Search Results (106)

Current electrolytic refining processes for crude solder commonly employ fluosilicic acid (H₂SiF₆) as the electrolyte with bone glue and β-naphthol additives yet suffer from poor electrolyte stability, coarse cathode crystallization, low current efficiency, and high energy consumption, adversely affecting product quality and economic viability. In order to solve these limitations, electrochemical techniques, XRD, SEM, and ICP-OES were used to study the effects of gelatin and sodium lignosulfonate on the deposition overpotential and cathode morphology, as well as the effects of process parameters on current efficiency and energy consumption. A novel approach was developed using an H₂SiF₆ system enhanced by gelatin and sodium lignosulfonate for crude solder refining. After optimization, 120 h electrolysis achieved a current efficiency >97.8%, smooth/dense cathode surface, average cell voltage of 0.24 V, and energy consumption of 98.15 kWh/t. Efficient deposition of 81.2% Sn and 75.2% Pb on the cathode was realized, while >93.3% of Sb, Bi, Ag, Cu, and As were enriched in anode slime to facilitate valuable metal recovery, and >90.6% of In/Al concentrated in the electrolyte enabled effective Sn-Pb impurity separation. This study provides theoretical and technical foundations for advancing sustainable and economical electrolytic refining of crude solder. Full article

Complex antimony pyrochlores Bi_2.7M_0.46Ni_0.70Sb₂O_10+Δ (M = Zn, Mg) were synthesized from oxide precursors, using the solid-state reaction method. For each composition variant, the pyrochlore phase formation process was studied during solid-state synthesis in the range of 500–1050 °C. The influence of zinc and magnesium on the phase formation process was established. The interaction of oxide precursors occurs at a temperature of 600 °C and higher, resulting in the formation of bismuth stibate (Bi₃SbO₇) as a binary impurity phase. Oxide precursors, including bismuth(III) and antimony(III,V) oxides, are fixed in the samples up to 750 °C, at which point the intermediate cubic phase Bi₃M_2/3Sb_7/3O₁₁ (sp. gr. Pn-3, M = Zn, Ni) is formed in the zinc system. Interacting with transition element oxides, it is transformed into pyrochlore. An intermediate phase with the Bi_4.66Ca_1.09VO_10.5 structure (sp. gr. Pnnm) was found in the magnesium system. The unit cell parameter of pyrochlore for two samples has a minimum value at 800 °C, which is associated with the onset of high-temperature synthesis of pyrochlore. The synthesis of phase-pure pyrochlores is confirmed by high-resolution Raman spectroscopy. The data interpretation showed that the cations in Ni/Zn pyrochlore are more likely to be incorporated into bismuth positions than in Ni/Mg pyrochlore. The nickel–magnesium pyrochlore is characterized by a low-porosity microstructure, with grain sizes of up to 3 μm, according to SEM data. Zinc oxide has a sintering effect on ceramics. Therefore, the grain size in ceramics is large and varies from 2 to 7 μm. Full article

The composition of platinum group minerals localized in sulfide droplets from peridotites of the Zhelos intrusion was studied on a scanning electron microscope and on an electron probe microanalyzer. As part of this study, also an analytical approach based on the variation in accelerating voltage, electron beam intensity and probe diameter is considered in order to estimate the X-ray generation region, when analyzing PGM microinclusions comparable in size to the radiation generation region or smaller. Estimates were made of the possibility of reducing the size of the local analysis area when the accelerating voltage was reduced. The influence of the matrix composition on the results of the local analysis of PGM microphases and accuracy of the Pd and Pt content determination was also evaluated. The findings of the experiments conducted allowed for the successful identification of elements belonging to the PGM microphases and the host matrix. This approach enabled the estimation of the precise levels of impurity elements in their composition. Using a scanning electron microscope in the automatic scanning mode for the detection of heavy elements, 10 single and composite grains of three platinum group minerals larger than 5 µm and 22 microphases ranging in size from 0.3 to 4 µm were detected in the sulfide droplets. The large phases are merenskyite, omeiite and michenerite, with merenskyite being predominant. Among the microscopic inclusions were identified Pd-Bi-Te, Os-Ru-As and Rh-As-S phases. The composition of the studied palladium bismuthotelluride samples indicates a formation temperature range of 489–700 °C. Full article

Thin films of bismuth(III) sulfide (Bi₂S₃) on fluorine doped tin oxide (FTO) coated glass slides were successfully formed by the chemical bath deposition (CBD) method. In this work, a new sulfur precursor L-cysteine was used instead of the typical sulfur precursors, such as urea, thiosulfate, or thioacetamide, used for the formation of the Bi₂S₃ films by the CBD method. The synthesized Bi₂S₃ thin film on the FTO substrate was subjected to characterization techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and UV–Visible spectroscopy analysis. An X-ray diffraction analysis showed that, initially, Bi₂S₃ films of an amorphous structure with elemental sulfur impurities were formed on the FTO surface. During the annealing of the samples, amorphous Bi₂S₃ was transformed into its crystalline phase with an average crystallite size of about 22.06 nm. The EDS studies confirmed that some of the sulfur that was not part of the Bi₂S₃ was removed from the films during annealing. The influence of the morphology of Bi₂S₃ films on their optical properties was confirmed by studies in the UV-visible range. Full article

Controlling the stability of colloidal nanoparticles in multicomponent systems is crucial for advancing formulations and separation processes. This study investigates the selective agglomeration approach for binary colloidal mixtures, providing both fundamental insights into stability/agglomeration mechanisms and a scalable separation strategy. First, we established a binary model system comprising gold nanoparticles (Au NPs) and ZnS quantum dots (QDs) to assess interparticle interactions. UV-visible spectroscopy revealed that impurities released from ZnS QDs, particularly thiol-based ligands and unbound Zn ions, triggered the aggregation of Au NPs depending on their surface stabilizers. Functionalization of Au NPs with bis(p-sulfonatophenyl) phenylphosphine (BSPP) significantly enhanced colloidal stability, with unpurified BSPP-functionalized Au NPs exhibiting superior resistance to agglomeration. Building on these insights, we applied selective agglomeration to separate a complex colloidal system consisting of InP/ZnS core–shell QDs and ZnS byproducts, a critical challenge in QD synthesis that is particularly relevant for post-processing of samples that originate from large-scale flow synthesis. By systematically tuning the ethanol concentration as a poor solvent, we successfully achieved composition-dependent fractionation. Optical and spectroscopic analyses confirmed that coarse fractions were enriched in InP/ZnS QDs, while fines fractions mainly contained pure ZnS QDs, with absorption peaks at 605 nm and 290 nm, respectively. Photoluminescence spectra further demonstrated a redshift in the coarse fractions, correlating with an increase in particle size. These results underscore the potential of selective agglomeration as a scalable, post-synthesis classification method, offering a framework for controlling stability and advancing post-synthesis separation strategies in colloidal multicomponent systems. Full article

A topological insulator with large bulk-insulating behavior and high electron mobility of the surface state is needed urgently, not only because it would be a good platform for studying topological surface states but also because it is a prerequisite for potential future applications. In this work, we demonstrated that tin (Sn) or indium (In) dopants could be introduced into a BiSbTeSe₂ single crystal. The impacts of the dopants on the bulk-insulating property and electron mobility of the surface state were systematically investigated by electrical transport measurements. The doped single crystals had the same crystal structure as the pristine BiSbTeSe₂, no impure phase was observed, and all elements were distributed homogeneously. The electrical transport measurements illustrated that slight Sn doping could improve the performance of BiSbTeSe₂ a lot, as the longitudinal resistivity (ρ_xx), bulk carrier density (n_b), and electron mobility of the surface state (μ_s) reached about 11 Ωcm, 7.40 × 10¹⁴ cm⁻³, and 6930 cm²/(Vs), respectively. By comparison, indium doping could also improve the performance of BiSbTeSe₂ with ρ_xx, n_b, and μ_s up to about 13 Ωcm, 1.29 × 10¹⁵ cm⁻³, and 4500 cm²/(Vs), respectively. Our findings suggest that Sn- or indium-doped BiSbTeSe₂ crystals should be good platforms for studying novel topological properties, as well as promising candidates for low-dissipation electron transport, spin electronics, and quantum computing. Full article

In order to study an algorithm that recognizes the state of health (SOH) of a battery rapidly and can be easily integrated into the micro-controller unit (MCU), it is proposed that signal temporal logic (STL) language is employed to describe the discharge curves, because the STL language is a formal language with strict mathematical definitions and the syntax is composed of simple logic, “and”, “or”, and “not”, under the constraints of time and parameter variation ranges, which is realizable and interpretable. Firstly, the drop voltage amplitude, drop time, voltage rebound amplitude, voltage rebound time, starting voltage, and ending voltage of the discharge curve are selected as the features of the STL formula, so the first-level and second-level primitive formulas are constructed to express the voltage of a battery in good health and poor health clearly. Secondly, the impurity measures of the information gain, misclassification gain, Gini gain, and robust extended gain are presented as the objective functions. Thirdly, the interpreter embedded in the MCU can interpret and execute each STL sentence. The voltage of a battery in good health rises slowly and falls slowly, while the voltage of a battery in poor health rises quickly and falls quickly. When the STL describes the discharge curve as “slow down slow up”, the battery is in good health. When the STL describes the discharge curve as “fast down, fast up”, the battery is in poor health. Among the different objective functions, the highest mean accuracy of the STL reaches 87.5%. In terms of the mean runtime, the extended misclassification gain and the extended Gini gain of the first-level primitives are 00851s and 0.0993, respectively. Under the same mean accuracy of 87%, the information gain and Gini gain of the second-level primitives are 0.2593 s and 0.2341 s. Compared with the existing machine learning algorithms, in terms of the mean runtime, the STL algorithm is superior to the CNN-BiLSTM-MHA model, RNN-LSTM-GRU model, and EC-MKRVM model. In terms of the mean accuracy, compared with the highest correct rate of the CNN-BiLSTM-MHA model, that is, 91.7%, the difference is 4%. As a means of quickly detecting whether the battery is in a healthy state, the accuracy difference is negligible, so the STL algorithm is apparently superior in terms of performance and realizability. Full article

The separation of lead from the impurity bismuth remains a significant challenge, with achieving effective separation being a critical bottleneck in the production of high-purity lead via the vacuum gasification method. This study focuses on lead as the primary subject of investigation, conducting both theoretical and experimental research on the auxiliary conversion of lead through vacuum gasification. The calculations of the Gibbs free energy indicate that, within the temperature range of 600 to 610 K, the impurity bismuth reacts completely with calcium and magnesium, resulting in the formation of the compound CaMg₂Bi₂. Under optimal experimental conditions, the bismuth compound CaMg₂Bi₂ is converted into BiCa₂. Notably, BiCa₂ is nonvolatile and remains in the crucible as a residue. The auxiliary calcium is entirely transformed into CaSe and CaTe, leading to a reduction in the calcium content of the volatile substances from 0.5% to 16 ppm. Similarly, the magnesium content in the volatiles decreases from 0.66% to 187 ppm. Ultimately, the bismuth content in the final product is reduced from 6 ppm to 1.4 ppm, achieving a removal rate of 76.6%, while the direct yield of metallic lead reaches 71%. This process effectively facilitates the separation of metallic lead from the bismuth impurities. Full article

The behavior of impurities in cast copper was investigated to simulate production with increased utilization of secondary sources within the framework of a circular economy. The incorporation of impurities, particularly Ni, Sn, and Sb, from recycled Cu may significantly impact the electrorefining process. In this study, commercial anodes were doped with Ni, Sn, and Sb concentrations of 2500–6500 g/t, 300–900 g/t, and 450–950 g/t, respectively. Anode concentrations of Pb and Bi were maintained at 1000 g/t and 350 g/t, respectively. As concentrations were examined at two levels, 860 or 1700 g/t, depending on the commercial anode used to create the doped samples. Electron microscopy with microprobe analysis revealed that the commercial anodes contained three predominant phases: Cu₂O, (Cu,Ag)₂(Se,Te), and a complex oxide phase of Cu, Pb, As, Sb, and/or Bi. Ni, the main impurity, primarily accumulated within the Cu grains, while Sn and Sb tended to form oxidized inclusions. The distribution of Ni in Cu grains was ca. 20% lower in the anodes doped at higher Ni concentrations due to the formation of nickel-bearing inclusions, such as Kupferglimmer and NiO. The doped anodes showed lower quantities of Cu₂O inclusions than the commercial anodes due to the preferential formation of oxides with other impurities, including SnO₂. These findings highlight potential challenges for Cu electrorefining in a circular economy, as Ni, Sb, and Sn may impact the deportment of these impurities to slimes or electrolyte and may cause copper depletion in the refining electrolyte. Full article

A series of Ag-loaded and oxygen vacancy (OV)-containing BiOBr_(OV)/BiOI_0.08 (Ag/BiOBr_(OV)/BiOI_0.08) photocatalysts with varying Ag loading levels were synthesized via the solvothermal–photocatalytic reduction method. As confirmed via optical, photoelectrochemical, and 4-chlorophenol photodegradation experiments, a low Ag loading level significantly enhanced the photogenerated charge carrier (PCC) transfer on the BiOBr_(OV)/BiOI_0.08 semiconductor surface and the performance of Ag/BiOBr_(OV)/BiOI_0.08 photocatalysts, which was attributable to the synergism between the effect of OVs and the localized surface plasmon resonance (LSPR) of Ag nanoparticles. Additionally, BiOBr_(OV)/BiOI heterojunctions facilitated efficient visible-light harvesting and PCC separation. As indicated by finite-difference time-domain (FDTD) simulations and density functional theory (DFT) calculations, the electric field intensity in the “hot spots” generated at the interface between the BiOBr_(OV)/BiOI_0.08 semiconductor and Ag nanoparticles increased by more than eight times, and the presence of OVs and Ag atomic clusters introduced impurity energy levels in the semiconductor bandgap, improving PCC separation and Ag/BiOBr_(OV)/BiOI_0.08 photocatalytic efficiency. However, an increase in silver loading renders the composite metallic, suggesting a reduction in its photocatalytic performance. This work provides new insights for designing highly active visible light catalysts and contributes to the development of more efficient plasmonic catalysts. Full article

With the advancement of high-integration and high-density interconnection in chip manufacturing and packaging, Cu bumping technology in wafer- and panel- level packaging is developed to micrometer-sized structures and pitches to accommodate increased I/O numbers on high-end integrated circuits. Driven by this industrial demand, significant efforts have been dedicated to Cu electroplating techniques for improved pillar shape control and solder joint reliability, which substantially depend on additive formulations and electroplating parameters that regulate the growth morphology, crystal structure, and impurity incorporation in the process of electrodeposition. It is necessary to investigate the effect of an additive on Cu pillar electrodeposition, and to explore the Kirkendall voids formed during the reflowing process, which may result from the additive-induced impurity in the electrodeposited Cu pillars. In this work, a self-synthesized polyquaterntum (PQ) was made out with dual suppressor and leveler effects, and was combined with prototypical accelerator bis- (sodium sulfopropyl)-disulfide (SPS) for patterned Cu pillar electroplating. Then, Sn96.5/Ag3.0/Cu0.5 (SAC305) solder paste were screen printed on electroplated Cu pillars and undergo reflow soldering. Kirkendall voids formed at the joint interfaces were observed and quantified by SEM. Finally, XRD, and EBSD were employed to characterize the microstructure under varying conditions. The results indicate that PQ exhibits significant suppressive and levelled properties with the new structure of both leveler and suppressor. However, its effectiveness is dependent on liquid convection. PQ and SPS work synergistically, influencing the polarization effect in various convective environments. Consequently, uneven adsorption occurs on the surface of the Cu pillars, which results in more Kirkendall voids at the corners than at the center along the Cu pillar surface. Full article

This paper studies the structural parameters and electrophysical properties (dielectric and piezo electric, as well as currents of thermostimulated depolarization) of samples of composition 0.20BiScO₃·0.45PbTiO₃·0.35PbMg_1/3Nb_2/3O₃ (or in short 0.20BS·0.45PT·0.35PMN) obtained by ceramic and melt-hardening methods of synthesis. In the ceramic method, the samples were obtained from the starting oxides by two-stage firing. In the melt method, amorphous precursors were first obtained from heat-treated and non-heat-treated starting oxide mixtures by melting and subsequent quenching under sharply gradient temperature conditions. Samples were obtained after grinding, pressing, and thermal annealing of the synthesized precursors, and four types of samples differing in size and shape of the intermediate precursor particles (crystallites) were obtained. The X-ray phase analysis showed that the predominant phase in the studied samples is the perovskite phase; in both types of samples, up to 5 wt.% of impurity phase with pyrochlore structure was also present. The samples of 0.20BS·0.45PT·0.35PMN exhibit dielectric properties characteristic of relaxor ferroelectrics, and the polarized samples exhibit a pronounced piezo effect with a piezo modulus value of d₃₃~200 pC/N. A comparative analysis of the properties of the samples obtained by different methods has been carried out. The essential advantage of the melt method is that its use allows obtaining varieties of four kinds of ferroelectric relaxors and reduces the time of synthesis of samples by 2–3 times. Full article

The effect of trace Bi impurities on the flow stress, microstructure evolution, and dynamic recrystallization (DRX) of the ultrahigh-purity copper was systematically investigated by a hot compression test at 600 °C. The results show that the peak stress of the ultrahigh-purity copper gradually decreases with increasing Bi content. Trace Bi impurities can refine the microstructure of ultrahigh-purity copper. However, the refinement effect of 50 wt ppm Bi is much more significant than that of 140 wt ppm Bi during the hot deformation. This effect is ascribed to the higher concentration of Bi at GBs, which induces severe GB cracks that reduces the driving force for the nucleation of DRX grains. In addition, the introduction of Bi inhibits the DRX of the ultrahigh-purity copper and transforms its DRX process from the discontinuous dynamic recrystallization (DDRX) to the coexistence of DDRX and continuous dynamic recrystallization (CDRX) mechanisms. Full article

This study investigates the application of the vertical zone refining process to produce ultra-high-purity tin. Computational fluid dynamics (CFD) simulations were conducted using an Sn-1 wt.%Bi binary alloy to assess the effects of two key parameters—heater temperature and pulling rate—on Bi impurity segregation. The simulations revealed a dynamic evolution in molten zone height, characterized by an initial rapid rise, followed by a gradual increase and ending with a sharp decline. Despite these fluctuations, the lower solid–liquid interface consistently remained slightly convex. After nine zone passes, impurities accumulated at the top of the sample, with dual vortices forming a rhombus- or gate-shaped negative segregation zone. The simulations demonstrated that lower heater temperatures and slower pulling rates enhanced impurity segregation efficiency. Based on these results, experiments were performed using 6N-grade tin as the starting material. Glow discharge mass spectrometry (GDMS) analysis showed that the effective partition coefficients (k_eff) for impurities such as Ag, Pb, Co, Al, Bi, Cu, Fe, and Ni were significantly less than 1, while As was slightly below but very close to 1, and Sb was above 1. Under optimal conditions—405 °C heater temperature and a pulling rate of 5 μm/s—over 60% of impurities were removed after nine zone passes, approaching 6N9-grade purity. These findings provide valuable insights into optimizing the vertical zone refining process and demonstrate its potential for achieving 7N-grade ultra-high-purity tin. Full article

Here, by using angle-resolved photoemission spectroscopy, we showed that Bi_2−xCr_xSe₃ single crystals have a distinctly well-defined band structure with a large bulk band gap and undistorted topological surface states. These spectral features are unlike their thin film forms in which a large nonmagnetic gap with a distorted band structure was reported. We further provide laser-based high resolution photoemission data which reveal a Dirac point gap even in the pristine sample. The gap becomes more pronounced with Cr doping into the bulk of Bi₂Se₃. These observations show that the Dirac point can be modified by the magnetic impurities as well as the light source. Full article