ nanoparticles were higher, the binary phase CuFe₂O₄/CuO nanosystems of similar crystallite size (28 nm) exhibited superior heating efficiency (4.21°C/s). For a field amplitude and frequency of 24 kA/m and 516 kHz, the heating rate of CuF and CFO ferrites with different crystallite sizes decreased in the order of 4.21 > 2.14 > 0.58 > 0.52°C/s for 29 nm > 25 nm > 12 nm > 15 nm, respectively. The results emphasize that binary phase ferrite nanoparticles are better thermoseeds than the single-phase ferrites for the magnetic hyperthermia application.     

Effect of pH on the detailed chemical nature and metal-carbonate species in as synthesized zirconia alumina composites

Zirconia was deposition precipitated on γ-alumina in pH range 7-10 from zirconium oxy-nitrate and soda ash. Zirconium formed its hydroxycarbonate as deduced from ICP-EOS, CHN, and TGA-MS. Higher pH favored formation of carbonate species of zirconium over its hydroxide. TGA-MS indicated formation of three different types of carbonate species. FTIR results corroborated this. Monodentate metal carbonate was observed irrespective of pH of preparation. In addition, bridged bidentate species formed at pH ≤ 8 which changed to chelating bidentate at pH > 8. XRD indicated that all the samples formed tetragonal-zirconia upon calcination irrespective of pH of preparation. Higher pH resulted in smaller crystallites of t-ZrO₂. Changes in chemical moiety with pH reflected on acidity and the deactivation rate for 2-methyl-3-butyn-2-ol which decreased by two orders of magnitude in samples prepared at higher pH. Surface area and pore volume benefited from deposition precipitation. SEM-EDAX showed reasonable distribution of zirconia over γ-Al₂O₃.     

碳化反沉淀法去除硫酸锰浸出液中钙、镁的研究

采用碳化沉锰法去除硫酸锰溶液中的钙、镁离子。以CO₂为碳化剂, 将硫酸锰溶液中的Mn²⁺以碳酸锰沉淀的形式从原溶液中分离出来, 然后用硫酸将沉淀物溶解, 从而达到除杂的目的。考查了CO₂流量、反应温度、pH值及反应时间对钙、镁离子去除效果的影响, 结果表明, 最适宜条件为反应温度45 ℃、溶液pH值7.0、CO₂流量2.7 L/min、反应时间60 min, 此时碳化产物中钙、镁离子含量分别为0.03%和0.01%, 达到了HG/T 2836-2011高纯碳酸锰Ⅰ型品的标准。     

酸性废水中As(Ⅲ)、Cu(Ⅱ)与铁粉的反应行为

在Fe-As(Ⅲ)-Cu(Ⅱ)-H₂O体系中, 研究了酸性废水中As(Ⅲ)、Cu(Ⅱ)与金属铁粉的反应行为, 考察了反应过程中As在气、液、固三相中的分配比。结果表明, As(Ⅲ)和Cu(Ⅱ)离子被Fe还原为单质As和Cu后, As、Cu进一步结合成Cu₅As₂等金属间化合物, 从而促进As(Ⅲ)沉淀反应的发生, 且无AsH3生成。在反应时间40min、铁粉过量系数1.2、溶液初始pH=0.0、温度40 ℃、Cu/As摩尔比1.0条件下, As在气、液、固三相中的分配比分别为0、20.7%和79.3%, 沉砷率为79.3%。     

一种镍基单晶高温合金高周疲劳引起的g′溶解行为研究

研究了一种镍基单晶高温合金SRR99在不同温度下的高周疲劳行为,试样采用[001]取向的单晶试棒。结果表明条件疲劳强度随着试验温度的升高先上升后降低,具有与高温拉伸强度表现出相同的变化规律。通过扫描电子显微镜和透射电子显微镜的观察发现g′相的形貌发生了显著变化,经过高温循环变形后g′析出相发生了溶解。在交变应力的作用下,g′与基体界面产生大量的位错,而位错的往复运动引起了g′相的溶解。因此循环加载过程中伴随着g′的不断溶解,共格界面的强化作用不断减弱。 除此之外,通过裂纹扩展方向与试样轴向的夹角可以判断出疲劳裂纹的扩展主要沿着(111)晶面进行,根据扫描电镜和透射电镜的观察结果对于循环加载的微观组织演化机理进行了讨论。     

Study on wax precipitation characteristics of wax deposit in pipes

Wax deposit properties are a significant concern in pipeline pigging during waxy crude oil transportation. In the present work, the impacts of flow conditions and oil properties on the wax precipitation characteristics of wax deposits are investigated. A flow loop apparatus was developed to conduct wax deposition experiments using four crude oils collected from different field pipes. The differential scanning calorimetry (DSC) technique was employed to observe the wax precipitation characteristics of crude oil and wax deposit. The results show that the wax content and the wax appearance temperature (WAT) of the deposits increase with shear stress and radial temperature gradient, and decrease with radial wax molecule concentration gradient near the pipe wall. The DSC tests on the wax deposits revealed that the deposit wax content is strongly correlated to the oil wax content. Furthermore, an empirical correlation was developed to predict the wax content and the WAT of the wax deposit. Verification of the empirical correlation using the different oils indicated that the average relative error of the wax content prediction and average absolute error of WAT prediction were 13.2% and 3.6°C, respectively.