2019 Vol. 26, No. 4

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Invited Review
Research progress in lead-less or lead-free three-dimensional perovskite absorber materials for solar cells
Huan-yu Zhang, Rui Li, Wen-wu Liu, Mei Zhang, and  Min Guo
2019, vol. 26, no. 4, pp. 387-403. https://doi.org/10.1007/s12613-019-1748-2
Abstract:
The trend toward lead-free or lead-less perovskite solar cells (PSCs) has attracted increasing attention over the past few years because the toxicity of lead (Pb) is one of the substantial restrictions for large-scale applications. Researchers have investigated the viability of substituting Pb with other elements (group 14 elements, group 2 elements, transition-metal elements, and group 13 and 15 elements) in the three-dimensional (3D) perovskites by theoretical calculations and experimental explorations. In this paper, recent research progress in Pb-less and Pb-free PSCs on the perovskite compositions, deposition methods, and device structures are summarized and the main problems that hinder the enhancement of device efficiency and stability are discussed in detail. To date, the fully Sn-based PSCs have shown a power conversion efficiency (PCE) of 8.12% and poor device stability. However, lead-less PSCs have shown higher PCE and a better stability. In addition, the introduction of double-perovskite materials also draws researchers' attention. We believe that the engineering of elemental composition, perovskite deposition methods, and interfacial modification are critical for the future development of Pb-less and Pb-free PSCs.
Research Article
Experimental study on dynamic mechanical property of cemented tailings backfill under SHPB impact loading
Yu-ye Tan, Xin Yu, Davide Elmo, Lin-hui Xu, and  Wei-dong Song
2019, vol. 26, no. 4, pp. 404-416. https://doi.org/10.1007/s12613-019-1749-1
Abstract:
Cemented tailings backfill (CTB) have increasingly been used in recent years to improve the stability of mining stopes in deep underground mines. Deep mining processes are often associated with rock bursting and high-speed dynamic loading conditions. Therefore, it is important to investigate the characteristics and dynamic mechanical behavior of CTB. This paper presents the results of dynamic tests on CTB specimens with different cement and solid contents using a split Hopkinson pressure bar (SHPB). The results showed that some CTB specimens exhibited one to two lower stress peaks after reaching dynamic peak stress before they completely failed. The greater the cement-to-tailings ratio is, the more obvious the strain reaction. This property mainly manifested as follows. First, the dynamic peak stress increased with the increase of the cement-to-tailings ratio when the impact velocity was fixed. Second, the dynamic peak stress had a quadratic relationship with the average stress rate. Third, the cement-to-tailings ratio could enhance the increase rate of dynamic peak stress with strain rate. In addition, the dynamic strength enhancement factor K increased with the increase of strain rate, and its value was larger than that of the rock samples. The failure modes of CTB specimens under low-speed impact were tensile failure and X conjugate shear failure, where were nearly the same as those under static uniaxial and triaxial compression. The CTB specimens were crushed and broken under critical strain, a failure mode similar to that of low-strength concrete. The results of the experimental research can improve the understanding of the dynamic mechanical properties of CTB and guide the strength design of deep mining backfills.
Research Article
Factors influencing the pumpability of unclassified tailings slurry and its interval division
Peng Li, Yun-bing Hou, and  Mei-feng Cai
2019, vol. 26, no. 4, pp. 417-429. https://doi.org/10.1007/s12613-019-1750-8
Abstract:
Tailings consolidation and discharging technology is currently a popular means for disposing tailings in China. In this study, we describe a laboratory investigation of the unclassified tailings slurry from an iron mine and analyze the influence of the concentration, amount of consolidation agent, and types of consolidation agent on the pumpability in terms of the slump, slump flow, and bleeding rate of the slurry. The results indicate that an increase in concentration leads to a pronounced decrease in the magnitude of the slump, slump flow, and the bleeding rate. Compared with the consolidation agents P.O42.5 and P.S.A32.5, the new consolidation agent offers substantial advantages in promoting the pumping performance of the slurry. The concentration more strongly affects the slump, slump flow, and the bleeding rate of the slurry than does the amount of the consolidation agent. We also constructed the pumpability interval of the slurry on the basis of the slump and bleeding rate and accordingly determined the proportioning parameters of the slurry with a concentration of 75wt% to 79wt% and with a consolidation agent concentration of 2wt%. In addition, we discussed the pumpability mechanism of the slurry.
Research ArticleOpen Access
Process mineralogy as a key factor affecting the flotation kinetics of copper sulfide minerals
Ataallah Bahrami, Mirsaleh Mirmohammadi, Yousef Ghorbani, Fatemeh Kazemi, Morteza Abdollahi, and  Abolfazl Danesh
2019, vol. 26, no. 4, pp. 430-439. https://doi.org/10.1007/s12613-019-1733-9
Abstract:
The aim of this study is to apply process mineralogy as a practical tool for further understanding and predicting the flotation kinetics of the copper sulfide minerals. The minerals' composition and association, grain distribution, and liberation within the ore samples were analyzed in the feed, concentrate, and the tailings of the flotation processes with two pulp densities of 25wt% and 30wt%. The major copper-bearing minerals identified by microscopic analysis of the concentrate samples included chalcopyrite (56.2wt%), chalcocite (29.1wt%), covellite (6.4wt%), and bornite (4.7wt%). Pyrite was the main sulfide gangue mineral (3.6wt%) in the concentrates. A 95% degree of liberation with d80 > 80 μm was obtained for chalcopyrite as the main copper mineral in the ore sample. The recovery rate and the grade in the concentrates were enhanced with increasing chalcopyrite particle size. Chalcopyrite particles with a d80 of approximately 100 μm were recovered at the early stages of the flotation process. The kinetic studies showed that the kinetic second-order rectangular distribution model perfectly fit the flotation test data. Characterization of the kinetic parameters indicated that the optimum granulation distribution range for achieving a maximum flotation rate for chalcopyrite particles was between the sizes 50 and 55 μm.
Research Article
Influence of metallurgical processing parameters on defects in cold-rolled steel sheet caused by inclusions
Rui Wang, Yan-ping Bao, Yi-hong Li, Zhi-jie Yan, Da-zhao Li, and  Yan Kang
2019, vol. 26, no. 4, pp. 440-446. https://doi.org/10.1007/s12613-019-1751-7
Abstract:
The cleanliness and defects for cold-rolled steel sheet caused by inclusions are greatly influenced by parameters in the metallurgical processing. Good control of parameters during the processing can lead to a better product. In this paper, data mining was used to explore the influence of parameters on defects in steel sheets. A decision tree model was established and it was found that the oxygen content before deoxidation, the end-point temperature of the converter, and the temperature before deoxidation had a great impact on the defects in the cold-rolled sheet that were caused by inclusions. This finding was confirmed by experiments with infrared absorption, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and automatic inclusion analysis methods. After optimization according to results from the model and experiments, the defect rate caused by the inclusions was reduced from 0.92% to 0.38%.
Research Article
Improving effect on forming quality and accuracy using a polyurethane board positioning/resetting the discrete steel pad in multi-point forming
Er-hu Qu, Ming-zhe Li, and  Rui Li
2019, vol. 26, no. 4, pp. 447-459. https://doi.org/10.1007/s12613-019-1752-6
Abstract:
To improve the quality of multi-point die forming, a new approach using discrete steel pads was proposed. The formability of three different multi-point die forming processes was analyzed through numerical simulation and experiments. Numerical simulation and experimental results showed that the use of discrete steel pads in the multi-point forming process can substantially improve the stress-strain state on the plate and suppress dimple, straight-edge, and wrinkle defects. This analysis verified that the use of discrete steel pads in a multi-point forming process can effectively improve the quality and accuracy with which sheet metal is formed.
Research Article
Segmented tubular synthesis of monodispersed microsized copper oxalate
Xun Liu, Xing Chen, and  Kai Huang
2019, vol. 26, no. 4, pp. 460-466. https://doi.org/10.1007/s12613-019-1753-5
Abstract:
Monodispersed microsized copper oxalate particles were prepared in a segmented continuous flow tube reactor, and the effect of the main parameters such as organic additive agent, initial copper ions concentration, residence time, and segmented media on the final products were investigated experimentally. The obtained copper oxalate microsized particles were disc-like in the presence of citrate ligand, which was the shape inducer for the precipitated copper oxalate. Thermodynamic equilibrium diagrams of the Cu(Ⅱ)-oxalate-H2O, Cu(Ⅱ)-oxalate-citrate-H2O, and Cu(Ⅱ)-oxalate-EDTA-H2O solution systems were drawn to estimate the possible copper species under the experimental conditions and to explain the formation mechanisms of copper oxalate particles in the segmented fluidic reactor. Both theoretical and experimental results indicated that the presence of chelating reagents such as citrate and EDTA had distinct effect on the evolution of particle shape. Air and kerosene were tested as media for the fluidic flow segmentation, and the latter was verified to better promote the growth of copper oxalate particles. The present study provides an easy method to prepare monodispersed copper oxalate microsized particles in a continuous scaling-up way, which can be utilized to prepare the precursor material for conductive inks.
Research Article
Biogenic amino acid methionine-based corrosion inhibitors of mild steel in acidic media
L. K. M. O. Goni, M. A. Jafar Mazumder, S. A. Ali, M. K. Nazal, and  H. A. Al-Muallem
2019, vol. 26, no. 4, pp. 467-482. https://doi.org/10.1007/s12613-019-1754-4
Abstract:
N,N-Diallyl methionine ethyl ester hydrochloride 5 underwent alternating copolymerization with SO2 via the Butler cyclopolymerization protocol in dimethyl sulfoxide (DMSO) to give water-soluble cycloterpolymer 6 with a~1:1 molar ratio of sulfide and sulfoxide groups as a result of oxygen transfer from DMSO. Half of the sulfide groups in 6 , upon oxidation with H2O2, afforded polymer sulfoxide 7 and polymer sulfone 8 . The solution properties of these polymers were determined via a viscometric technique. The thermal stability of these polymers was determined by thermogravimetric analysis. The inhibition efficiency obtained from gravimetric mass loss, potentiodynamic polarization, and electrochemical impedance spectroscopy techniques agreed well with each other. The corrosion efficiencies increase with increasing concentration of the polymers. At a polymer concentration of 175 μM, the maximum inhibition efficiency of copolymer compounds 6-8 was determined to be 92%, 97%, and 95%, respectively. The synthesized polymer compounds acted as mixed-type inhibitors. Polymer compound 7 adsorbed onto the metal surface via chemisorption and physisorption and obeyed Langmuir, Temkin, and Freundlich adsorption isotherms. Analyses by X-ray photoelectron spectroscopy and scanning electron microscopy-energy-dispersive X-ray spectroscopy indicated that the adsorbed polymers formed a thin film on the metal surface and prevented further corrosive attack.
Research Article
Effect of titanium content on the precipitation behavior of carbon-saturated molten pig iron
Lei-zhang Gao, Tong-xiang Ma, Meng-jun Hu, Zhi-ming Yan, Xue-wei Lü, and  Mei-long Hu
2019, vol. 26, no. 4, pp. 483-492. https://doi.org/10.1007/s12613-019-1755-3
Abstract:
The use of iron ores bearing titanium as a raw material is an effective measure to prevent hearth erosion and prolong the life of a blast furnace. In this research, the effect of titanium content on the precipitation behaviors of high-melting phases of carbon-saturated molten pig iron were studied by confocal scanning laser microscopy. The results showed that, when the titanium content was less than 0.25wt%, Fe3C was precipitated as a single phase from the molten carbon-saturated iron. The growth rate of the precipitated Fe3C crystals was very high, reaching 7387 μm2/s. When the titanium content in the molten pig iron was greater than 0.47wt%, TiC crystals precipitated first. The shape and size of the precipitated TiC crystals did not obviously change. After TiC was precipitated, the fluidity of the molten pig iron worsened. With a decrease in temperature, Fe3C was also precipitated but the growth rate of Fe3C was limited by the presence of the first precipitated TiC phase. The crystal size of the precipitated Fe3C was much smaller than that of pure Fe3C.
Research Article
Effect of cooling rate during quenching on the microstructure and creep property of nickel-based superalloy FGH96
Ye-fei Feng, Xiao-ming Zhou, Jin-wen Zou, and  Gao-feng Tian
2019, vol. 26, no. 4, pp. 493-499. https://doi.org/10.1007/s12613-019-1756-2
Abstract:
The effect of cooling rate during quenching on the microstructure and creep property of nickel-based superalloy FGH96 was investigated. Three groups of samples were quenched continuously with three fixed cooling rates, respectively, then subjected to a creep test under a constant load of 690 MPa at 700℃. Clear differences in size of secondary γ' precipitates, creep properties and substructure of creep-tested samples were observed. The quantitative relationship among cooling rate, the size of secondary γ' precipitates, and steady creep rate was constructed. It was found that with increasing cooling rate, the size of secondary γ' precipitates decreases gradually, showing that the relationship between the size of secondary γ' precipitates and the cooling rate obeys a power law, with an exponent of about -0.6, and the creep rate of steady state follows a good parabola relationship with cooling γ' precipitate size. For 235℃/min, FGH96 alloy exhibited very small steady creep rate. The density of dislocation was low, and the isolated stacking fault was the dominant deformation mechanism. With decreasing cooling rates, the density of dislocation increased remarkably, and deformation microtwinning was the dominant deformation process. Detailed mechanisms for different cooling rate were discussed.
Research Article
Effect of Ti and Al on microstructure and partitioning behavior of alloying elements in Ni-based powder metallurgy superalloys
Yin-long Shao, Jing Xu, Hao Wang, Yi-wen Zhang, Jian Jia, Jian-tao Liu, Hai-liang Huang, Ming Zhang, Zhi-cheng Wang, Hong-fei Zhang, and  Ben-fu Hu
2019, vol. 26, no. 4, pp. 500-506. https://doi.org/10.1007/s12613-019-1757-1
Abstract:
The microstructure and partitioning behaviors of alloying elements in the γ and γ' phases in Ni-based powder metallurgy superalloys with different Ti and Al contents were investigated. The results showed that Ti and Al were mainly enriched in the γ' phase, partially partitioned in the γ matrix, and slightly distributed in the carbides. Different Ti and Al contents in various alloys influenced the composition and amount of MC carbides but did not influence the MC carbides' morphology. With increasing Ti and Al contents, γ + γ' fan-type structures formed at the grain boundary, eventually resulting in a coarsened γ' phase. In addition, the morphology of the secondary γ' phase transformed from nearly spherical to cuboidal. The saturation degrees of Cr, Co, and Mo in the γ matrix were substantially improved with increasing Ti and Al contents.
Research Article
Fine-tuning the ductile-brittle transition temperature of Mg2Si intermetallic compound via Al doping
Ao Li, Xin-peng Zhao, Hai-you Huang, Yuan Ma, Lei Gao, Yan-jing Su, and  Ping Qian
2019, vol. 26, no. 4, pp. 507-515. https://doi.org/10.1007/s12613-019-1758-0
Abstract:
Brittleness is a dominant issue that restricts potential applications of Mg2Si intermetallic compounds (IMC). In this paper, guided by first-principles calculations, we found that Al doping will enhance the ductility of Mg2Si. The underlying mechanism is that Al doping could reduce the electronic exchange effect between Mg and Si atoms, and increase the volume module/shear modulus ratio, both of which are beneficial to the deformation capability of Mg2Si. Experimental investigations were then carried out to verify the calculation results with Al doping contents ranging from Al-free to 10wt%. Results showed that the obtained ductile-brittle transition temperature of the Mg2Si-Al alloy decreased and the corresponding ductility increased. Specifically, the ductile-brittle transition temperature could be reduced by about 100℃. When the content of Al reached 6wt%, α-Al phase started to precipitate, and the ductile-brittle transition temperature of the alloy no longer decreased.
Research Article
Development of non-shrinkable ceramic composites for use in high-power microwave tubes
N. Dandapat and  S. Ghosh
2019, vol. 26, no. 4, pp. 516-522. https://doi.org/10.1007/s12613-019-1759-z
Abstract:
Al2O3-CaO-SiC-based ceramic composites with four different compositions were sintered at 1700℃ for 3 h in an air furnace. The phase analysis, microstructural characterization, and elemental composition determination of the developed composites were performed by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and energy-dispersive X-ray (EDAX) analysis, respectively. The shrinkage, thermal properties, and electrical resistivity of the composites were also studied. The experimental results showed the effects of adding silicon carbide and calcia to alumina on the thermal, electrical, and shrinkage properties of the resultant composites. Among the four investigated ceramic composites, the one composed of 99wt% alumina, 0.5wt% CaO, and 0.5wt% SiC exhibited the best characteristics for use as a potting material in a dispenser cathode of a microwave tube. The material exhibited slight expansion instead of shrinkage during drying or firing. Other properties of the composite powder, such as its thermal properties and electrical resistivity, were comparable to those of a commercial alumina powder.
Research Article
A study of interparticulate strain in a hot-extruded SiCp/2014 Al composite
Ying Hu, Qiu-bao Ou-yang, Lei Yao, Sheng Chen, and  Lan-ting Zhang
2019, vol. 26, no. 4, pp. 523-529. https://doi.org/10.1007/s12613-019-1760-6
Abstract:
We report a correlative study of strain distribution and grain structure in the Al matrix of a hot-extruded SiC particulate-reinforced Al composite (SiCp/2014 Al). Finite element method (FEM) simulation and microstructure characterization indicate that the grain structure of the Al matrix is affected by the interparticulate strain distribution in the matrix during the process. Both electron-backscattered diffraction (EBSD) and selected-area electron diffraction (SAED) indicated localized misorientation in the Al matrix after hot extrusion. Scanning transmission electron microscopy (STEM) revealed fine and recrystallized grains adjacent to the SiC particulate and elongated grains between the particulates. This result is explained in terms of recrystallization under an interparticulate strain distribution during the hot extrusion process.