High Purity Tin Research Articles

The effect of metal quantity on the temperature plateau time

In recent years, the miniaturization and portability of fixed-point containers are becoming a trend. This paper introduces a sealed small container, which is filled with 99.9999% high purity tin, with related reproducing experiments carried out in a Fluke dry-well furnace. A precision platinum resistance thermometer with 3.6 mm diameter is put into the bottom of the temperature well for running several tests. The differences in temperature plateau time are compared between the 40 g case and the 16 g case. The data shows that the reduction of the tin filling can significantly shorten the temperature plateau time.

Purification of High-Purity Tin via Vertical Zone Refining

The present investigation delves into the potential of vertical zone refining as an effective purification technique for achieving high-purity tin (Sn) metal. The utilization of vertical zone refining offers distinct advantages over traditional horizontal zone refining, as it allows for enhanced control over the molten zone and solid–liquid interface, ultimately leading to superior impurity separation efficiency. The present study reveals that the solute partition coefficients (k0) of various impurity elements, such as Zn, Ag, Al, Mg, Ca, Ni, In, Co, Cu, As, Pb, Fe, and Bi, during the vertical zone refining process consistently demonstrate values below one. Notably, the partition coefficient of Sb deviates slightly from the others, being greater than one but approaching one. The authors achieve exceptional levels of purity in both the bottom and middle regions of the rod by subjecting the Sn melt to nine passes of vertical zone refining at a heating temperature of 405 °C and a downward pulling rate of 10 µm/s, resulting in purities exceeding 6N4. Furthermore, by evaluating the effective partition coefficients (keff), it was determined that impurity elements, such as Cu and Bi, closely approach their equilibrium partition coefficients, reaching values of approximately 0.492 and 0.327, respectively. To further enhance the purity of Sn metal and maximize product yield, we propose the utilization of electrolytic refining and vacuum distillation, with particular emphasis on the efficient separation of five specific elements, including Cu, Fe, As, Pb, and Sb. By elucidating these findings, this study not only contributes valuable insights into the efficacy of vertical zone refining as a purification technique for high-purity tin metal, but also offers important recommendations for refining strategies and impurity element separation.

Characteristics of tin oxide nanoparticles produced by pulsed laser ablation technique in various concentrations of chitosan liquid and their potential application as an antibacterial agent

Tin oxide nanoparticles (SnO2 NPs) have become a potential candidate as an antibacterial agent for gram-negative and gram-positive bacteria. In this present work, SnO2 NPs have been successfully synthesized in the chitosan liquid medium by using the pulse laser ablation method utilizing quite low energy Nd:YAG laser (30 mJ). The produced tin oxide nanoparticles were then applied as an antibacterial agent for gram-negative and gram-positive bacteria. Experimentally, a pulse Nd:YAG laser beam is irradiated and focused on the surface of a high-purity tin metal plate placed at the bottom of the Petri dish that is filled with chitosan liquid medium. The effect of chitosan concentrations (0.05%, 0.1%, and 0.2%) on the characteristics of produced SnO2 NPs was examined. The higher concentration of chitosan (0.2%) gains the smallest diameter size (15.05 nm) and lowest concentrations of produced tin oxide nanoparticles. The application of produced SnO2 NPs as the antibacterial agent was demonstrated using gram-negative (Escherichia coli) and gram-positive (Bacillus subtilis) utilizing disk diffusion technique. The result certified that increment of the SnO2 NPs concentrations (100, 125, and 150 ppm) increases the diameter of inhibition zone (DIZ) both for E coli and B subtilis bacteria, which approve that the produced tin oxide nanoparticles can effectively be used as antibacterial agents for both gram-negative and gram-positive bacteria.

Preparation of High-Purity Tin Dichloride

Preparation of High-Purity Tin Dichloride

Synthesis of Tin Oxide Nanoparticles by Pulsed Laser Ablation Method Using Low-Energy Nd: YAG Laser as an Antibacterial Agent

Tin oxide nanoparticles (SnNPs) are very useful to be employed as an antibacterial agent for both gram-positive and gram-negative bacteria. In this present work, the synthesis of SnNPs was successfully carried out using the neodymium yttrium aluminum garnet (Nd:YAG) laser with a wavelength of 1064 nm, pulse duration of 7 ns, and a laser frequency of 10 Hz. Experimentally, a pulse Nd:YAG laser was directed and focused on a high-purity tin (Sn) metal, immersed in various liquid media including pure water and ethylene glycol. A brownish colloidal colour was produced both in pure water and ethylene glycol liquid media. Characterizations of tin oxide nanoparticles were made using UV-Vis, EDX, FTIR, and TEM. UV-Vis characterization produced absorbance values in pure water and ethylene glycol media of 1.314 a.u. and 1.119 a.u., respectively. TEM images show that the shape of tin oxide nanoparticles produced is spherical. Measurement of nanoparticle size distribution was made using image-J software and the average diameter of nano-size in the ethylene glycol medium is 12.55 nm, which is smaller than the size in the pure water of 19.98 nm. The EDX spectrum analysis results show that there are only Sn and O atoms in colloidal tin oxide nanoparticles (SnNPs). FTIR results show the formation of tin oxide (SnO2) spectrum at the wavenumber of 629.03 cm-1. The produced colloidal SnNPs were then applied as an antibacterial agent of E. coli using the disk diffusion method. Results certified that various concentrations of SnNPs of 10 ppm, 20 ppm, and 30 ppm gain the diameter of inhibition zone (DIZ) in sequence 6.50 mm, 6.75 mm, and 9.50 mm. Based on these experimental results, it shows that the higher the concentration of SnNPs given, the greater the ability to degrade and inhibit bacteria.

Structure and Mechanical Properties of Bimetal Nb/Cu Rods for Production of Nb3Sn Superconductors

To construct magnetic systems in modern high-energy physics projects, such as creation of the Future Circular Collider (FCC) and modernization of the Large Hadron Collider (HL-LHC), Nb3Sn superconductors with a high level of electrophysical properties, above all being a high current carrying capacity, are requisite. Such multifilament Nb3Sn superconductors are obtained by the technique of internal feeding of tin (IFT), consisting in deformation of a composite including high-purity niobium, copper, and tin to make a wire smaller less than 1 mm in diameter. The presence of such components as tin-based alloys or pure tin with Tm = 232°C in the composite wire composition precludes the possibility of Nb recrystallization annealing, which imposes strict requirements on the Nb mechanical properties, which determine the Nb capability for plastic deformation. In the study, the influence of the design and conditions of creating bimetal Nb/Cu rods on the grain structure of niobium and the state of the boundary between it and a copper sheath is discussed. The mechanical properties of rods at different steps of their fabrication are investigated. The results will be applied in development of the technological conditions of manufacture of Nb3Sn superconductors by the IFT technique.

Field effect transistor photodetector based on two dimensional SnSe<sub>2</sub>

Two dimensional materials have been attracting intensive interest due to their unique physical and optoelectronic properties. As an emerging two dimensional materials, SnSe<sub>2</sub> have shown a considerable potential for next-generation electronic and optoelectronic. Herein, SnSe<sub>2</sub> bulk crystals have been prepared by a chemical vapour transport method with high purity tin and selenium powder as precursors. Then SnSe<sub>2</sub> multilayers has been successfully prepared by a micromechanical exfoliation method from the SnSe<sub>2</sub> bulk crystals. The phase structures and elemental composition of the bulk crystal are investigated using an X-Ray diffractometer, an X-ray photoelectrons spectrometer and a Raman spectrometer. And the morphologies are observed using an optical microscope, an atomic force microscope and a transmission electron microscope. The measurement results show that the SnSe<sub>2</sub> bulks are single crystals with a high crystallization and purity. The SnSe<sub>2</sub> multilayers have a size of 25–35 μm and a thickness of 1.4 nm. To detect the electronic and photoresponse characteristics of the SnSe<sub>2</sub> multilayers, a field effect transistor based on such SnSe<sub>2</sub> are fabricated via a photolithographic-pattern-transfer method. The transistor has a smooth surface without wrinkles and bubbles, and also has a good contact with Au electrodes. The transistor shows a linear output characteristic and an obvious rectification. The on/off ratio of the device is 47.9 and the electron mobility is 0.25 cm<sup>2</sup>·V<sup>–1</sup>·s<sup>–1</sup>. As a photodetector, the field effect transistor exhibits obvious photoresponse to three visible lights with the wavelengths of 405, 532, and 650 nm. As the lasers are turned on and the device is under illuminations of three visible lights, the current increase rapidly to a saturation state. Then as the lasers are switched off, the current decrease and recover to the original state. The drain-source current can alternate between high and low states rapidly and reversibly, which demonstrates photoresponse characteristics of the devices are stable and sensible. Notably, it shows a strongest response to the 405 nm light at an intensity of 5.4 mW/cm<sup>2</sup> with a high responsivity of 19.83 A/W, a good external quantum efficiency of 6.07 × 10<sup>3</sup>%, a normalized detectivity of 4.23 × 10<sup>10</sup> Jones, and a fast response time of 23.8 ms. The results of this work demonstrate that layered SnSe<sub>2</sub> can be a suitable and excellent candidate for visible light photodetector and has a huge potential for high-performance optoelectronic devices.

Preparation of High-Purity Tin by Zone Melting

High-purity tin is widely used in advanced technologies such as aerospace, electronic information, and nuclear industry. It has become a key material supporting the development of human science and technology innovation. However, there are few studies on the preparation methods of high purity tin. A novel technique was developed to purify 99.99682% tin by zone refining in an argon atmosphere. The impacts of zone melting conditions, such as the segregation coefficient, zone melting rate, and the number of zone melting passes, on the purity of refined tin were experimentally studied. The results showed that the segregation coefficients of Ag, Al, As, Bi, Ca, Cu, Fe, Ni, Pb, Au, Co, and Zn were less than 1, and the segregation coefficient of Sb was greater than but close to 1. Zone melting rates had an obvious effect on zone refining, while the number of passes had little effect. The 99.99682% purity tin was refined into 99.99906% purity tin under the optimized conditions at a zone melting rate of 0.6 mm/min and after 10 cycles of zone melting and cooling.

Preparation and study of morphology of mesoporous anodic films grown on tin foil

Mesoporous anodic layers were obtained on high-purity tin foils in electrolyte of two types: 0.3 M oxalic acid and 1 M NaOH in various anodizing modes. It was demonstrated that in both cases at low voltages below 4 V barrier films form. In acidic electrolyte the formation of tin (II) oxalate was observed whereas in basic electrolytes SnO2·nH2O seems to be formed.At intermediate voltage values from 4 to 8 V mesoporous films may be obtained with average size of pores of 20–40 nm, mesopores are rather uniformly distributed along the surface. It was found that in contrast to alumina anode films no linear dependency between pore diameter and voltage was observed at anodizing of tin foil. At voltages above 8 V and/or long-term anodization the film cracks and the film split to separate islands.

Carbothermal reduction of oxidized tin and recovery of deep supercool

Deep supercooling of tin is a characteristic sign of a high-purity sample having fewer nucleation sites. However, due to the risk of oxidation during the cell fabrication (especially during the initial sample filling process), oxidized tin can be present in the sample, which manifests itself as a nucleation agent and significantly affects the realization of the freezing temperature of tin. In this work, the effect of the oxidation of high-purity tin (nominally 99.9999% pure) and an effective means of reducing the oxidized sample were investigated. We fabricated an open-type tin freezing point cell using 1.15 kg of high purity tin shot, which was poured into the crucible in air, giving rise to a high risk of oxidation. The oxidized tin sample showed abnormally small supercools of about 0.1 °C which were caused by additional nucleation sites introduced by the oxidation. The oxidized sample also exhibited a melting temperature inversion over the entire range of the melting with a temperature depression of about 1.9 mK. The oxidized sample was carbothermally reduced by melting the sample in its graphite crucible and holding at a temperature of 750 °C for a total duration of 365 h. The carbothermal reduction of the oxidized sample caused the satisfactory recovery of the deep supercool, and the recovered supercool was about 10.6 °C after about 100 h of reduction, and 10.7 °C after 365 h of reduction. At the end of the reduction process, the melting curve inversion was significantly alleviated, having 0.1 mK temperature depression over less than 10% of the melting range. Importantly, the carbothermal reduction at 750 °C was found to be an effective means of removing the oxide nucleation sites and of recovering the characteristic deep supercool of tin.

Study on the Performance of Nano-Titanium Nitride-Coated Stainless Steel Electrodes in Electro-Fenton Systems.

The electro-Fenton (EF) process is a type of electrochemical oxidation process; ·OH radicals are generated on the cathode using electricity and decolorize dye wastewaters. Most studies on EF systems in the past have focused on the operating parameters of this process. In recent years, the influence of electrode performance on the EF process has begun to receive more attention. In this study, direct nitridation was used to prepare titanium nitride powders, which were thereafter coated on an SUS304 stainless steel substrate. The performance of this system in the treatment of rhodamine B dye wastewaters via the EF process was investigated. The experimental methods used in this work include: (1) scanning electron microscopy (SEM); (2) X-ray diffraction (XRD); (3) electrochemical Tafel curves; (4) linear sweep voltammetry (LSV); (5) and cyclic voltammetry (CV). It was shown that high-purity TiN can be formed at nitriding temperatures above 900 °C, and the strength of the (111) crystal plane increases with the increase in nitriding temperature; the TiN coating effectively activates the reactive surface of the electrode owing to its porous structure. In terms of corrosion resistance, the corrosion potential and corrosion current of the TiN 1000 °C/SUS304 electrode were 116.94 mV and 205 nA/cm2, respectively, and the coating had a coating porosity of 0.89 × 10−7. As compared with SUS304 stainless steel, the TiN 1000 °C/SUS304 composite electrode had a significantly greater degree of corrosion resistance and exhibited higher redox activity in LSV tests. This composite electrode could achieve a decolorization rate of 49.86% after 30 min, and 94.46% after 120 min. In summary, the TiN 1000 °C/SUS304 composite electrode is very stable and has excellent decolorization efficacy in the EF process. Our findings will serve as a useful reference for future studies on EF electrodes.

Vacancy-like defects in nanocrystalline SnO2: influence of the annealing treatment under different atmospheres

The study of electronic and chemical properties of semiconductor oxides is motivated by their several applications. In particular, tin oxide is widely used as a solid state gas sensor material. In this regard, the defect structure has been proposed to be crucial in determining the resulting film conductivity and then its sensitivity. Here, the characteristics of vacancy-like defects in nanocrystalline commercial high-purity tin oxide powders and the influence of the annealing treatment under different atmospheres are presented. Specifically, SnO2 nanopowders were annealed at 330 °C under three different types of atmospheres: inert (vacuum), oxidative (oxygen) and reductive (hydrogen). The obtained experimental results are discussed in terms of the vacancy-like defects detected, shedding light to the basic conduction mechanisms, which are responsible for gas detection.

주석도금폐액으로부터 이온교환 및 사이클론 전해채취를 이용한 고순도 주석의 회수

주석도금폐액으로부터 이온교환 및 사이클론 전해채취를 이용한 고순도 주석의 회수

Investigation of the Influence of Annealing Temperature on the Morphology and Growth Kinetic of Ni3Sn4 in the Ni-Sn-Solder System

The reaction between high purity nickel (99.999%) and high purity tin (99.999%) was investigated in the temperature range of 232℃ - 330℃, at short periods of annealing (1 - 60 s). The reaction kinetic was studied using cross-sectional scanning electron microscope (SEM) images. The intermetallic compound (IMC) growth was analyzed using the empirical power law and a time dependence in the range of 0.26 to 0.33 was found. The morphology of the IMC was investigated by SEM in the temperature range of 235℃ - 290℃, at annealing periods of 10 s, 30 s, and 60 s by selectively etching away the remaining elementary tin. The exposed IMC displays a change in morphology with increasing annealing temperature, demonstrating that the growth velocity of certain crystallographic orientations of the IMC is strongly influenced by the annealing temperature. Additionally, coarsening and crumbling of the IMC grains is observed, and will be discussed with respect to the responsible mechanisms.

Uncertainty assessment of enthalpy of fusion measurements performed by using an improved Calvet calorimeter

The French National Metrology Institute LNE-LCM has developed a new in situ electrical calibration system which is integrated into a heat flux Calvet calorimeter in order to perform accurate and reliable measurements of enthalpy of fusion from 23 °C to 1000 °C. The measurement procedure consists in putting a sample inside the calibration system and in performing the heat calibration of the calorimeter by electrical substitution (Joule effect) before and after the enthalpy of fusion measurement during the same heating run. This procedure directly takes into account the temperature dependence of the calibration factor (sensitivity) and keeps the calibration and measurement experimental conditions strictly the same. Uncertainties of the enthalpy of fusion measurements, performed by using this facility and procedure, have been assessed according to the ‘guide to the expression of uncertainty in measurement’. The detailed uncertainty budgets are presented here in the case of three pure metallic materials (indium, tin and silver). The relative expanded uncertainty (k = 2) of the enthalpy of fusion measurement is estimated to be less than 0.4% for the high purity indium and tin, and less than 1% in the case of silver.

Construction of Home-Made Tin Fixed-Point Cell at TUBITAK UME

TUBITAK UME Temperature Laboratory initiated a new study which focuses on the construction of a tin freezing-point cell as a primary temperature standard. The design is an open-cell type similar to the National Institute of Standards and Technology design. With this aim, a brand new vacuum and filling line employing an oil diffusion pump and two cold traps (liquid nitrogen and dry ice) was set-up. The graphite parts (crucible, thermometer well, etc.) have been baked at high temperature under vacuum. Each cell was filled with approximately 1 kg of high-purity tin (99.9999 %) in a three-zone furnace. Then several melting and freezing curves were obtained to assess the quality of the home-made cell, and also the new cell was compared with the existing reference cell of the laboratory. The results obtained are very close to the reference cell of UME, indicating that the method used for fabrication was promising and satisfactory and also seems to meet the requirements to have a primary level temperature standard.

주석도금폐액으로부터 이온교환수지를 이용한 주석 회수

Abstract In order to recover tin from the waste tin plating solution, we used the ion exchange method using three types of ion exchangeresins. The ion exchange resin with tertiary functional group(Lewatit TP 272) has not adsorption ratio of tin. The ion exchangeresin with iminodiacetic functional group(Lewatit TP 207) has high adsorption ratio of tin, but impurity content in the recoveredtin solution was relatively high. Whereas, in case of the ion exchange resin with functional group of ethylhexyl-phos-phate(Lewatit VP OC 1026), adsorption ratio of tin was less than that of Lewatit TP 207. However, it was possible to removeimpurities in the recovered tin solution by controlling the pH of the solution. High purity tin solution can be recovered by remov-ing the organic materials with water washing process. Key words : Ion exchange resin, tin, recovery, waste plating solution 1. 서론 주석은 LED TV, 합금재료, 도금재료, 전기 및 전자제품의 필수 소재로 사용되는 금속으로 차세대 핵심소재로 부각되면서 수요도 꾸준히 증가하고 있다. 그러나주석 자원의 경우 동남아 등 일부 국가에만 편중되어

Structural and optical characterization of reactive evaporated tin diselenide thin films

Tin diselenide thin films with thickness of the order of 300 nm are deposited on glass substrate at a substrate temperature of 523±5 K and pressure of 10−5 mbar using reactive evaporation, a variant of Gunther's three temperature method. High purity tin (99.999%) and selenium (99.99%) were used as the elemental starting materials. The deposited film is characterized structurally using X-Ray Diffraction (XRD). The structural parameters such as lattice constant, particle size, dislocation density, number of crystallites per unit area and strain in the film are evaluated. Optical absorption spectrum of the film is analysed using UV-Vis- NIR Spectrophotometer.

Prospect for SnmSb2nS3n+m (n = 1, m = 1, 2, 3) sulfosalt compounds

In an effort to prepare thin films of novel semiconductor materials that contain only cost effective, abundant, and relatively less-toxic materials, SnmSb2nS3n+m (n = 1, m = 1, 2, 3) ingots sulfosalts materials were successfully grown via horizontal Bridgman method using high-purity tin, antimony and sulphur elements. Crushed powders of these ingots were used as raw materials for the vacuum thermal evaporation. So, SnSb2S4, Sn2Sb2S5 and Sn3Sb2S6 thin films were deposited by single source vacuum evaporation onto non-heated glass substrates. Their structure, composition and morphology are studied by X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), atomic force microscopy, Raman scattering and optical measurements. XRD patterns show that polycrystalline SnmSb2nS3n+m thin films were obtained without heating the substrates. Optical measurements indicated a direct band gap in the range 1.47–1.63 eV and a strong absorption coefficient between 104 and 2.105 cm−1.

Effect of Equal Channel Angular Pressing on Different Face Center Cubic (FCC) Metals

Equal channel angle pressing (ECAP) of commercial purity aluminum (1050), oxygen free high conductivity copper (OFHC Cu) and high purity tin (99,99% Sn) were conducted using C processing route. The variation of microstructure, of micro-Vickers hardness and of macroscopic material parameters with number of pressings was documented up to ten passes. Tensile tests were used to evaluate post ECAP deformation response. Optical microscope was used to obtain statistical information on the microstructure developed during ECAP. The present results showed that, as it can be found in the literature, first ECAP pass has resulted in enhancement of mechanical properties. Further ECAP processing, as original observation, has resulted in slight improvement and after ~7 pressing decreasing of hardness can be observed. The true stress–strain curve for ECAP-ed specimens tested under tension showed the evolution of macroscopic material properties is similar. This behavior can be connected with the deformation microstructure of the specimen, grain deformation and fragmentation.