- Reduction of tin oxide by hydrogen radicals
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The effect of a reducing hydrogen ambient on textured tin oxide thin films on glass substrates has been investigated. Hydrogen treatments were done at 230 and 430 °C by hot wire (HW) and rf plasma-decomposed hydrogen with pure H2 as source gas. By these treatments the possible reduction of the substrate during the deposition of a-Si:H for solar cells is simulated. Ion beam techniques revealed that the exposure to HW-decomposed H-radicals leads to the formation of a tin-rich surface layer of 40 nm in 1 min at both 230 and at 430 °C. The loss of oxygen is higher for the high-temperature treatment. The optical transmission at a wavelength of 800 nm is reduced from 80% to less than 20%, while the sheet resistance increases from 6 to 8 Ω/□. At both temperatures the reduction of fluorine-doped tin oxide (FTO) by a HW-treatment occurs faster than by rf plasma-decomposed H. The H radical concentration, which is higher for the HW-decomposed hydrogen as compared to rf plasma-decomposed hydrogen, is the most important factor in determining the rate of the reduction process. For short exposures to H radicals, the transparency and conductivity of the tin oxide may be completely restored by means of reoxidation in air at 400 °C. In contrast, prolonged exposure to H-radicals induces irreversible loss of transparency and conductivity, concomitant with formation of granule-like particles of metallic tin on the surface. A thin plasma-deposited a-Si:H-layer was found to effectively protect the FTO-layer against reduction due to HW-generated H-radicals.
- Wallinga,Arnoldbik,Vredenberg,Schropp,Van Der Weg
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- Bimodal microstructure and reaction mechanism of Ti2SnC synthesized by a high-temperature reaction using Ti/Sn/C and Ti/Sn/TiC powder compacts
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High purity of titanium tin carbide (Ti2SnC) powder was fabricated by pressureless sintering two types of mixtures of Ti/Sn/C and Ti/Sn/TiC powders under different conditions. A bimodal microstructure of Ti2SnC with plate-like and rod-like forms was first observed, which is determined by the grain growth rate in different planes, the C particle's size, and the growth environment. Based on the microstructure observation, a reaction model was proposed to understand the reaction mechanism for the formation of Ti2SnC. Further investigation of the thermal stability of Ti2SnC demonstrates that Ti2SnC decomposes to TiC and Sn in vacuum atmosphere at 1250 C.
- Li, Shi-Bo,Bei, Guo-Ping,Zhai, Hong-Xiang,Zhou, Yang
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- SrSn4: A Superconducting Stannide with Localized and Delocalized Bond Character
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The title compound is the tin-richest phase in the system Sr-Sn and is obtained by stoichiometric combination of the elements, SrSn4 peritecticly decomposes under formation of SrSn3 and Sn at 340 °C. The structure determined from a single crystal shows a new structure type with a novel structure motive in tin chemistry. It can be described by a corrugated, distorted quadratic net of tin atoms as the only building unit. The nets intersect at common Sn atoms, and the resulting channels host the Sr atoms, The structure can alternatively be described as an intergrowth structure of the AlB2-type and W-type. The atoms that are connected by the two shortest Sn-Sn distances (2,900 and 3.044 A) form a two-dimensional net consisting of hexagons of tin atoms. The hexagons have boat conformation in contrast to the rather similar α-As structure type, where hexagons have a chair conformation. Further tin atoms connect the two-dimensional net of Sn hexagons. Temperature-dependent magnetic susceptibility measurements show that SrSn4 is superconducting with Tc = 4.8 K at 10 G. LMTO band structure and density of states calculations verify the metallic behavior of SrSn4. An analysis of the electronic structure with the help of the electron localization function (ELF) shows that localized covalent bonds beside delocalized bonds coexist in SrSn4.
- Hoffmann, Stefan,Faessler, Thomas F.
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- Electrochemical nitriding of Sn in LiCl-KCl-Li3N systems
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Electrochemical nitriding of a liquid phase tin metal has experimentally been confirmed by using the oxidation of nitride ions in molten LiCl-KCl-Li 3N melts according to the following reactions:N3-=Nads+3e-Nads+Sn= SnNx From the XPS analysis, N 1s signal and Sn 3d signals are observed, which corresponds to the formation of SnNx, after conducting argon ion sputtering for 1000 s. This showed that a thick and stable nitride film was formed by electrochemical nitriding.
- Goto, Takuya,Ito, Yasuhiko
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- Preparation and characterization of three-dimensional tin thin-film anode with good cycle performance
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Three-dimensional tin thin-film anode was prepared by electroless plating tin onto three-dimensional (3D) copper foam (which served as current collector), and characterized physically by SEM, EDS and XRD. Its electrochemical property and mechanism were studied by charge-discharge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The SEM and EDS results indicated that tin film with 500 nm thickness was formed over the whole surface of copper branches. The XRD results suggested that a new phase of Cu6Sn5 was formed between copper and tin. Besides the tin microflake structure of 500 nm thickness, the interaction effects of the copper foam and Cu6Sn5 phase formed between copper and tin resulted in good cycle performance with first discharge capacity of 737 mAh g-1, 97% capacity retention after 20 cycles and still 84% after 40 cycles.
- Du, Zhijia,Zhang, Shichao,Jiang, Tao,Bai, Zhiming
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- Thermolysis specifics of Tin(IV) and Tin(II) complex derivatives: Thermolysis of (Acac)2SnX2 (X = Cl, N3), (CO)5MSnCl2(thf) (M = Cr, Mo, W), (CO) 5MSn(Acac)2, (CO)5MSn
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Differential scanning calorimetry and thermogravimetry are used to study the thermolysis of following complexes: (Acac)2Sn(N3)Cl (1); (Acac)2SnCl2 (2); (CO)5MSn(Acac) 2 with M = Cr (3) or W
- Dobrokhotova,Koroteev,Novotortsev,Egorov,Nefedov
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- Development of lead free pulse electrodeposited tin based composite solder coating reinforced with ex situ cerium oxide nanoparticles
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Pure Sn and Sn-CeO2 nanocomposite films have been pulse electrodeposited from an aqueous electrolyte containing stannous chloride (SnCl2-2H2O) and triammonium citrate (C6H 17N3O7). The codeposition is achieved by adding different amounts of ball milled CeO2 nanopowders (1-30 g/L) with a mean particle size of ～30 nm to the electrolyte. Microstructural characterizations have been carried out by X-ray diffraction analysis, scanning electron microscopy coupled with an energy dispersive spectroscopy, and transmission electron microscopy. The microstructural observations show that a uniform microstructure is obtained at a concentration of ～6 wt% CeO 2 in the deposits corresponding to 15 g/L CeO2 in electrolyte. Thus, incorporation of an optimum amount of CeO2 in a composite provides better mechanical, and wear and friction properties, without sacrificing the electrical resistivity significantly.
- Sharma, Ashutosh,Bhattacharya, Sumit,Das, Siddhartha,Fecht,Das, Karabi
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- ELECTRODEPOSITION OF TIN ONTO A WELL-DEFINED Pt(111) SURFACE FROM AQUEOUS HBr SOLUTIONS: STUDIES BY LEED AND AUGER ELECTRON SPECTROSCOPY.
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The authors report on instance in which the energetic driving force for electrosorption, in this case the substantial affinity of tin-oxygen monolayers for the Pt surface, was sufficient to cause spontaneous deposition of monolayer quantities of material upon immersion (of Pt into Sn(II) solutions) at open circuit. Since the electrodeposition of Sn species occurred without flow of current in the external circuit, the deposited species were detected, identified, and quantitated by Auger electron spectroscopy.
- Stickney,Schardt,Stern,Wieckowski,Hubbard
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- Electrodeposited tin coating as negative electrode material for lithium-ion battery in room temperature molten salt
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A new room temperature molten salt (RTMS) [1-methyl-3-ethylimidazolium/AlCl3/SnCl2 (3:2:0.5)] was developed for depositing tin on a copper electrode. Different tin crystallites were deposited at different temperatures, giving widely different performances of the assembled lithium cell [Sn (Cu)/LiCl buffered MEICl-AlCl3 RTMS/lithium]. Tin film deposited at 50°C or higher gave a more desirable crystal structure and an improved performance than films obtained at lower temperatures. Both cyclic voltammetry and galvanostatic cycling show the formation of three major lithium-tin alloy phases corresponding to the phase transition of LiSn/Li7Sn3, Li13Sn5/Li7Sn2, and Li7Sn2/Li22Sn5. Increases in the charging and discharging capacities were found with the deposition of higher lithium-rich tin alloys, though at the degradation of the irreversible capacity at the first cycle. The discharging capacity decreased rapidly, producing loose, expanded, and irregular crystallites upon cycling at a high current density (cd) (1.0 mA/cm2). However, an average capacity of 140 mAh/g, coulombic efficiency around 85%, and more than 200 cycles were obtained at a low cd (0.4 mA/cm2). The improvement is attributed to the deposition of small and regular tin crystallites that allows reversible insertion and removal of lithium from a more stable crystal structure without a significant volume change during cycling.
- Fung,Zhu
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- Amorphous Sn/Crystalline SnS2 Nanosheets via In Situ Electrochemical Reduction Methodology for Highly Efficient Ambient N2 Fixation
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Electrochemical nitrogen reduction reaction (NRR) as a new strategy for synthesizing ammonia has attracted ever-growing attention, due to its renewability, flexibility, and sustainability. However, the lack of efficient electrocatalysts has hampered the development of such reactions. Herein, a series of amorphous Sn/crystalline SnS2 (Sn/SnS2) nanosheets by an L-cysteine-based hydrothermal process, followed by in situ electrochemical reduction, are synthesized. The amount of reduced amorphous Sn can be adjusted by selecting electrolytes with different pH values. The optimized Sn/SnS2 catalyst can achieve a high ammonia yield of 23.8 μg h?1 mg?1, outperforming most reported noble-metal NRR electrocatalysts. According to the electrochemical tests, the conversion of SnS2 to an amorphous Sn phase leads to the substantial increase of its catalytic activity, while the amorphous Sn is identified as the active phase. These results provide a guideline for a rational design of low-cost and highly active Sn-based catalysts thus paving a wider path for NRR.
- Li, Pengxiang,Fu, Wenzhi,Zhuang, Peiyuan,Cao, Yudong,Tang, Can,Watson, Angelica Blake,Dong, Pei,Shen, Jianfeng,Ye, Mingxin
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- Stabilization of a dialkylstannylene by unusual B-H...Sn γ-agostic-type interactions. A structural, spectroscopic, and DFT study
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The reaction between SnCl2 and the lithium salt [[{nPr 2P(BH3)}(Me3Si)CCH2]Li(THF) 2]2 yields the cyclic dialkylstannylene [{nPr 2P(BH3)}(Me3Si)CCH2]2Sn (6) as a 1:1 mixture of rac and meso diastereomers. Fractional crystallization from n-hexane gives samples of pure rac-6 and meso-6 which have been studied by X-ray crystallography, UV/visible, infrared, and multi-element NMR spectroscopy. In the solid state, rac-6 exhibits two short agostic-type B-H...Sn contacts, one to each BH3 group, whereas meso-6, in which both BH3 groups lie on the same side of the heterocycle, exhibits a single B-H...Sn contact. Multi-element and variable-temperature NMR spectroscopy suggests that these contacts persist in solution, resulting in unusual 119Sn chemical shifts of 587 and 787 ppm for the rac and meso diastereomers, respectively, significantly upfield in comparison to other dialkylstannylenes. Variable-temperature 1H, 31P{ 1H}, and 11B{1H} NMR studies reveal dynamic equilibria for the meso diastereomer involving competitive binding of the two BH3 groups to the electron-deficient tin center and restricted rotation about the P-C bond of the free phosphine-borane group. DFT studies confirm that the B-H...Sn contacts are an integral part of the structures; the HOMO and LUMO of both stereoisomers are comprised of an orbital of essentially 5p character on tin and an orbital of predominantly 5p character on tin perpendicular to the plane of the heterocycle, respectively. There is significant donation of electron density from the B-H σ-bonds to the vacant 5p orbital on tin; these B-H...Sn interactions stabilize the electron-deficient Sn(II) center by 30 kcal mol-1 for meso-6 and 40 kcal mol-1 for rac-6.
- Izod, Keith,McFarlane, William,Tyson, Brent V.,Carr, Ian,Clegg, William,Harrington, Ross W.
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- Pulsed laser ablation of Sn and SnO2 targets: Neutral composition, energetics, and wavelength dependence
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We report time-of-flight mass spectrometric studies of neutral gas-phase species generated in 532 and 355 nm laser ablation of Sn and SnO2 targets at intensities of ≈108 W cm-2, below the plasma threshold. A wavelength-dependent yield of Sn:SnxOy species is observed for the oxide target, with SnxOx (x = 1-3) the primary products at 532 nm and atomic Sn dominant at 355 nm. Sn and Sn2 are the primary products of Sn metal ablation, and the relative Sn:Sn2 yield increases at the shorter wavelength. The speed distributions of neutrals ejected from the oxide target are well represented by unshifted time-transformed Maxwell-Boltzmann (MB) distributions, while those ejected from the metal target exhibit bimodal MB distributions. Typical most-probable speeds are (1-2) × 105 cm s-1, with peak kinetic energies (KEs) of 1-2 eV. The implications of our results for pulsed laser deposition of SnOx films will be emphasized.
- Reid, Scott A.,Ho, Wei,Lamelas
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- The Chemical Preparation of Tin Organosol
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A stable colloidal tin suspension in an organic solvent was prepared by the chemical reduction of tin(II) chloride with sodium tetrahydridoborate in the presence of a protective agent.The tin organosol was examined by means of the Moessbauer absorption spectra of 119Sn in the frozen solution and by means of an electron microscope.
- Ichiba, Sumio,Ono, Hiroaki,Kawasaki, Shunji,Nakagawa, Sakae,Yamada, Masaaki
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- Chemical interaction of Cu-In, Cu-Sn, and Cu-Bi solid solutions with liquid Ga-In and Ga-Sn eutectics
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The reactions of copper-based Cu-In, Cu-Sn, and Cu-Bi solid solutions with liquid Ga-In and Ga-Sn eutectics have been studied in situ by synchrotron x-ray diffraction. The results indicate that the dynamics of the process and the phase composition, grain
- Ancharov,Grigorieva,Tsybulya,Boldyrev
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- Nucleation of tin and tin-silver alloy on copper and nickel in acid plating baths
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The rate of nucleation and number density of nuclei of tin and tin-silver deposits on copper and nickel substrates in acid sulfate and acid methanesulfonate baths were measured by application of a nucleation model to chronoamperometric data. Based on the dependence of nucleation rate on overpotential, the critical Gibbs free energy of nucleation and the critical nucleation size were calculated. A mechanism of alloy nucleation in the presence of thiourea is proposed.
- Zhang,Barkey
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- Organic compounds for preparing lustrous tin coatings
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Organic compounds for preparing lustrous tin coatings were selected taking into account their ionization potential. The best electrolyte composition for plating these coatings was determined.
- Medvedev,Makrushin,Dubenkov
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- Super-hydrophobic tin oxide nanoflowers
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Super-hydrophobic 3D SnO2 flowers with nanoporous petals were produced from the 3D Sn nanoflowers using a controlled shape-preserving thermal oxidation process.
- Chen, Aicheng,Peng, Xinsheng,Koczkur, Kalium,Miller, Brad
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- Size-dependent melting properties of tin nanoparticles
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Tin nanoparticles with various sizes were synthesized by the chemical reduction method and their thermal properties were first studied by differential scanning calorimetry. Both particle size dependent melting temperature and latent heat of fusion have be
- Jiang, Hongjin,Moon, Kyoung-sik,Dong, Hai,Hua, Fay,Wong
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- MOESSBAUER SPECTROSCOPY OF ELECTRODEPOSITED TIN-NICKEL ALLOYS AND THERMALLY PREPARED Ni3Sn2, NiSn, and Ni3Sn4.
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Stoichiometric mixtures equivalent to Ni//3Sn//4, NiSn, and Ni//3Sn//2 were prepared from the melt. The value of the isomer shift, characteristic of the s-electron density at the tin nucleus, was a linear function of the tin concentration, decreasing with increase in nickel concentration. Electrodeposited NiSn yielded a Moessbauer spectrum similar to the thermally prepared material. Alloys containing more than 50 atomic percent (a/o) tin electrodeposited on copper substrates yielded Moessbauer spectra in which elemental tin, a nickel-tin alloy, and a copper-tin alloy were detected. The relative amounts of the constituents varied with the composition of the deposit. No copper-tin intermetallic compound is observed when the deposited alloy had compositions approximating NiSn.
- Leidheiser Jr.,Czako-Nagy,Varsanyi,Vertes
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- Advanced structures in electrodeposited tin base negative electrodes for lithium secondary batteries
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Tin anodes deposited electrochemically on a copper foil current collector are studied to develop a next-generation lithium-ion battery with higher energy density. Better cycle performance through ten initial cycles under full charge and discharge conditions was attained by annealing tin electrodeposited on a rough surface copper foil. The annealing process was found to change the main active material from Sn to Cu6Sn5 with some minor compounds. Furthermore, a microcolumnar structure of the active material portion was found to be self-organized in accordance with the surface profile of the foil during the first charge-discharge cycle. Advantages of these structural features are discussed in terms of the initial charge and discharge performance, including specific capacity and coulombic efficiency measured by using a three-electrode cell.
- Tamura, Noriyuki,Ohshita, Ryuji,Fujimoto, Masahisa,Kamino, Maruo,Fujitani, Shin
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- The stability of an acidic tin methanesulfonate electrolyte in the presence of a hydroquinone antioxidant
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The electrodeposition of tin at a (0.28 cm2) copper surface from 0.014 mol dm-3 SnSO4 and 12.5 vol.% methanesulfonic acid (MSA 1.93 mol dm-3) at 296 K was studied. Hydroquinone concentrations of 0.005, 0.05 and 0.5 mol dm-3 (corresponding to a molar concentration ratio of hydroquinone to stannous ions of 0.36, 3.6 and 36, respectively) were used. Cyclic and linear sweep voltammetry served to characterise the electrochemical behaviour of tin deposition and stripping. The effects of potential sweep rate and electrode rotation speed on the voltammetry were studied. The stability of the electrolyte with storage time was quantified by changes in the limiting current density for tin deposition at a smooth rotating disc electrode and the peak current density at a static disc electrode. The influence of hydroquinone on mass transport controlled tin deposition and suppression of hydrogen evolution was evaluated. Crown Copyright
- Low,Walsh
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- Photoionization mass spectrometric study of neutral species from pulsed laser ablation of SnO2
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We report the application of vacuum ultraviolet (VUV) photoionization mass spectrometry (PIMS) to probe neutral species generated in the 532 nm laser ablation of sintered SnO2 targets. The major (>90%) Sn containing species are of composition (SnO)x (x=1,2,3), with near-natural abundance isotopic distributions. The translational energy distribution was determined for each product and compared to a Maxwellian velocity distribution. The utility of VUV PIMS as a universal probe of neutral species produced in laser ablation is discussed.
- Reid
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- Electrochemical lithiation of new graphite-nanosized tin particle materials obtained by SnCl2 reduction in organic medium
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SnCl2 was reduced in the presence of graphite by t-BuONa-activated NaH. The resulting (tin/graphite)-based system was composed of nanosized tin particles deposited on the graphite surface and of free tin aggregates. Lithium electrochemical insertion occurs in graphite and in tin. A reversible specific charge of 500 mAh/g is found stable upon cycling. This value is lower than the maximum theoretical one (650 mAh/g) assuming a Sn/12C molar composition and the formation of the highest lithium content alloy Li22Sn5. It is suggested that the part of tin responsible for the stable reversible capacity is the one bound to graphite. To the contrary, free tin aggregates could contribute to a capacity which decreases upon cycling in connection with the volume changes accompanying lithium insertion/extraction in/out of these aggregates.
- Balan,Schneider,Ghanbaja,Willmann,Billaud
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- Physicochemical and functional peculiarities of metal oxide whiskers
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Practical aspects of preparation and prospects for practical use of a series of the metal oxide whiskers were studied. The procedures for the synthesis were proposed, and the phase composition, micromorphology, and electrochemical and sensor characteristics of the macroscopic (up to 5-10 mm long) whiskers in the Ba-V-O, Ba-Mn-O, and Sn-O systems were analyzed. The electroconducting BaV8O21-δ whiskers were prepared by the hydrothermal treatment. These whiskers possess stable electrochemical characteristics appropriate for the development of novel secondary current sources. The protonated form of the Ba6Mn24O48 whiskers produced by the isothermal vaporization of chloride fluxes is a mixed conductor with the proton and electron conductivity at a level of mS units at 25 °C. A new procedure by the thermal disproportionation of tin(ii) oxide under nitrogen was proposed for the growth of SnO2 whiskers of various morphology. The produced whiskers have substantial sensor sensitivity toward a series of toxic components of the gaseous medium, such as nitrogen dioxide.
- Goodilin,Pomerantseva,Semenenko,Kocherginskaya,Itkis,Kulova,Skundin,Leonova,Dobrovol'Skii, Yu. A.,Rumyantseva,Gas'Kov,Balakhonov,Churagulov,Tretyakova, Yu. D.
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- Molecular structure of and restricted internal rotation about the tin-tin bond in [ClSn(CH2CH2CH2)2NCH 3]2 and solution isomerism and isomerizations in [CH3Sn(CH2CH2CH2) 2NCH3]2, two compounds with five-coordinate tin centers bound to each other
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The crystal structure of [ClSn(CH2CH2CH2)2NCH 3]2 (1) has been determined by an X-ray study. The crystal data are as follows: triclinic space group P1, a = 10.757 (6), b = 7.673 (3), c = 12.662 (7) ?; α = 83.49 (4), β = 90.26 (4), γ = 72.48 (4)°; V = 989.4 ?3; Z = 2. The structure was refined to R = 0.045. The two five-coordinate tin moieties exhibit approximately trigonal-bipyramidal geometries with the chlorine and nitrogen atoms occupying apical positions and the tin-tin and tin-carbon bonds occupying equatorial positions and are twisted with respect to one another by about 120° along the tin-tin bond. The 1H, 13C, and 119Sn NMR data indicate that in solution 1 exists as only one isomer having the same structure as in the solid state. At low temperature, the 13C spectra reveal restricted internal rotation about the tin-tin bond with an activation barrier of about 11.5 ± 0.5 kcal/mol. In contrast, [CH3Sn(CH2CH2CH2) 2NCH3]2 (2) exists in solution as a mixture of at least three isomers, A, B, and C. NMR data on the major isomer A of 2 are explained in terms of a structure with the two methyl groups and the two intramolecularly coordinating nitrogen atoms in apical positions at each tin and the two ring carbon chains and the tin-tin bond in equatorial positions, in agreement with both the cyclic ligand structure and the polarity rule. For the medium and minor isomers of 2, B and C, respectively, no unambiguous structure can be proposed: B and C either have respectively only one and no methyl group in the apical position, with one and two tin atoms in the apical position, or have one and two four-coordinate tin centers, respectively. An analysis of the cross peaks of a two-dimensional EXSY 119Sn NMR spectrum of 2 reveals that the isomers A and B interconvert through an uncorrelated rearrangement of one tin center at a time. No evidence could be found that the internal rotation about the tin-tin bond is restricted in 2 on the NMR time scale at temperatures at which it is in 1. The differences between the dynamic stereochemical behaviors of 1 and 2 are explained in terms of the apicophilicity differences between a methyl group and a chlorine atom.
- Jurkschat,Tzschach,Mügge,Piret-Meunier,Van Meerssche,Van Binst,Wynants,Gielen,Willem
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- Synthesis and stability of Sn(II)-containing perovskites: (Ba,SnII)HfIVO3 versus (Ba,SnII)SnIVO3
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While Sn(II)-containing perovskite oxides have long drawn attention as Pb(II) substitutes in technologically-relevant dielectric materials, they are also highly thermodynamically unstable and potentially impossible to prepare. Investigations into the new flux-mediated syntheses of metastable Sn(II)-containing hafnate and stannate perovskites were aimed at understanding the key factors related to their synthesizability. The BaHfO3 perovskite was reacted with SnClF from 250 to 350 ?°C for 12–72 ?h, yielding an unprecedented Sn(II) concentration on the A-site of up to ~70 ?mol%, i.e., (Ba0.3Sn0.7)HfO3 in high purity. Elemental mapping using EDS shows the Sn(II) cations diffuse gradually throughout the crystallites, with two reaction cycles needed to give a nearly homogeneous distribution. In contrast, similar reactions with BaSnO3 and as little as 10 ?mol% Sn(II) result in decomposition to SnO, SnO2, and BaSnO3. The (Ba1-xSnx)HfO3 compositions exhibit a primary cubic perovskite structure (Pm3ˉm; for x ?= ?1/3, 1/2 and 2/3) by powder X-ray diffraction (XRD) methods, with the Sn(II) cations substituted on the A-site. Total energy calculations show the thermodynamic instability versus the ground state (i.e., metastability) for (Ba1-xSnx)HfO3 increases with Sn(II) substitution, reaching a maximum of ~446 ?meV atom?1 at ~70 ?mol% Sn(II). The decomposition pathway of (Ba1/3Sn2/3)HfO3 was probed by ex situ XRD as well as in situ electron microscopy methods. An onset of thermally-induced decomposition begins at ~350–400 ?°C to give the more stable oxides which are found to segregate out in surface layers. These results help to elucidate the factors underpinning the synthesizability of highly metastable Sn(II)-containing perovskites, which increases with their cohesive energy and with the absence of lower-energy polymorphs or other ground states that can be reached without significant ion diffusion.
- Broughton, Rachel,Gabilondo, Eric A.,Jones, Jacob L.,Maggard, Paul A.,O'Donnell, Shaun
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- Electrodeposition of mesoporous tin films
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Mesoporous metallic tin has been electrodeposited, from the homogeneous hexagonal mesophase of a series of amphiphilic non-ionic surfactants, with a controllable repeat structure in the range of 5-10 nm.
- Whitehead, Adam H.,Elliott, Joanne M.,Owen, John R.,Attard, George S.
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- Passivating ability of surface film derived from vinylene carbonate on tin negative electrode
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The passivating ability of surface film derived from vinylene carbonate (VC) is addressed on tin (Sn) negative electrode after a comparative study on the thickness, film growth pattern, chemical composition, and mechanical flexibility of the surface films generated from VC-free and VC-added electrolytes. The surface film derived from the former electrolyte is enriched by inorganic fluorinated and carbonate species, and shows a poor passivating ability to cause a continued electrolyte decomposition, film growth and eventual electrode failure. In contrast, organic carbon-oxygen species are dominant in the film derived from the VC-added electrolyte. Even if this film is thinner than the other, it passivates the Sn electrode surface more effectively. As a result, the film growth and electrode polarization are less significant. The superior passivating ability of organic-rich surface film has been ascribed to a uniform coverage and higher mechanical flexibility.
- Park, Sangjin,Heon Ryu, Ji,Oh, Seung M.
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- An unexpected dependence on the SnII base; Reactions of Sn(NR2)2 with aromatic dithiols
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Unexpectedly, the reactions of the SnII base Sn(NMe 2)2 with 1,2-benzodithiols [L(SH)2] do not give the stannylenes, L(S)2Sn, which are generated with Sn{N(SiMe 3)2}2, instead the ion-separated Sn IV compounds [Sn{L(S)2}]2- 2[R 2NH2]+ are formed in high yields.
- Melen, Rebecca L.,McPartlin, Mary,Wright, Dominic S.
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- Thermal expansion and melting temperature of the half-Heusler compounds: MNiSn (M = Ti, Zr, Hf)
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Half-Heusler compounds: MNiSn (M = Ti, Zr, Hf) are considered as a candidate of environmentally friendly and low-cost thermoelectric (TE) materials. Although the thermomechanical properties are quite important when utilizing the half-Heusler compounds in TE devices, such properties have been scarcely reported. In the present study, we tried to collect the data of the thermal expansion coefficient and the melting temperature (Tm) of MNiSn. The thermal expansion coefficient was evaluated by means of two methods: the dilatometer measurement and the high temperature X-ray diffraction analysis. The Tm was evaluated from the differential thermal analysis. The relationship between the thermal expansion coefficient and the Tm of the half-Heusler compounds was studied.
- Jung, Do-young,Kurosaki, Ken,Kim, Chang-eun,Muta, Hiroaki,Yamanaka, Shinsuke
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- Structural and morphological modifications of a nanosized 62 atom percent Sn-Ni thin film anode during reaction with lithium
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Nanosized electrodeposited 62 atom % Sn-Ni alloy was tested to highlight the effects of volume changes on the cycling life of the electrode during lithiation and delithiation. X-ray diffraction showed that the Ni 3Sn4 was the main phase of the as-deposited alloy. A unique feature of the 62 atom % Sn-Ni is that it exhibited a capacity recovery upon cycling. When cycled galvanostatically, the Sn62Ni38 offers low capacity fade while reversibly incorporating lithium up to 600 mAh/g. At the first charge LiSn alloy phases are formed. This led to volume expansion of the electrode causing the formation of cracks. At the following cycles the Ni3Sn4, phase was restored and preserved over extensive cycling revealing the reversibility of the reaction between Ni 3Sn4, and Li+. As to the reasons of the capacity recovery noticed with this alloy, scanning electron microscopy images provided evidence of modifications of the surface condition accompanying a volume change during cycling. The chemical diffusion coefficient (D Li) value determined from electrochemical impedence spectroscopy measurements during lithium insertion was within 10-9 to 10 -10 cm2 s-1.
- Mukaibo, Hitomi,Momma, Toshiyuki,Mohamedi, Mohamed,Osaka, Tetsuya
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- Spectroscopic, thermogravimetric and antibacterial studies for some bivalent metal complexes of oxalyl-, malonyl- and succinyl-bis(4-p- chlorophenylthiosemicarbazide)
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Anodic oxidation of Co, Cu, Zn, and Sn metals in an anhydrous acetone solution of 1,1-oxalyl-, malonyl- or succinyl-bis(4-p- chlorophenylthiosemicarbazide) yields a new polynuclear complexes. The isolated complexes have the general composition [M2(L)(H2O) 6], L = pClSuTS and M = Co(II), Cu(II) or Sn(II), [M 2(L)(H2O)n]·nH2O where M = Cu(II), Co(II) or Sn(II), L = pClOxTS and n = 2 or 6, and [M2(L)(ac) 2]·nH2O where M = Co(II) or Zn(II), L = pClOxTS or pClSuTS and n = 2. The thermogravimetry (TG) and derivative thermogravimetry (DTG) have been used to study the thermal decomposition of the investigated bisthiosemicarbazide ligands and their metal complexes. The kinetic thermodynamic parameters such as: E, ΔH, ΔS and ΔG are calculated using Horowitz-Metzger (HM) and Coats-Redfern (CR) equations. The kinetic thermodynamic parameters such as: E, ΔH, ΔSand ΔG are calculated from the DTG curves. The tested compounds show a reasonable activity against four strains of Gram-negative bacteria; Escherichia coli, Pseudomonas aeruginosa species and Gram-positive bacteria; Bacillus cereus and Staphylococcus aureus.
- Amin, Ragab R.,Yamany, Yamany B.
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- Electrodeposition of Ni, Sn and Ni-Sn alloy coatings from pyrophosphate-glycine bath
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In this work the electrodeposition of Ni, Sn and Ni-Sn alloy from the solution containing pyrophosphate andor glycine has been investigated by cyclic voltammmetry (CV), potentiostatic pulse and polarization curve measurements on two substrates, Ni and GC.
- Lacnjevac,Jovic,Jovic
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- ELECTRON-INDUCED DECOMPOSITION OF TIN(IV) SULPHIDE IN THE ELECTRON MICROSCOPE CONTROLLED BY EPITAXY ON INNER LATTICE PLANES
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Electron microscope experiments show that the mechanism of electron- induced decomposition of tin(IV) sulfide differs from that of thermal decomposition. Hexagonal tin(IV) sulfide is converted to tetragonal tin in three equivalent orientations with (100)Sn parallel to (100)SnS2 and (001)Sn parallel to (001SnS2. Experiments on epitaxic growth of tin on tin )IV( sulfide )001( surfaces and theoretical considerations of relative interface energies show that the reaction is controlled by epitaxy and not by a threedimensional relation between the two lattices.
- GUENTER JR,OSWALD HR
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- Superconducting proximity effect in single-crystal Sn nanowires
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An in situ template-based electrochemical method was used to fabricate single-crystal Sn nanowires, of 6 μm in length and 30-200 nm in diameter, in contact with two bulk film electrodes of Au, Sn, or Pb. Superconductivity in these Sn nanowires was found t
- Liu, Haidong,Ye, Zuxin,Zhang, Hong,Wu, Wenhao,Luo, Zhiping,Rathnayaka,Naugle
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- Beneficial effects of Mo on the electrochemical properties of tin as an anode material for lithium batteries
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A simple, novel method for improving the electrochemical response of Sn in lithium cells is proposed that involves preparing Sn by a reduction procedure in the presence of Mo powders. Four different MoxSn1 - x mixtures (0 x 0.26) were electrochemically tested and their structural and textural properties determined by using X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical properties of the resulting composites in lithium cells were studied by galvanostatic, step potential electrochemical spectroscopy (SPES) and electrochemical impedance spectroscopy (EIS) measurements. The mixtures were found to consist of crystalline Sn and Mo; however, the presence of the latter element modified the Sn habit in two ways, namely, by significantly decreasing particle size and increasing the reactivity towards oxygen. Although Mo is inert towards lithium, it increased both the discharge capacity and the capacity retention of the electrode in relation to pure Sn. The improved interparticle connectivity, reduced electrolyte decomposition and decreased charge-transfer resistance observed in the Mo-containing samples appear to be beneficial effects of the addition of Mo.
- Fernández,Martín,Morales,Ramos-Barrado,Sánchez
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- Structurally Ordered Intermetallic Cobalt Stannide Nanocrystals for High-Performance Electrocatalytic Overall Water-Splitting
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The synthesis of structurally ordered non-noble intermetallic cobalt stannide (CoSn2) nanocrystals and their utilization for high-performance electrocatalytic overall water-splitting is presented. The structurally and electronically beneficial properties of the tetragonal CoSn2 exhibit a considerably low overpotential for the oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) on fluorine-doped tin oxide (FTO) and Ni foam (NF). Loss of Sn from the crystal lattices and oxidation of Co under strongly alkaline conditions furnishes highly disordered amorphous active CoOx(H), the catalytically active structure for OER. The Co0 atoms in the CoSn2 act as active sites for HER and the presence of Sn provides efficient electrical conductivity. This intermetallic phase is a novel type of cost-effective and competitive bifunctional electrocatalysts and predestinated for overall water-splitting devices: A two-electrode electrolyzer with CoSn2 on NF delivers a cell voltage of merely 1.55 V at 10 mA cm?2 maintaining long-term stability.
- Menezes, Prashanth W.,Panda, Chakadola,Garai, Somenath,Walter, Carsten,Guiet, Amandine,Driess, Matthias
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- Structure and applications of organotin complex based on trimethyltin cation and quinaldic acid
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The reaction between aqueous solution of Me3SnCl and acetonitrile solution of quinaldic acid (quinH) at room temperature affords a new organotin complex, [Me3Sn(quinH)(quin)]?6H2O (1). Complex 1 was structurally characterized using infrared, UV–visible and NMR spectra, thermogravimetric analysis and single-crystal X-ray analysis. The network structure of 1 is developed by a limitless number of discrete mononuclear molecules forming a one-dimensional chain via hydrogen bonds. Extensive hydrogen bonds and π–π stacking associate the one-dimensional chains creating a two-dimensional array. The two-dimensional arrays are additionally associated via hydrogen bonds through the water molecules and the methyl groups forming a three-dimensional network. The cytotoxic impact of 1 on the viability of MCF-7 cells was also examined using MTT assay, exhibiting great inhibiting action against MCF-7 cells. Furthermore, the catalytic degradation performance of 1 towards methylene blue dye in the presence of H2O2 as oxidant was investigated. The reaction is first order with respect to methylene blue dye.
- El-bendary, Mohamed M.,Etaiw, Safaa El-din H.
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- BINDUNGSABSTAENDE ZWISCHEN ORGANYLSUBSTITUIERTEN ZINNATOMEN II. CYCLO-TETRASTANNANE
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The crystal structures of octa-t-butyl-cyclo-tetrastannane (t-Bu2Sn)4 and octa-t-amyl-cyclo-tetrastannane (t-Am2Sn)4 have been determined by X-ray analysis.The four-membered tin ring of (t-Bu2Sn)4 is planar and the molecules are highly ordered in the crys
- Puff, Heinrich,Bach, Christa,Schuh, Willi,Zimmer, Rene
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- Acid–Base Interaction Enhancing Oxygen Tolerance in Electrocatalytic Carbon Dioxide Reduction
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Hybrid electrodes with improved O2 tolerance and capability of CO2 conversion into liquid products in the presence of O2 are presented. Aniline molecules are introduced into the pore structure of a polymer of intrinsic microporosity to expand its gas separation functionality beyond pure physical sieving. The chemical interaction between the acidic CO2 molecule and the basic amino group of aniline renders enhanced CO2 separation from O2. Loaded with a cobalt phthalocyanine-based cathode catalyst, the hybrid electrode achieves a CO Faradaic efficiency of 71 percent with 10 percent O2 in the CO2 feed gas. The electrode can still produce CO at an O2/CO2 ratio as high as 9:1. Switching to a Sn-based catalyst, for the first time O2-tolerant CO2 electroreduction to liquid products is realized, generating formate with nearly 100 percent selectivity and a current density of 56.7 mA cm?2 in the presence of 5 percent O2.
- Li, Pengsong,Lu, Xu,Malpass-Evans, Richard,McKeown, Neil B.,Sun, Xiaoming,Wang, Hailiang,Wu, Yueshen,Wu, Zishan
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supporting information
p. 10918 - 10923
(2020/04/27)
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- High stability three-dimensional porous PtSn nano-catalyst for ethanol electro-oxidation reaction
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In addition to the theoretical research, direct ethanol fuel cells have great potential in practical applications. The performance of direct ethanol fuel cells largely depends on the electrocatalysts. Pt-based electrocatalysts have been promising candidates for advancing direct ethanol fuel cells for its high catalytic activity and great durability. Here, a PtSn catalyst with unique three-dimensional porous nanostructure has been designed and synthesized via a two-step liquid phase reduction reaction. Sn formed a self-supporting framework in PtSn alloy particles (～3.5 nm). In ethanol electro-oxidation reaction, the PtSn catalyst exhibited high mass activity and excellent recycling time compared with that of Pt/C. After the morphology characterization before and after potential cycling, the PtSn alloy-based nano-catalyst showed good stability. The PtSn catalysts effectively avoid structural instability due to the external carriers, and prolong the leaching time of Sn. In addition, the introduction of a certain amount of Sn can also solve the poisoning phenomenon of active sites on Pt surface. The design strategy of porous alloy nano-catalyst sheds light on its applications in direct ethanol fuel cells.
- Sun, Yue,Xiang, Haiyan,Li, Huimin,Yu, Gang,Chen, Hong,Liu, Song
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p. 2491 - 2494
(2020/06/23)
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- Synthesis, characterization of active Sn(0), and its application in selective propargylation of aldehyde at room temperature in water
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Active Sn(0) particles are synthesized in high yields by the chemical reduction of the blue-black stannous oxide using freshly prepared sodium stannite solution as reducing agent at 40 °C and 60 °C. The Sn(0) particles are characterized using powder XRD, SEM, and DSC. The as-synthesized Sn(0) particles are applied as reagent for the regioselective synthesis of homopropargyl alcohols from propargyl bromide and aldehydes in distilled water at room temperature (in 50%-84% yields). No assistance of heat, microwave, ultrasound, organic co-solvent, co-reagent, or inert atmosphere is required for this reaction. The propargylation reaction is highly chemoselective towards aldehyde over other less electrophilic carbonyl functional groups such as ketone, amide, and carboxylic acid. Our in-house synthesized homopropargyl alcohols can be used to synthesize conjugated 1,3-diynes.
- Chatterjee, Paresh Nath,Paul, Dipankar,Sawkmie, Micky Lanster,Sinha, Arun Kumar,Khatua, Snehadrinarayan
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supporting information
p. 29 - 36
(2019/01/10)
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- Nitrosubstituted hydroxamate ligands in new triphenyltin(IV) complexes as prospective antimicrobial agents
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New triphenyltin(IV) hydroxamate complexes, [Ph3Sn(4-NO2CnH)] and [Ph3Sn(4-NO2BzH)] have been synthesized by the reactions of Ph3SnCl with potassium 4-nitrocinnamo hydroxamate [4-NO2C6H4CHCHCONHOK] (KHL1) and potassium 4-nitro benzohydroxamate [4-NO2C6H4CONHOK] (KHL2). The complexes were synthesized in 1:1 molar ratio in MeOH + C6H6 and characterized by physicochemical and IR, 1H NMR, and mass spectrometry. The bidentate hydroxamate involving bonding through carbonyl and hydroxamic oxygen (O, O coordination) has been inferred from IR spectra. The electrochemical behavior of complexes has been analyzed. Quasi-irreversible two electron metal-centered cathodic process of type SnIV/SnII redox couple was indicated by cyclic voltammetric technique. The thermal behavior of 1 and 2 studied by TGA has shown continuous decomposition to yield Sn + 0.5SnO2 and SnO2 as final residues. The in vitro antimicrobial activity assays of 1 and 2 against pathogenic Gram-positive bacteria (Bacillus subtilis and Staphylococcus aureus), Gram-negative bacteria (Salmonella typhi and Pseudomonas aeruginosa), and fungi (Aspergillus fumigatus and Alternaria alternata) were done by MIC method. The complexes have exhibited appreciable antimicrobial activity relative to the respective standard Gentamycin and Nystatin drugs.
- Kumari, Shilpa,Sharma, Neeraj
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p. 584 - 599
(2019/05/14)
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- H2MBH2 and M(μ-H)2BH2 Molecules Isolated in Solid Argon: Interelement M-B and M-H-B Bonds (M = Ge, Sn)
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Laser-ablated boron atoms react with GeH4 molecules to form novel germylidene borane H2GeBH2, which undergoes a photochemical rearrangement to the germanium tetrahydroborate Ge(μ-H)2BH2 upon irradiation with light of λ = 405 nm. For comparison, the boron atom reactions with SnH4 only gave the tin tetrahydroborate Sn(μ-H)2BH2. Infrared matrix-isolation spectroscopy with deuterium substitution and the state-of-the-art quantum-chemical calculations are used to identify these species in solid argon. A planar structure of H2GeBH2 with an electron-deficient B-Ge bond with a partial multiple bond character (bond order = 1.5) is predicted by quantum-chemical calculations. In the case of M(μ-H)2BH2 (M = Ge, Sn) two 3c-2e B-H-M hydrogen bridged bonds are formed by donation of electrons from the B-H σ-bonds into empty p-orbitals of M.
- Zhao, Jie,Beckers, Helmut,Huang, Tengfei,Wang, Xuefeng,Riedel, Sebastian
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p. 2218 - 2227
(2018/02/23)
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- Synthesis, solid-state structures and reduction reactions of heteroleptic Ge(II) and Sn(II) β-ketoiminate complexes
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A series of new heteroleptic divalent germaniun and tin complexes of the general type L1,4GeN(SiMe3)2 (1, 2) and L1-4SnN(SiMe3)2 (3-6) were synthesized by reaction of β-ketimines L1-4
- Wiederkehr, Jessica,W?lper, Christoph,Schulz, Stephan
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p. 813 - 820
(2018/01/19)
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- Smart Solution Chemistry to Sn-Containing Intermetallic Compounds through a Self-Disproportionation Process
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Developing new methods to synthesize intermetallics is one of the most critical issues for the discovery and application of multifunctional metal materials; however, the synthesis of Sn-containing intermetallics is challenging. In this work, we demonstrated for the first time that a self-disproportionation-induced in situ process produces cavernous Sn?Cu intermetallics (Cu3Sn and Cu6Sn5). The successful synthesis is realized by introducing inorganic metal salts (SnCl2?2 H2O) to NaOH aqueous solution to form an intermediate product of reductant (Na2SnO2) and by employing steam pressures that enhance the reduction ability. Distinct from the traditional in situ reduction, the current reduction process avoided the uncontrolled phase composition and excessive use of organic regents. An insight into the mechanism was revealed for the Sn?Cu case. Moreover, this method could be extended to other Sn-containing materials (Sn?Co, Sn?Ni). All these intermetallics were attempted in the catalytic effect on thermal decompositions of ammonium perchlorate. It is demonstrated that Cu3Sn showed an outstanding catalytic performance. The superior property might be primarily originated from the intrinsic chemical compositions and cavernous morphology as well. We supposed that this smart solution reduction methodology reported here would provide a new recognition for the reduction reaction, and its modified strategy may be applied to the synthesis of other metals, intermetallics as well as some unknown materials.
- Zhang, Yuelan,Li, Liping,Li, Qi,Fan, Jianming,Zheng, Jing,Li, Guangshe
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supporting information
p. 14196 - 14204
(2016/09/23)
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- Elucidating the promotional effects of niobia on SnO2 for CO oxidation: Developing an XRD extrapolation method to measure the lattice capacity of solid solutions
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A series of Sn-Nb binary catalysts have been prepared by using a co-precipitation method and used for CO oxidation. All the catalysts show much higher specific surface areas than the individual oxides, indicating their improved thermal stability. It was found that Nb5+ cations can be doped into the lattice of tetragonal rutile SnO2 to replace a portion of the Sn4+ to form a solid solution structure. Using an XRD extrapolation method, the SnO2 lattice capacity for Nb2O5 has been quantified, which proves that only 25% of the Sn4+ in the SnO2 lattice can be replaced by Nb5+ to form a stable solid solution. For the samples with Nb contents below the capacity, the formed solid solution structure can induce the formation of a large quantity of stable and active surface deficient oxygen species due to charge imbalance and lattice defects, which improve the CO oxidation activity remarkably. For the samples with Nb contents above the capacity, the excess Nb is present as free Nb2O5 in the catalysts, which is harmful to their activity. It is concluded that Nb, as an effective promoter for SnO2, must be incorporated into its lattice as Nb5+ to form a solid solution. A Sn-Nb solid solution without excess Nb2O5 is not only a promising catalyst itself, but also a good support for precious metals to prepare catalysts for CO oxidation.
- Xu, Xianglan,Liu, Fang,Han, Xue,Wu, Yuanyuan,Liu, Wenming,Zhang, Rongbin,Zhang, Ning,Wang, Xiang
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p. 5280 - 5291
(2016/07/21)
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- Synthesis and melting behaviour of Bi, Sn and Sn-Bi nanostructured alloy
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Lead-free solders based on Bi-Sn bimetallic nanoclusters with eutectic composition (Bi43Sn57) were synthesized at low temperature by simultaneous reduction reaction from aqueous solution containing bismuth and tin chlorides, using potassium borohydride as a reducing agent. By the same processing route, pure bismuth and tin nanoparticles have also been prepared. Microstructure, morphology and composition of the samples were characterized by X-ray powder diffraction (XRD), transmission (TEM) and scanning electron microscopy (SEM). TEM images of Bi-Sn nanoparticles show average size ranging from 30 to 100 nm. Thermal behaviour of Bi-Sn nanopowders was studied by DSC (differential scanning calorimetry) and a melting temperature (135 °C) lower than that of the corresponding microcrystalline sample (139 °C) was observed. SEM micrographs of the thermally treated sample up to 400 °C show fine spherical grains in the micrometer range with finer powder particles on the surface. XRD powder diffraction analysis indicates the formation of bismuth and tin nanophases with an average particle size of 85 and 126 nm, respectively. The oxidation behaviour of the samples was also investigated. The results obtained have been analyzed in view of theoretical models describing the melting temperature depression of nanoparticles.
- Frongia,Pilloni,Scano,Ardu,Cannas,Musinu,Borzone,Delsante,Novakovic,Ennas
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- Synthesis of active tin: An efficient reagent for allylation reaction of carbonyl compounds
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High purity Sn(0) has been obtained as a result of reduction of SnO by sodium stannite (Na2SnO2) in aqueous solution. The process stands unique for the production of tin metal. The as-synthesized tin finds applications in synthetic organic chemistry as a reagent for the allylation of aldehydes and ketones in distilled water at room temperature to give rise to the corresponding homoallylic alcohols with high yield. The reaction occurs without the assistance of heat, ultrasonic vibration, co-solvents/co-reagents, etc. Enhancement of the reaction rate of allylation was observed in water rather than THF. The manipulation of allylation reaction becomes easy with active tin material.
- Sinha, Arun Kumar,Sil, Amit,Sasmal, Anup Kumar,Pradhan, Mukul,Pal, Tarasankar
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p. 1685 - 1690
(2015/03/30)
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- Electrochemical reduction of CO2 to HCOOH on a synthesized Sn electrocatalyst using a Co3O4 anode
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The present work investigates the electrocatalytic effect of tin (Sn) and cobalt oxide (Co3O4) on the reduction of CO2 to products electrochemically (RCPE). Electrocatalytic (Sn) powder was synthesized by an electrodeposition method from a SnCl2·2H2O solution. Experiments were conducted using Co3O4 and Sn electrodes as the anode and cathode, respectively, in 0.5 M potassium and sodium carbonate and bicarbonate solutions. The electrodes were prepared by coating the electrocatalysts onto a graphite plate surface. The experiments were conducted with different applied voltages (1.5 to 3.5 V) and time intervals (5, 10, 15, 20 and 25 min) in the various electrolyte solutions. It was observed that HCOOH acid was the only product formed for all the applied conditions. At 1.5 V and 2 V, maximum Faradaic efficiencies of 74.04% and 92.6% for HCOOH production were obtained from 20 and 5 min reactions in a KHCO3 electrolyte solution. The ability of Co3O4 to perform water oxidation and the Sn electrocatalyst to reduce CO2 to HCOOH was established from the obtained results. The optimized reaction conditions to achieve high Faradaic efficiencies are explained in detail.
- Yadav,Purkait
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p. 68551 - 68557
(2015/09/01)
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- Investigation of the reaction progress between stannous chloride and zirconium in molten LiCl-KCl
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LiCl-KCl-ZrCl4 melt was prepared by an in situ displacement reaction between SnCl2 and Zr in LiCl-KCl melt at 773 K, and the progress of the reaction between SnCl2 and Zr was also investigated by dynamic electrochemical measurements, such as cyclic voltammetry, square wave voltammetry and open circuit chronopotentiometry. The results reveal that the concentration of Zr(iv) increases gradually and reaches a maximum value with the reaction time increasing from 0 to 210 min, while the concentration of Sn(ii) decreases gradually and drops below the detection limit. In addition, the chemical analyses of Zr(iv) and Sn(ii) in the melt at various times were also carried out and the results are in good agreement with those of the electrochemical measurements. Finally, LiCl-KCl-ZrCl4 melts with a low concentration of Sn(ii) (0.01 wt%) were obtained, when the reaction time was prolonged to 210 min.
- Cai, Yanqing,Liu, Hongxia,Xu, Qian,Song, Qiushi,Liu, Huijun
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p. 31648 - 31655
(2015/04/22)
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- [2]Ferrocenophanes with Nitrogen in Bridging Positions
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Three [2]ferrocenophanes ([2]FCPs) bridged by nitrogen and silicon (7SiMe2) and nitrogen and tin (7SnMe2, 7SntBu2) were synthesized by salt metathesis between a dilithioferrocene derivative, prepared in situ from 1-bromo-1′-(trimethylsilylamino)ferrocene (6), and Me2SiCl2, Me2SnCl2, and tBu2SnCl2, respectively. A multistep synthesis of precursor 6 is described. Only 7SiMe2 and 7SntBu2 could be prepared as analytically pure compounds. The molecular structures of all three [2]FCPs were determined by single-crystal X-ray analysis. Expectedly, the tilting of the Cp ligands in the silicon species 7SiMe2 is larger [α = 15.73(13)°] than in the tin compounds 7SnMe2 [α = 9.36(17) and 9.45(18)°] and 7SntBu2 [α = 10.13(11)°]. Ring-opening polymerizations of 7SiMe2 and 7SntBu2 were attempted using the common methods of thermal, transition-metal-catalyzed, anionic, and photocontrolled ring-opening polymerization, but none of the experiments gave polymeric materials. (Figure Presented).
- Dey, Subhayan,Quail, J. Wilson,Müller, Jens
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p. 3039 - 3046
(2015/06/30)
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- A comparative study of enhanced electrochemical stability of tin-nickel alloy anode for high-performance lithium ion battery
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Sn and Sn-Ni alloy nanoparticles are synthesized readily by co-precipitation method for their applications in Li-ion batteries. It is found that nickel not only affects the phase structure and morphology of the alloy, but also impacts Li-Sn alloying and dealloying behaviors. In Li-ion batteries, the alloy electrodes deliver stronger cycling stability than the pure Sn anode. In tests the former exhibits a final capacity of 228.5 mA h g-1over 50 cycles, while the latter displays 14.3 mA h g-1. Smaller current for battery cycles increases capacities of the alloys beyond 408.4 mA h g-1. The mechanism of enhanced stability of Sn-Ni alloys is examined. Redox reaction characteristics and Li-ion transfer kinetics at these anodes after different cycles are investigated by cyclic voltammetry and electrochemical impedance spectroscopy, which are considered to associate with buffering effects of nickel and structural integrity of electrodes. Li-Sn alloying and dealloying reactions cause volume changes and induce stress that releases in the formation of tiny cracks within the particles. The cracks accelerate side reactions and decelerate charge transport, detrimental to the electrode stability. Nickel cushions the volume variations and reduces the stress and cracks at Sn-Ni alloy anodes to allow them to maintain better electrode integrity and smaller charge resistance, thus yielding their improved Li-ion intercalation stability during long-term cycling.
- Guan, Dongsheng,Li, Jianyang,Gao, Xianfeng,Yuan, Chris
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p. 464 - 471
(2014/12/10)
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- Formation of Cu2SnSe3 from stacked elemental layers investigated by combined in situ X-ray diffraction and differential scanning calorimetry techniques
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Stacked elemental layers of Mo/Cu/Sn and Mo/Cu/Sn/Se were employed as samples for investigating the formation reaction of Cu-Sn intermetallic compounds as well as Cu2SnSe3 phases by in situ technique of X-ray diffraction and differential scanning calorimetry. The use of a combined in situ technique allows a real-time observation on solid-state reactions as well as any crystalline phase changes during annealing towards the crystallization of Cu2SnSe3. It is found that Cu and Sn form intermetallic compounds of Cu6Sn5, Cu3Sn and Cu41Sn11 as the annealing temperature rises from 30 to 550 C. The reaction of Se with Cu to form a CuSe phase dominates the binary phase formation at a low annealing temperature. The annealing of a stacked Mo/Cu/Sn/Se layer suggests that only Cu6Sn5 intermetallic compound directly acts as a reactant for the Cu-selenide phase formation. A SnSe phase mostly forms from a liquid-state reaction of Sn and Se above the Sn melting point. The in situ investigation also reveals a complete set of Cu-selenide peritectic decompositions of CuSe2 → CuSe → Cu1.8Se at 360 and 412 C. The formation of Cu2SnSe 3 phase starts at 450 C as a product from a reaction between Cu 1.8Se and SnSe in a presence of liquid Se. Comparisons on the initial formation temperatures of all involved phases and on the formation pathways between Cu2SnSe3 and Cu2SnS3 are discussed as well.
- Wibowo, Rachmat Adhi,Moeckel, Stefan,Yoo, Hyesun,Hoelzing, Astrid,Hock, Rainer,Wellmann, Peter J.
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p. 254 - 258
(2014/01/06)
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- Wide electrochemical window ionic salt for use in electropositive metal electrodeposition and solid state Li-ion batteries
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A stable hydrophobic ionic crystalline solid comprised of the N-propyl-N-methylpiperidinium cation and hexafluorophosphate anion PP 13PF6 exhibits a remarkably wide electrochemical window of 7.2 V. This high purity crystalline ionic salt has versatility for use as an electrolyte in the electrodeposition of reactive metals such as tin. Moreover, this ionic salt can be used as a solid state electrolyte in Li-ion batteries. Theoretical calculations indicate that this solid state electrolyte has vacant sites that are preferential for Li-ion conductivity with an energy barrier of 0.4 eV. Further, the ionic crystals exhibit molecular rotations which facilitate facile Li-ion transport.
- Murugesan, Sankaran,Quintero, Oliver A.,Chou, Brendan P.,Xiao, Penghao,Park, Kyusung,Hall, Justin W.,Jones, Richard A.,Henkelman, Graeme,Goodenough, John B.,Stevenson, Keith J.
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p. 2194 - 2201
(2014/02/14)
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- Preparation of reduced iron powder using combined distribution of wood-charcoal by microwave heating
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In this paper, the influences of microwave heating with wood-charcoal as the reducing agent, on the reducing characterization of mill-scale were systematically investigated. The microstructures of the samples were characterized before and after microwave
- Ye, Qianxu,Zhu, Hongbo,Zhang, Libo,Ma, Ji,Zhou, Li,Liu, Peng,Chen, Jian,Chen, Guo,Peng, Jinhui
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p. 102 - 106
(2014/07/08)
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- Dependence of microhardness on solidification processing parameters and dendritic spacing in directionally solidified Sn-Ni peritectic alloys
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Sn-Ni peritectic alloys were directionally solidified using a Bridgman type directional solidification furnace. Microhardness (Hv) of both primary Ni3Sn2 phase and peritectic Ni3Sn4 phase and microstructure length scales including primary dendrite arm spacing λ1 were measured as a function of growth rate. Dependency of microhardness on the solidiication processing parameters and primary dendrite arm spacing (λ1) in the directionally solidified Sn-36at.%Ni alloys were experimentally analyzed. The relationships between the solidification processing parameters (growth rate v and temperature gradient G) and microhardness, and primary dendrite arm spacing and microhardness were obtained by linear regression analysis: for primary Ni3Sn2 phase, Hv = 501.06 ν0.07, Hv = 5896.3λ1-0.42; for peritectic Ni3Sn4 phase, Hv = 306.76ν0.10, Hv = 843.6λ1-0.69. It has been found that the values of λ1 decreases with the increasing values of ν while the values of microhardness (Hv) increase with growth rate under constant G.
- Peng, Peng,Li, Xinzhong,Su, Yanqing,Li, Jiangong,Guo, Jingjie,Fu, Hengzhi
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- Influence of the operating conditions and kinetic analysis of the selective hydrogenation of oleic acid on Ru-Sn-B/Al2O3 catalysts
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The influence of the operating conditions on the selectivity and activity of Ru-Sn-B/Al2O3 catalysts for the hydrogenation of oleic acid to oleyl alcohol was studied. It was found that the Ru-Sn-B/Al 2O3 catalyst is selective to oleyl alcohol while Ru or Ru-B/Al2O3 catalysts are not selective to produce oleyl alcohol. The electronic and catalytic properties of Ru are modified by the strong interaction between Sn and B. The incorporation of Sn leads to catalysts capable of producing oleyl alcohol. The experiments of oleic acid hydrogenation showed that an increase in reaction temperature leads to an increase in activity while the selectivity to oleyl alcohol goes through a maximum. This is because the reactions of hydrogenation of CC double bond have lower activation energies than hydrogenolytic reactions. The increase in operating pressure has a positive effect on conversion and a more important effect on selectivity. A very simple first order kinetic model is proposed and reasonably represents the results obtained. This model can be useful to compare catalyst performance more rationally.
- Sánchez, María A.,Pouilloux, Yannick,Mazzieri, Vanina A.,Pieck, Carlos L.
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p. 552 - 558
(2013/09/23)
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- The reaction and materials chemistry of [Sn6(O) 4(OSiMe3)4]: Chemical vapour deposition of tin oxide
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[Sn6(O)4(OSiMe3)4] and [{Sn(OSiMe3)2}2] have been used to deposit SnO thin films by chemical vapour deposition. Films derived from [Sn 6(O)4(OSiMe3)4] comprise uniform cubes and are highly oriented, whereas those deposited from [{Sn(OSiMe 3)2}2] are made up of a continuous non-oriented layer with oriented cubes on the surface. The structure of a co-crystal, 2 Sn6(O)4(OSiMe3)4× [Sn(OSiMe3)2]2×4 THF, shows that [{Sn(OSiMe3)2}2], a liquid at room temperature, adopts a μ-OSiMe3-bridged dimeric structure. [Sn 6(O)4(OSiMe3)4] reacts with O 2 in a controlled manner to afford the novel oxo-cluster [Sn 4(O)(OSiMe3)8], the structure of which is reported. In addition, a crystal of {[Sn4(O)(OSiMe3) 5]+2[Sn(O)(OSiMe3) 4Cl]+2}[Cl]-4 has been fortuitously isolated from the presence of SnCl2 in the starting material for the preparation of [Sn6(O)4(OSiMe 3)4], and has been shown to incorporate two novel cationic oxo-tin clusters. Copyright
- Barbul, Ioana,Johnson, Andrew L.,Kociok-Koehn, Gabriele,Molloy, Kieran C.,Silvestru, Christian,Sudlow, Anna L.
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p. 866 - 874
(2013/09/02)
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- Various metal nanoparticles produced by accelerated electron beam irradiation of room-temperature ionic liquid
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Various metal nanoparticles including base metal were produced by a brief accelerated electron beam irradiation of 1-alkyl-3-methylimidazolium bis((trifluoromethyl)sulfonyl)amide room-temperature ionic liquid without a stabilizing agent, which is usually employed so as to prevent aggregation.
- Tsuda, Tetsuya,Sakamoto, Taiki,Nishimura, Yoshitomo,Seino, Satoshi,Imanishi, Akihito,Kuwabata, Susumu
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p. 1925 - 1927
(2012/03/13)
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- Synthesis and characterization of Sn-rich Ni-Sb-Sn nanosolders
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Nano-crystalline samples of pure Sn and of Sn-rich ternary Ni-Sb-Sn alloys, with compositions ranging from 80 to 97.5 at% Sn and a Ni to Sb molar ratio of 1:1, were synthesized by reduction of stoichiometric metal chloride solutions with NaBH4 at 0 °C in alkaline medium. The particle sizes of the obtained alloys, measured by TEM/SEM, were found to be in the range of 40-350 nm. A relative decrease in melting temperature of up to 15 °C was observed for these alloys compared to a bulk sample. A sample with 95 at% Sn was subjected to heat treatment at 180 °C for various time periods up to 5.0 h to study particles with well defined average sizes between 50 and 135 nm. The melting temperatures of the annealed samples were found to increase progressively with increasing particle size. At the same time, the excess surface energy of these heat treated samples was measured as a function of particle size using a Calvet-type calorimeter. From the differences of the (H573-H299) values between nano and bulk samples, the excess enthalpies for nano-sized samples were derived to be between 18.8 ± 1.9 and 0.8 ± 1.4 kJ g-1 for particle sizes between 50 and 135 nm.
- Mishra, Ratikanta,Zemanova, Adela,Kroupa, Ales,Flandorfer, Hans,Ipser, Herbert
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p. 224 - 229
(2012/03/09)
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- Electrochemical performances of Sn anode electrodeposited on porous Cu foam for Li-ion batteries
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A three-dimensional Sn electrode is fabricated by the electrodeposition of Sn on a porous Cu foam substrate that consists of grape-like Cu nanodeposits. It is revealed from the XRD results that a small amount of Cu6Sn 5 is formed at the interface of Sn deposits and the Cu foam, thereby forming Sn-Cu6Sn5/Cu foam electrode. The electrode shows better cyclic performance and higher charge capacity than the Sn electrode electrodeposited on a smooth Cu foil does. The improved electrochemical performances of the Sn-Cu6Sn5/Cu foam electrode is due to the fact that the porous Cu foam accommodates the volumetric expansion of Sn-Cu6Sn5, and hence inhibits the pulverization or delamination of the active materials from the substrate. Furthermore, ex situ XRD analysis and SEM observation demonstrate that Sn deposits electrodeposited on the Cu foam are gradually blended with the Cu deposits, causing the transformation of Sn into Cu6Sn5. The phase transformation of Sn into Cu6Sn5 enhances the bonding force between the Sn and the Cu foam, and reducing the volume changes of active materials during cycling.
- Nam, Do Hwan,Kim, Ryoung Hee,Han, Dong Wook,Kwon, Hyuk Sang
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p. 126 - 132
(2012/07/14)
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- Sn-doped polyhedral In2O3 particles: Synthesis, characterization, and origins of luminous emission in wide visible range
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Sn-doped octahedronal and tetrakaidecahedronal In2O3 particles were successfully synthesized by simple thermal evaporation of indium grains using SnO as dopant. Structural characterization results demonstrated that the Sn-doped tetrakaidecahedronal In2O3 particle had additional six {001} crystal surfaces compared with the octahedronal one. The luminous properties of both samples were characterized by photoluminescence (PL) and cathodoluminescence (CL) spectroscopy. A broad visible luminous emission around 570 nm was observed. Studies revealed that the emission consisted of three peaks of 511 nm, 564 nm, and 622 nm, which were attributed to radioactive recombination centers such as single ionized oxygen vacancy, indium interstitial, and antisite oxygen, respectively. We believe that the Sn donor level plays an important role in the visible luminous emission.
- Zhu, Yunqing,Chen, Yiqing
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p. 182 - 188
(2012/03/12)
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- Hypervalent sulfur-functionalized diphosphagermylene and diphosphastannylene compounds
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The reaction between either GeCl2(1,4-dioxane) or SnCl 2 and 2 equiv of the lithium phosphide [{(Me3Si) 2CH}P(C6H4-2-SMe)]Li(tmeda) gives the corresponding diphosphatetrylenes [{(Me3Si)2CH}P(C 6H4-2-SMe)]2E [E = Ge (10), Sn (11)] in good yields. Both 10 and 11 crystallize as discrete monomers in which the Ge and Sn atoms are coordinated by both P and S atoms. Although 10 and 11 crystallize as racemic mixtures of the RR and SS diastereomers, variable-temperature NMR experiments suggest that, in solution, these compounds are in dynamic equilibrium with small amounts of the corresponding RS and SR diastereomers. DFT calculations reveal that the lowest-energy minima for both 10 and 11 possess rac stereochemistry; two higher-energy minima were located for each of 10 and 11, both of which have meso stereochemistry. The two calculated meso diastereomers differ in the location of the sulfur and phosphorus substituents within the pseudo-trigonalbipyramidal structures. Both 10 and 11 decompose on exposure to light, generating the diphosphine {(Me3Si) 2CH}(C6H4-2-SMe)P-P(C6H 4-2-SMe){CH(SiMe3)2} (14) as the major product.
- Izod, Keith,Clark, Ewan R.,Clegg, William,Harrington, Ross W.
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p. 246 - 255
(2012/05/04)
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- Stannylplumbylenes: Bonding between tetravalent tin and divalent lead
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Depending on stoichiometry, reactions of the mixed valence Sn(0)/Sn(iii) compound Sn(SnAr3)2 (1) (Ar = C6H 4(OiPr)2-2,6) with the likewise substituted plumbylene PbAr2 (3) afforded either the homoleptic distannylplumbylene Pb(SnAr3)2 (4) or the heteroleptic arylstannylplumbylene Pb(Ar)SnAr3 (5), a valence isomer of a stannaplumbene. The Royal Society of Chemistry 2012.
- Drost, Christian,Loennecke, Peter,Sieler, Joachim
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p. 3778 - 3780
(2012/06/04)
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- Activation of metallic aluminum by tin and gallium chlorides in oxidation with water
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We have studied the effect of gallium chloride and tin chloride solutions on the water oxidation of aluminum at SnCl2 concentrations of 0.68 and 6.32 wt %, GaCl3 concentrations of 0.56 and 2.67 wt %, and MCln : Al(M = Sn, Ga; n = 2, 3) molar ratios from 0.017 to 0.3. The results indicate that, when aluminum is oxidized in the presence of these salts, the reaction rate and hydrogen yield increase with reaction temperature and salt concentration and reach the highest levels when a mixture of gallium and tin chlorides is used. The reaction products are identified and the likely mechanism of the processes involved in the oxidation of aluminum is discussed. Pleiades Publishing, Ltd., 2012.
- Burlakova,Shilkin,Kravchenko,Dremova,Kravchenko,Ivanov,Bulychev
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p. 238 - 243
(2012/07/02)
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- Synthesis and characterization of highly conductive charge-transfer complexes using positron annihilation spectroscopy
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Molecular charge-transfer complexes of the tetramethylethylenediamine (TMEDA) with picric acid (Pi-OH), benzene-1,4-diol (QL), tin(IV) tetrachloride (SnCl4), iodine, bromine, and zinc chloride (ZnCl2) have been synthesized and investigated by elemental and thermal analysis, electronic, infrared, Raman and proton-NMR, energy-dispersive X-ray spectroscopy, X-ray powder diffraction and positron annihilation lifetime spectroscopy, and scanning electron microscopy. In this work, three types of acceptors π-acceptors (Pi-OH and QL), σ-acceptors (iodine and bromine), and vacant orbital acceptors (SnCl4 and ZnCl2) were covered. The results of elemental analysis indicated that the CT complexes were formed with ratios 1:1 and 1:2 for QL, SnCl4, and ZnCl2 acceptors and iodine, Pi-OH, and Br2 acceptors, respectively. The type of chelating between the TMEDA donor and the mentioned acceptors depends upon the behavior of both items. The positron annihilation lifetime parameters were found to be dependent on the structure, electronic configuration, and the power of acceptors. The correlation between these parameters and the molecular weight and biological activities of studied complexes was also observed. Regarding the electrical properties, the AC conductivity and the dielectric coefficients were measured as a function of frequency at room temperature. The TMEDA charge-transfer complexes were screened against antibacterial (Escherichia coli, Staphylococcus aureus, Bacillus subtilis, and Pseudomonas aeruginosa) and antifungal (Aspergillus flavus and Candida albicans) activities.
- Adam, Abdel Majid A.,Refat, Moamen S.,Sharshar,Heiba
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p. 458 - 477
(2012/07/17)
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- {4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C6H 2Sn}2: An intramolecularly coordinated organotin(I) compound with a Sn-Sn single bond, its disproportionation toward a diorganostannylene and elemental tin, and its oxidation with PhI(OAc) 2
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Syntheses of the intramolecularly coordinated organotin(I) compound {4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C6H 2Sn}2 (2), which crystallized in two different pseudopolymorphs 2 and 2·C7H8, of the diorganostannylene {4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C 6H2}2Sn (3) and of the organotin(II) acetate 4-t-Bu-2,6-[P(O)(O-i-Pr)2]2C6H 2SnOAc (4) are reported. The compounds were characterized by multinuclear NMR, IR (3 and 4), UV-vis spectroscopy (2), electrospray ionization mass spectrometry (3 and 4), and single-crystal X-ray diffraction analyses. Density functional theory calculations on compound 2 revealed the stabilizing effect of the intramolecular P=O → Sn coordination.
- Wagner, Michael,Dietz, Christina,Krabbe, Stefan,Koller, Stephan G.,Strohmann, Carsten,Jurkschat, Klaus
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p. 6851 - 6859
(2012/07/28)
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- Electrochemistry of tin in the 1-ethyl-3-methylimidazolium dicyanamide room temperature ionic liquid
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The electrochemistry of Sn(II) was studied in the room temperature ionic liquid 1-ethyl-3-methylimidazolium dicyanamide (EMI-DCA) on a glassy carbon (GC) and a polycrystalline Pt electrode at 40 °C. The Sn(II) species was introduced into the ionic liquid by either dissolution of SnCl2 or anodizing a Sn wire. The reduction potential of the Sn(II)/Sn couple produced in these two solutions was found to be different, indicating that different Sn(II) species may be present. The order of the reduction potential of the two Sn(II) species indicates that the Gutmann donor ability of the anions is likely to be DCA- > Cl-. Cyclic voltammetry indicates the stripping efficiency is >90% on the Pt but only 40% on the GC electrode. Analysis of the chronoamperometric transient behavior during electrodeposition suggests that the deposition of Sn on the GC electrode involves a three dimensional progressive nucleation on a finite number of active sites. The diffusion coefficient of SnCl2 dissolved in the EMI-DCA was found to be 9.8 × 10-7 cm2 s-1 which is in the same order of magnitude as those reported for SnCl2 in several other ionic liquids. Depending on the deposition potentials, potentiostatic electrolysis produced Sn deposits with various unusual morphologies such as hexagonal tubes, spiral nanowires, and dendrite.
- Leong, Tin-Iao,Hsieh, Yi-Ting,Sun, I-Wen
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p. 3941 - 3946
(2011/07/31)
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- The effect of tin content to the morphology of Sn/carbon nanofiber and the electrochemical performance as anode material for lithium batteries
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By using electrospinning and carbonization, tin nanoparticles enwrapped in carbon nano-fibers (Sn/C) present high capacity and well cyclic performance. The precursor compositions of SnCl2 and polyacrylonitrile (SnCl 2/PAN) have a significant effect on the crystal structure, morphology of Sn/C composites, and the electrochemical performance. Along with the increased concentration of tin in the precursors of SnCl2/PAN, the diameters of the carbonized Sn/C nanofibers are decreased. The samples of SnCl2/PAN with starting weight ratio 3:2 (Sn3Pan2), 1:1 (Sn1Pan1) and 2:3 (Sn2Pan3) present the initial discharge capacity 977.8, 1329.8, and 1137.0 mAh g-1, respectively. In the following cycles, the Sn/C nanofibers present high capacity and well cyclic performance. The sample Sn1Pan1 retains a charge capacity of 741.1 mAh g-1 (92% of the initial charge capacity) after 40 cycles. Because the nanoparticles of tin metal are enwrapped in carbon nanofibers, the volume change and aggregation of metal anode are decreased during charging and discharging processes.
- Wang, Haiying,Gao, Po,Lu, Saifeng,Liu, Haidong,Yang, Gang,Pinto, Jo?o,Jiang, Xuefan
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- Solvothermal synthesis of carbon-coated tin nanorods for superior reversible lithium ion storage
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This paper reports the large-scale synthesis of carbon-coated tin (Sn-C) nanorods through a facile solvothermal carbonization approach by using Sn nanorods as templates and ethanol as a solvent. The as-synthesized Sn-C nanorods have been applied as anode materials for lithium-ion batteries. The Sn-C anode, which exhibits relatively higher initial Coulombic efficiency and lithium storage capacities, is more attractive than the previously reported tin oxide or sulfide anodes. The superior performance of the Sn-C nanorods makes it a promising anode material in high-energy density batteries.
- Wu, Ping,Du, Ning,Liu, Jie,Zhang, Hui,Yu, Jingxue,Yang, Deren
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p. 2278 - 2282
(2012/01/04)
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- High reversible capacity of SnO2/graphene nanocomposite as an anode material for lithium-ion batteries
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A gas-liquid interfacial synthesis approach has been developed to prepare SnO2/graphene nanocomposite. The as-prepared nanocomposite was characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, and Brunauer-Emmett-Teller measurements. Field emission scanning electron microscopy and transmission electron microscopy observation revealed the homogeneous distribution of SnO2 nanoparticles (2-6 nm in size) on graphene matrix. The electrochemical performances were evaluated by using coin-type cells versus metallic lithium. The SnO2/graphene nanocomposite prepared by the gas-liquid interface reaction exhibits a high reversible specific capacity of 1304 mAh g-1 at a current density of 100 mA g-1 and excellent rate capability, even at a high current density of 1000 mA g-1, the reversible capacity was still as high as 748 mAh g-1. The electrochemical test results show that the SnO2/graphene nanocomposite prepared by the gas-liquid interfacial synthesis approach is a promising anode material for lithium-ion batteries.
- Lian, Peichao,Zhu, Xuefeng,Liang, Shuzhao,Li, Zhong,Yang, Weishen,Wang, Haihui
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p. 4532 - 4539
(2011/06/22)
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- Elaborated 1H NMR study for the ligitional behavior of two thiosemicarbazide derivatives towards some heavy metals (Sn(II), Sb(III), Pb(II) and Bi(III)), thermal, antibacterial and antifungal studies
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A new series of heavy metal complexes are prepared. Sn(II), Sb(III), Pb(II) and Bi(III) are the metal ions used in complexation with two thiosemicarbazide ligands. The IR and 1H NMR spectra of the free ligands display their presence in thiole-thione forms coincide with each other. The IR spectra of the complexes support the presence of 2:2 molar ratio (M:HL) with HL1 ligand and 1:1 beside 1:2 with HL2. The ligand coordinates as bi molecules in some complexes and displays two tautomer forms at the same complex molecule 1H NMR spectra of Sn(II) and Sb(III) complexes were done and comes coincide with IR data. The electronic spectral analysis displays a lower shift appearance in n → π* charge transfer band in most isolated complexes. As well as, a new band is shinned in visible region with Sb(III), Bi(III) complexes and Sn(II)-HL2. This band is pointed to its use in spectrophotometric analysis for these metal ions. The TG analysis for all isolated compounds was briefly discussed. The molecular modeling parameters support the stability of thiole form of the free ligands in comparing with their thiones by a small difference. The antibacterial and antifungal activities were studied against some organisms and reveal the priority of most investigated complexes.
- El-Metwaly, Nashwa M.,Refat, Moamen S.
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p. 519 - 528
(2011/11/29)
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- Sn diffusion during Ni germanide growth on Ge1- xSnx
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We report on the redistribution of Sn during Ni germanide formation on Ge1-xSnx/Ge(100) and its influence on the thin filmgrowth and properties. These results show that the reaction involves th e formation of Ni5Ge3 and NiGe. Sn redistributes homogenously in both phases, in which the Sn/Ge ratio retains the ratio of the as-deposited Ge1-xSnx film. Sn continues to diffuse after full NiGe formation and segregates in two regions: (1) at the interface between the germanide and Ge1-xSnx and (2) at the surface, which has major implications for the thin film and contact properties.
- Demeulemeester, J.,Schrauwen, A.,Nakatsuka, O.,Zaima, S.,Adachi, M.,et al.
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- Effect of the temperatures on structural and optical properties of tin oxide (SnOx) powder
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A series of composite SnOx materials were prepared by SnO powder heating at different temperatures in air for 2 hr. Depending on treatment conditions it was found that SnO, with its tetragonal structure, could transform into the Sn phase or tetragonal SnO and tetragonal SnO2. The influence of heating at different temperatures on the properties of SnOx has been studied. The influences of annealing temperatures in air on the structural and optical properties of SnOx have been investigated. Correlations between the structural and optical properties of the products were found.
- Hadia,Ryabtsev,Seredin,Domashevskaya
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p. 313 - 317
(2010/05/01)
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- Charge-discharge characteristics of a layered-structure electroplated Cu/Sn anode for Li-ion batteries
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An electroplated copper/tin (Cu/Sn) anode with a layered structure is described that minimizes the high-voltage irreversible capacity observed in an electroplated Sn anode at a potential over 1 V. The high-voltage irreversible capacity is caused by the electrolyte decomposition at the catalytic site of the Sn anode. In the electroplated Cu/Sn anode, the upper Cu layer effectively suppresses the exposure of the newly formed Sn surfaces, resulting in the absence of the high-voltage irreversible capacity. Therefore, the electroplated Cu/Sn anode exhibits a higher cycle performance than the electroplated Sn anode.
- Park, JungWon,Eom, JiYong,Kwon, HyukSang
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p. 1825 - 1828
(2010/06/12)
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- Sn(I) halides: Novel binary compounds of tin and their application in synthetic chemistry
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Metalloid cluster compounds are ideal model compounds for the area between the molecular and solid state, i.e. the nanometer regime. For the synthesis of metalloid cluster compounds, the disproportionation reaction of a metastable subhalide is a fruitful synthetic route. In the case of tin, monohalides are needed for this synthetic route as tin(II) halides are too stable to be used. Due to thermodynamic data, gaseous SnBr should be formed at 1370 °C, and by applying a co-condensation technique it can be trapped at -196 °C and prepared in synthetic scale. Herein first analyses of SnBr are presented, showing that SnBr is more reactive than the corresponding GeBr, already disproportionating quantitatively to elemental tin and SnBr2 on heating to room temperature. By applying nitrogen-based donor molecules like NnBu3 or pyridine, the reactivity can be moderated and the solubility is enhanced leading e.g. to an SnBr emulsion, which can be used for the synthesis of metalloid cluster compounds of tin.
- Pacher, Andreas,Schrenk, Claudio,Schnepf, Andreas
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p. 941 - 944
(2010/06/14)
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- Bimetallic multidimensional supramolecular coordination polymers containing triphenyltin cation and CuCN
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The reaction of K3[Cu(CN)4] in H2O with a solution of Ph3SnCl and 4-methylpyrimidine (mpym) in acetonitrile affords, at room temperature, the white powder [(Ph3Sn) 3Cu(CN)4.mpym·H2O], II, precipitating in the mother liquor and colourless platelet crystals [(Ph3Sn) 2Cu(CN)3], I, which was obtained from the filterate after two days. The copper site in I assumes distorted trigonal plane geometry. The network structure of I is constructed via 3D-puckered layers constructed of infinite parallel [CuCN-(μ-Ph3Sn)-CN] chains forming waves where the CNSnPh3 fragments locate the peak and bottom positions of the waves as side arms. The 2D-layers are connected by hydrogen bonds and π-π stacking. This is the first example for a Cu-coordination polymer containing the tetrahedral and bipyramidal configured tin atoms. The pyramidal tetrahedral [Cu(CN)4]3- anion, in II, are interconnected by two kinds of nanometer spacers; -CN→Sn(Ph3)←O(H)H...NC- and -CN→Sn(Ph3)-N(mpym)N-Sn(Ph3)←NC- creating super-Prussian blue 3D-network structure. The reaction of K3[Cu(CN) 4] in H2O with a solution of Ph3SnCl and 4-methylpyrimidine (mpym) in acetonitrile affords, at room temperature, the white powder [(Ph3Sn)3Cu(CN)4. mpym·H2O], II, precipitating in the mother liquor and colourless platelet crystals [(Ph3Sn)2Cu(CN)3], I, which was obtained from the filtrate after two days. The copper site in I assumes trigonal bipyramidal configuration. The network structure of I is constructed via 3D-puckered layers constructed of infinite parallel [CuCN-(μ-Ph3Sn)-CN] chains forming waves where the CNSnPh 3 fragments locate the peak and bottom positions of the waves as side arms.
- Etaiw, Safaa Eldin H.,Fayed, Tarek A.,Abdou, Safaa N.
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p. 1918 - 1923
(2010/09/09)
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