- A facile route to fabricate single-crystalline antimony nanotube arrays
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Single-crystalline antimony nanotube arrays are fabricated in the anodic alumina membranes using the pulsed electrodeposition technique for the first time. The thickness of Au layer sputtered on the anodic alumina membrane and the pulsed electrode-position technique are two key factors to produce single-crystalline nanotubes. Copyright
- Li, Liang,Xiao, Yanhe,Yang, Youwen,Huang, Xiaohu,Li, Guanghai,Zhang, Lide
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- Thermal behavior of antimony nanowire arrays embedded in anodic aluminum oxide template
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Highly oriented single crystal antimony nanowire arrays have been synthesized within anodic aluminum oxide (AAO) template by pulsed electrodeposition. Thermal behavior and oxidation analysis of the antimony nanowires have been investigated by means of thermogravimetry and differential scanning calorimetry in Ar and air atmosphere, respectively. Compared to bulk antimony, the antimony nanowires exhibit a lower sublimation temperature at 496.4°C. Evident oxidation of the Sb nanowires occurs at 429.8°C in air atmosphere and α-Sb2O4 nanowires have been obtained as the oxidation product. The results indicate that the sublimation and the oxidation of the antimony nanowires in the AAO template is a slow multi-step process. The present results are of relevance when processing antimony nanowries for thermoelectric applications at high temperatures.
- Zhang,Ding,Zhang,Hao,Meng,Zhang
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- Chemistry of polyfunctional molecules - 123.1 reactions of BiBr3, SbI3 and AsI3 with LiN(PPh2)2; X-ray structure of a cyclophosphazene salt containing arsenic(I)
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BiBr3 or SbI3 react at 20°C with LiN(PPh2)2 (1) to give elementary Bi or Sb and the P-P coupled phosphazene ligand Ph2P-N=PPh2-PPh2=N-PPh2 (2). The reaction of AsI3 with 1 at room temperature formed yellow needles of the eight-membered heterocycle AsPPh2NPPh2AsPPh2NPPh2 (3), whereas AsI3 interacted at 80°C with 1 in the molar ratio of 1:3 to give elementary arsenic and 2. Treatment of AsI3 and 1 at 20°C in a 1:2 stoichiometry yielded the seven-membered, cyclic arsenium (I) salt [As-...PPh2-N=PPh2-PPh2=N-PPh 2] I · 4THF (5 · 4THF), which was characterized by elemental analysis, conductivity, mass, IR and NMR spectroscopy and single-crystal X-ray structural analysis. Copyright
- Dotzler, Martina,Schmidt, Astrid,Ellermann, Jochen,Knock, Falk A.,Moll, Matthias,Bauer, Walter
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- Solution synthesis of a new thermoelectric Zn1+ xSb nanophase and its structure determination using automated electron diffraction tomography
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Engineering materials with specific physical properties have recently focused on the effect of nanoscopic inhomogeneities at the 10 nm scale. Such features are expected to scatter medium- and long-wavelength phonons thereby lowering the thermal conductivity of the system. Low thermal conductivity is a prerequisite for effective thermoelectric materials, and the challenge is to limit the transport of heat by phonons, without simultaneously decreasing charge transport. A solution-phase technique was devised for synthesis of thermoelectric Zn4Sb3 nanocrystals as a precursor for phase segregation into ZnSb and a new Zn-Sb intermetallic phase, Zn 1+δSb, in a peritectoid reaction. Our approach uses activated metal nanoparticles as precursors for the synthesis of this intermetallic compound. The small particle size of the reactants ensures minimum diffusion paths, low activation barriers, and low reaction temperatures, thereby eliminating solid-solid diffusion as the rate-limiting step in conventional bulk-scale solid-state synthesis. Both phases were identified and structurally characterized by automated electron diffraction tomography combined with precession electron diffraction. An ab initio structure solution based on electron diffraction data revealed two different phases. The new pseudo-hexagonal phase, Zn1+δSb, was identified and classified within the structural diversity of the Zn-Sb phase diagram.
- Birkel, Christina S.,Mugnaioli, Enrico,Gorelik, Tatiana,Kolb, Ute,Panthoefer, Martin,Tremel, Wolfgang
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- Preparation and electrochemical properties of binary SixSb immiscible alloy for lithium ion batteries
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The novel binary SixSb immiscible alloy was synthesized using chemical reduction-mechanical alloying methods and first investigated as possible anodes for lithium ion batteries. The microstructures, morphologies and electrochemical properties were investigated utilizing X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), constant-current charge/discharge tests, cyclic voltammetry and electrochemical impedance spectroscopy (EIS). Results showed that tiny Si particles were dispersed homogeneously in Sb active matrix. Cyclic voltammetry results indicated that the Li+-transport rates were significantly enhanced in the Si xSb immiscible alloy. Results also showed that the Si0.8Sb exhibited the best cyclability with a reversible capacity of 596.4 mAh g -1 after 50 cycles. The cyclability can be improved by restricting either the upper or lower cutoff voltage, which can control the lithiation/delithiation degree and prevented the powdering and shredding of the active materials after Li+ trapped into electrode materials.
- Wang, Jingwei,Wang, Yang,Zhang, Peixin,Zhang, Dongyun,Ren, Xiangzhong
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- Preparation of nanosized antimony by mechanochemical reduction of antimony sulphide Sb2S3
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The preparation of nanosized antimony (grain size 19 nm) by high-energy milling of antimony sulphide Sb2S3 with elemental Fe as reducing element is reported. The mechanochemical reduction was performed in a planetary ball mill for 10-180 min. The process is rather straightforward with elemental antimony and iron sulphide (pyrrhotite-4H) being the only solid-state products. The process kinetics as described by X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) magnetometry shows that most of the reduction is complete after 60 min of milling.
- Balá?,Takacs,Godo?íková,?korvánek,Ková?,Choi
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- Antimony film electrode for direct cathodic measurement of sulfasalazine
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The antimony film electrode (SbFE) is presented for the first time for direct cathodic voltammetric measurement of an organic compound, i.e. sulfasalazine, which has been chosen due to its aptness for electrochemical reduction and its great importance as a pharmaceutical product. The SbFE was prepared ex situ on the surface of a glassy carbon supporting electrode and several important parameters were studied and optimized, such as preparation of the SbFE, stripping voltammetric settings, pH of the measurement solution, etc. In addition, the electroanalytical performance of the SbFE was compared to its bismuth counterpart and bare glassy carbon electrode. The SbFE exhibited excellent linear dependence in the examined concentration range of 3 × 10-6-2.5 × 10-4 M together with the detection limit of 7.8 × 10-7 M and good reproducibility with the RSD of ±0.7%. Finally, the applicability of the SbFE was successfully demonstrated through convenient measurements of sulfasalazine in its dosage forms of sulfasalazine delayed-release tablets.
- Nigovi?, Biljana,Hocevar, Samo B.
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- Chalcogenolato Complexes of Bithmuth and Antimony. Syntheses, Termolysis Reactions, and Crystal Structure of Sb(SC6H2(i-Pr)3-2,4,6)3
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Antimony(III) and bismuth(III) complexes of sterically demanding arenechalcogenolato ligands, M(EC6H2R'3-2,4,6)3 (E = S or Se; M = Sb or Bi; R' = Me, i-Pr or t-Bu) have been prepared by either protolysis of the amides M3 with arenechalcogenols, or from MCl3 by halide exchange (M = Bi or Sb).The complexes are monomeric in the solid state and sublime readily.The crystal structure of Sb(SC6H2(i-Pr)3-2,4,6)3 has been determined by X-ray diffraction.The compound possesses a trigonal-pyramidal geometry, with Sb-S distances of 2.418(2)-2.438(2) Angstroem and S-Sb-S angles of 94.69(7)-98.29(8) deg.Preliminary X-ray results on Bi(SeC6H2(i-Pr)3-2,4,6)3 showed that the compounds of Sb and Bi are isostructural.Thermolytic decomposition of some of the compounds has been carried out in the solid state.Compounds with R' = Me or i-Pr undergo reductive elimination to give elemental bismuth or antimony, whereas the bulky selenolates M(SeC6H2(t-Bu)3-2,4,6)3 afford M2Se3.
- Bochmann, Manfred,Song, Xuejing,Hursthouse, Michael B.,Karaulov, Alexander
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- Scalable synthesis of Sb(III)Sb(V)O4 nanorods from Sb 2O5 powder via solvothermal processing
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Scalable Sb(III)Sb(V)O4 nanorods from Sb2O 5 powder were prepared using solvothermal route. XRD and HRTEM demonstrate that the nanorods are single-crystal orthorhombic-Sb 2O4 phase with several micrometers long and 200-300 nm diameter size. XPS result further shows that the antimony cations in the nanorods are composed of three valence and five valence antimony ions. The emission of the nanorods appears around 450 nm wavelength. The formation mechanism of the Sb(III)Sb(V)O4 nanorods was discussed in detail.
- Ji, Tianhao,Tang, Maoyu,Guo, Lin,Qi, Xingyi,Yang, Qinglin,Xu, Huibin
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- Phase stability and thermoelectric properties of Cu10.5Zn1.5Sb4S13 tetrahedrite
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Cu10.5Zn1.5Sb4S13 tetrahedrite compound was prepared by mechanical milling of Cu2S, ZnS and Sb2S3 powders and spark plasma sintered (SPS) to dense samples. The phase formation, chemical homogeneity, thermal stability of the compound and the thermoelectric properties of the sintered samples were evaluated. Single phase tetrahedrite with the crystallite size of 40 nm was obtained after 30 h of milling followed by annealing at 573 K for 6 h in an argon atmosphere. In-situ high-temperature X-ray diffraction studies revealed that the phase is stable up to 773 K. The Seebeck coefficient of the sintered samples of density >98% shows p-type behavior with maximum thermopower of 170 μV/K at 573 K. The electrical resistivity (ρ) decreases with temperature up to 475 K and then increases. A low thermal conductivity of 0.5 W/(m?K), in combination with moderate power factor gave a maximum ZT of ~0.038 at 573 K in Cu10.5Zn1.5Sb4S13 sample having a grain size of ~200 nm.
- Harish, Subramaniam,Sivaprahasam, Duraisamy,Battabyal, Manjusha,Gopalan, Raghavan
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- Influence of temperature and of structure of antimony substrate on gallium diffusion into the GaSb semiconductor compound
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The diffusion coefficient of Ga electrodeposits on Sb electrodeposited thin films, either amorphous or crystalline, was investigated to determine the influence of the morphology and structure of the antimony substrates on the diffusion and reaction process. The Ga/Sb bilayer was studied by SEM-EDS and X-ray diffraction before and after heating at temperatures of 50, 75 and 100 °C. The formation of the GaSb semiconductor compound was particularly considered and the activation energy and frequency factor of the process was determined. At these temperatures, Ga was at least partially molten and the diffusion coefficient showed that the geometrical factor was prevailing over the structural one. For example, at 75 °C, the values of the diffusion coefficient were 1.5×10-17 and 6.3×10-17 m2 s-1 for the amorphous and crystalline antimony, respectively. On the contrary, at 20 °C, a temperature at which Ga is in the solid state, the structural factor prevailed over the geometrical one and values were obtained lower by around three orders of magnitude. The prevailing influence at 20 °C was identical to that previously observed for In diffusion into amorphous and crystalline Sb with InSb formation. The experimental results, both at low and high temperatures, are discussed also taking the behaviour of the In-Sb system into account.
- Kozlov, Valentin M.,Peraldo Bicelli, Luisa
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- Thermoelectric properties of the Ru2Ni2Sb 12 ternary skutterudite
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The synthesis of the Ru2-xNi2-xSb12 compounds (0≤x≤0.2), their structural characterization and temperature dependencies of selected transport and thermal properties are reported. At x=0, Ru2-xNi2-xSb12 displays cubic symmetry, space group Im3 with lattice parameter a=9.1767(1) A. From increasing electrical conductivity above 600 K the band gap (Eg~0.06 eV) was estimated using an Arrhenius plot. Different signs of the Seebeck coefficient (negative) and the Hall coefficient (positive) have been explained as a consequence of a multicarrier transport. The substitution on a cation site, i.e., formation of the Ru2-xNi2-xSb12 ternary skutterudites proved to be effective way in suppressing of the thermal conductivity.
- Navratil, Jiri,Laufek, Frantisek,Plechacek, Tomas,Drasar, Cestmir
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- Synthesis and Structural Evolution of RuSb3, a New Metastable Skutterudite Compound
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A thin-layer synthesis technique was used to synthesize bulk amounts of the metastable phase, RuSb3, a novel compound with the skutterudite structure. The compound crystallized at 350 °C and was stable to 525 °C. When annealed above 550 °C, it decomposed into RuSb2 and Sb. Rietveld refinement of X-ray diffraction data showed the presence of excess Sb residing in the interstitial site in the skutterudite structure. X-ray diffraction and thermal analysis experiments allowed us to examine the evolution of the sample as a function of annealing and determine the reaction pathway. The activation energy for the crystallization of the compound was determined to be 3 eV/nucleation event, while the activation energy for decomposition was approximately 8 eV.
- Smalley, Arwyn L. E.,Jespersen, Michael L.,Johnson, David C.
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- Reaction of arsane with cobalt or iron carbonyls, and the X-ray crystal structures of 4-As)>2 and 4-AsCo3(CO)8>3
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Reaction of AsH3 with Fe(CO)5 in a hydrocarbon solvent at 110 deg C provides an improved route to (μ3-As)2Fe3(CO)9, while the corresponding reaction at 70 deg C with Fe2(CO)9 has given the new cluster 4-As)>2, which has been shown by X-ray crystallography to consist of four AsFe2 triangles linked by spiro-As atoms and an Fe-Fe edge.The reaction at 20 deg C of AsH3 with Co2(CO)8 gave the known trimer 4-AsCo3(CO)9>3 which was fully characterised by an X-ray diffraction study.
- Arnold, Leslie J.,Mackay, Kenneth M.,Nicholson, Brian K.
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- Nanoscale electrocrystallisation of Sb and the compound semiconductor AlSb from an ionic liquid
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Aluminium antimonide nanoclusters with an apparent band gap energy of 0.92 ± 0.2 eV have been electrodeposited from the neutral ionic melt AlCl 3-1-butyl-3-methylimidazolium chloride {AlCl3-[C 4mim]+Cl-/su
- Aravinda,Freyland
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- Chemical route for formation of intermetallic Zn4Sb3 phase
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Synthesis of intermetallic zinc antimonide phases via low temperature solution route was investigated. Trial experiments were carried out under inert atmosphere at 70 °C using metallic Zn, SbCl3 and NaBH4 as reactants and tetrahydrofuran (THF), dimethylsulfoxide (DMSO) as organic media. Powder X-ray analysis confirmed the nucleation and growth of ZnSb phases in presence of excess Zn. SEM analysis revealed the existence of core-shell structure comprising of Zn core and Sb shell. Such particles get transformed into Zn4Sb3 crystalline phases upon thermal treatment at 300 °C/6 h in a silica tube closed under high secondary vacuum.
- Denoix,Solaiappan,Ayral,Rouessac,Tedenac
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- Synthesis and sodium storage performance of Sb porous nanostructure
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Porous Sb nanostructure has been prepared via a magnesiothermic reduction reaction and a succedent HCl solution etching process. The Sb product is made up of connected uniform porous particles. The pores have an average pore size of ~80 nm. Sodium storage performance of porous Sb product has been investigated. An initial reversible capacity of 570.3 mAh/g was obtained at 50 mA/g. At the 50th cycle, a reversible capacity of 538.7 mAh/g was retained, corresponding to a high retention rate of 94.5percent.
- Shi, Liang,Wang, Wenhui
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- Thermally stable thermoelectric Zn4 Sb3 by zone-melting synthesis
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The thermal stability of thermoelectric Zn4 Sb3 has been investigated on samples produced by a new zone-melting technique, as well as by the conventional quench method. The multitemperature synchrotron powder diffraction data reveal that while conventionally synthesized, Zn4 Sb3 samples have almost 40% degradation in the first heating cycle at 625 K, samples prepared by zone melting only have 3% degradation. Repeated thermal cycling induces additional degradation of the quenched sample of up to 58%, compared to ~9% degradation in the zone-melted sample. Thus, zone-melting produces Zn4 Sb3 samples that are significantly more thermally stable, which make them promising for commercial implementation.
- Pedersen,Iversen
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- Growth of Sb2O3 nanotubes via a simple surfactant-assisted solvothermal process
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Sb2O3 nanotubes were successfully prepared via a simple surfactant-assisted solvothermal method. The nanotubes have an orthorhombic structure with outer diameter range from 40 to 150 nm, the wall thickness of 10 to 40 nm and a length of up to several micrometers. The formation of nanotubes followed a rolling-up mechanism.
- Zhang, Yunxia,Li, Guanghai,Zhang, Lide
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- A rational complexing-reduction route to antimony nanotubes
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Antimony nanotubes with inner diameters of 15-80 nm, wall thickness of 10-30 nm and lengths of up to several micrometers have been successfully prepared by a rational complexing-reduction route using zinc powder as reductant at low temperature (80-140°C).
- Hu, Hanmei,Mo, Maosong,Yang, Baojun,Shao, Mingwang,Zhang, Shuyuan,Li, Qiaowei,Qian, Yitai
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- Thin films of Cu2Sb and Cu9Sb2 as anode materials in Li-ion batteries
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Thin Cu2Sb films have been prepared by heat-treating Sb films, electrodeposited on Cu substrates. The influence of the electrodeposition conditions and the heat-treatment period on composition and morphology of the films were investigated (SEM and XRD) and the obtained films were tested as anode materials for Li-ion batteries. The Cu2Sb material showed a stable capacity of 290 mAh g-1 (close to the theoretical capacity of 323 mAh g-1) during more than 60 cycles. The presence of 9-11% (w/w) Sb2O3 in the electrodeposited films resulted in smaller particles but also slowed down formation of Cu2Sb during the heat-treatment step. The presence of Sb2O3 was found to decrease the cycling stability although structural reversibility of Cu2Sb was obtained both with and without Sb2O3. Longer heat-treatments of pure Sb films resulted in the formation of Cu9Sb2 which was shown to be reduced at a lower potential than Cu2Sb. The Cu9Sb2 was converted to Cu2Sb during repeated cycling and the capacity of the latter Cu2Sb material was found to be 230 mAh g-1. While reduction of the materials was complicated by simultaneous formation of an SEI layer, three plateaus could be identified during the oxidation of Li3Sb, indicating the presence of three separate one-electron oxidation reactions.
- Bryngelsson, Hanna,Eskhult, Jonas,Nyholm, Leif,Edstr?m, Kristina
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- An Investigation of the Titanium-Antimony-Oxygen System by X-Ray Diffraction, Antimony-121 Moessbauer Spectroscopy, and Temperature-programmed Reduction
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Titanium -antimony oxides have been prepared by precipitation methods and investigated by a number of techniques.Powder X-ray diffraction has shown the initial precipitates to be amorphous materials which begin to form distinguishable crystalline phases when calcined in air at temperatures exceeding ca. 500 deg C.The nature of the crystalline phases depends on the relative concentration of the titanium and antimony cations in the initial precipitates and the calcination temperatures.The oxidation states of antimony in the materials have been determined by antimony-121 Moessbauer spectroscopy.The materials formed at temperatures exceeding 1000 deg C may be described as solid solutions of ca. 4 percent antimony(V) in titanium(IV) oxide.The reducibility of some amorphous hydroxides and crystalline oxides of titanium and antimony when treated in hydrogen and the nature of the reduction products has been studied by temperature-programmed reduction and antimony-121 Moessbauer spectroscopy.The results demonstrate the complementary nature of the two techniques and their capacity to examine the character of reduction processes in the amorphous and crystalline solid state.Similar investigations of the titanium-antimony oxides showed that the reduction properties of the materials in hydrogen are sensitive to the precalcination history and antimony concentration.Low concentrations of antimony in the mixed oxide phases dried in air at low temperatures suffered facile reduction in hydrogen at moderate temperatures, whereas similar concentrations of antimony(V) in titanium dioxide formed by high-temperature calcination were particularly stable to reduction in hydrogen.
- Berry, Frank J.,Gogarty, Patricia M.,Jenkins, John W.
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- Soft-Chemical Method for Synthesizing Intermetallic Antimonide Nanocrystals from Ternary Chalcogenide
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The synthesis of intermetallic antimonides usually depends on either the high-temperature alloying technique from high-purity metals or the flux method in highly poisonous Pb-melt. In this paper, we introduced a soft-chemical method to synthesize intermetallic antimonides from ternary chalcogenide precursors under an argon atmosphere below 200 °C. Powder X-ray diffraction and compositional analysis clearly indicate that a new phase of the Ag3Sb nanocrystal was synthesized from the Ag3SbS3 precursors. Three types of trialkylphosphines (TAPs) were applied as desulfurization agents, and the transformation mechanism was elucidated. The capability of the desulfurization agent follows the sequence of triphenylphosphine (TPP) > tributylphosphine (TBP) > trioctylphosphine (TOP). Besides, this TAP-driven desulfurization route to synthesize the intermetallic phase could also be possible for AgSbSe2 and Sb2S3. Therefore, this paper provides an efficient and mild technique for the fabrication of intermetallic nanocrystals.
- Jiang, Yilan,Yuan, Long,Xu, Yanyan,Ma, Jiaojiao,Sun, Yu,Gao, Xia,Huang, Keke,Feng, Shouhua
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- Antimony nanowires self-assembled from Sb nanoparticles
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For the first time, we introduced a simple method of synthesizing segregated thin antimony nanowires based on the principle that nanoparticles can spontaneously self-assemble into crystalline nanowires (a??20 nm) in the absence of any rigid templates at room temperature. By collecting electron energy loss spectra from individual Sb nanowires with different diameters, we investigated the effect of nanowire diameter on plasmon excitations in Sb nanowires. As the diameter of Sb nanowire decreases, we find that the peak energy of surface plasmon shifts toward the lower energy.
- Wang, Ye Wu,Hong, Byung Hee,Lee, Ju Young,Kim, Jeong-Sun,Kim, Geun Hong,Kim, Kwang S.
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- Thermal reduction of mechanically activated cinnabar (HgS) and stibnite (Sb2S3)
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The reduction of cinnabar (HgS) and stibnite (Sb2S3) by hydrogen was investigated. These investigations were performed in the temperature region 636-765 K for cinnabar and in the region 825-954 K for stibnite. It has appeared that the mechanical activation positively affects the thermal reduction of the sulphides. The thermal decomposition of HgS is accompanied by a change in mechanism taking place at 744 K. As to Sb2S3, the change in mechanism in the investigated temperature region was not observed.
- Balaz,Godocikova
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- Synthesis of colloidal InSb nanocrystals via in situ activation of InCl3
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Indium antimonide (InSb), a narrow band gap III-V semiconductor is a promising infrared-active material for various optoelectronic applications. Synthetic challenge of colloidal InSb nanocrystals (NCs) lies in the limited choice of precursors. Only a few successful synthetic schemes involving highly toxic stibine (SbH3) or air- and moisture-sensitive metal silylamides (In[N(Si-(Me)3)2]3 or Sb[N(Si-(Me)3)2]3) as the precursor have been reported. We found that commercially available precursors InCl3 and Sb[NMe2]3 directly form highly crystalline colloidal InSb nanocrystals in the presence of a base such as LiN(SiMe3)2 or nBuLi. The mean size of the particles can be controlled by simply changing the activating base. This approach offers a one-pot synthesis of InSb NCs from readily available chemicals without the use of complex organometallic precursors.
- Tamang, Sudarsan,Kim, Kyungnam,Choi, Hyekyoung,Kim, Youngsik,Jeong, Sohee
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- Mechanism of formation and electronic structure of semiconducting ZnSb nanoclusters electrodeposited from an ionic liquid
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Electrocrystallization of Sb and the compound semiconductor ZnSb has been investigated by in situ SPM methods at the electrified ionic liquid/Au(1 1 1) interface at an elevated temperature of 50 °C for the first time employing the ionic liquid ZnCl2-[C4mim]+Cl- (45:55). Prior to the underpotential deposition (UPD) process of Sb, ZnCl3- anions adsorb on the gold surface at the open-circuit potential (OCP). An ordered region - showing the characteristic of a Moire?-like pattern - coexists with a disordered region indicative of an interfacial phase transition. When the potential is reduced to -0.40 V versus Pt/Pt(II), 2D electrocrystallization of Sb starts showing a typical fenced(sqrt(3) × sqrt(3)) structure of the first monolayer. Further decreasing the potential to -0.5 V a second layer of Sb islands occurs. Stepping the potential from the UPD region to -0.60 V, the OPD of Sb sets in showing randomly dispersed clusters of homogeneous size. Near the ZnSb deposition potential, at ~-0.95 V, a nearly homogeneous distribution of clusters of spherical shape with diameters up to 15 nm is found. Their corresponding STS curves exhibit an obvious semiconducting behaviour with a gap-energy of ~0.6 ± 0.2 eV. Experiments at deposition conditions on the Sb-rich or Zn-rich side relative to the ZnSb deposition potential show an obvious doping effect - in the case of Zn excess - which is revealed by the corresponding normalized conductance (NC) spectra.
- Mann, Olivier,Freyland, Werner
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- Extending the time: Solvothermal syntheses, crystal structures, and properties of two non-isostructural thioantimonates with the composition [Mn(tren)]Sb2S4
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The two novel compounds, [Mn(tren)]Sb2S4 (1 and 2), were obtained by the reaction of elemental Mn, Sb, and S in aqueous solutions of tren (tren = tris(2-aminoethyl)amine, C6H18N4) after different reaction times. Compound 1 is formed up to a reaction time of 13 d, and an extension of the reaction time leads to the formation of 2. Both compounds crystallize in monoclinic space groups (1, P21/c, 2, C2/c). In 1, the two unique SbS3 trigonal pyramids share a common S atom to form a Sb2S5 unit. Two S atoms of this group have a bond to Mn2+ yielding a MnSb2S3 heteroring in the boat conformation. The Sb2S5 moieties are joined via common corners into the final undulated ∞1[Sb 2S4]2- anion which is directed along [001]. The structure of 2 contains the [Mn(tren)]2+ ion, one SbS3 pyramid, and a SbS4 unit. Two symmetry-related SbS4 groups share an edge, forming a Sb2S6 group containing a Sb 2S2 ring. This group is joined via corners to two SbS 3 pyramids on both sides producing a Sb4S4 ring. The Sb2S2 and Sb4S4 rings are condensed into the final ∞1[Sb2S 4]2- anion which runs along [010]. The [Mn(tren)] groups are bound to the thioantimonate(III) backbone on opposite sides of the Sb 4S4 ring, and a small MnSbS2 ring is formed. In both structures, weak S...H bonds are found which may contribute to the stability of the materials. The two compounds decompose in one step upon heating, and only MnS and Sb2S3 could be identified as the crystalline part of the decomposition products. Both compounds can also be prepared under solvothermal conditions using MnSb2S4 as starting material. Compounds 1 and 2 are obtained from this ternary material in a high yield.
- Schaefer, Michael,Kurowski, Daniel,Pfitzner, Arno,Naether, Christian,Rejai, Zomaje,Moeller, Karina,Ziegler, Nancy,Bensch, Wolfgang
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- Characterization of CuSbSe2 crystallites synthesized using a hot injection method
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In this study, a novel and facile hot injection method for the synthesis of single phase CuSbSe2 crystallites was developed by using low toxic triethylene glycol (TEG) as both the solvent and reducing agent and triethylenetetramine (TETA) as co-reducing agent. The effects of the amounts of TETA addition and reaction temperatures on the phase development were investigated. The crystalline structures, morphologies, chemical compositions and optical characterization of the synthesized products were investigated using XRD, TEM, EDS, XPS, and UV-Vis-NIR. A single phase CuSbSe2 crystallites can be obtained by using triethylene glycol as the solvent and reducing agent and triethylenetetramine as co-reducing agent. TETA addition plays a key role in determining the final phase. The presence of the intermediate phase, Cu3SbSe4 phase could be due to the existence of Cu2+, resulting from the insufficient reducibility in the solution. A sufficient amount of TETA can facilitate the reduction of Cu2+ into Cu+, leading to the preformed Cu3SbSe4 phase dissolved and reacted with Sb2Se3 to form CuSbSe2. The obtained CuSbSe2 phase had a direct band gap with the band gap value of 1.06 eV.
- Hsiang, Hsing-I.,Yang, Chang-Ting,Tu, Jui-Huan
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- In situ TEM observation of synergistic electronic-excitation-effects of phase stability in III-V binary compound nanoparticles
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Electronic-excitation-effects of phase stability in III-V binary compound nanoparticles have been studied by TEM. When GaSb particles were excited by 75 keV electrons, the compound transforms to a two-phase consisting of an antimony core and a gallium shell or an amorphous phase, or remains the original crystalline phase, depending on particle size and/or temperature. It is suggested that such nonlinear responses of the phase stability may arise from synergistic effects of bond instability under excited states, formation of high density of excited states, chemical equilibrium under excited states and temperature dependence of defects mobility. EDP Sciences/Societa? Italiana di Fisica/Springer-Verlag 2007.
- Yasuda,Tanaka,Usui,Mori,Lee
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- Solvothermal Synthesis and Crystal Structures of Two Thioantimonate(V) Compounds with the [SbS4]3- Anion Acting as a Monodentate Ligand: See abstract
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The two novel thioantimonate(V) compounds [Mn(C6H 18N4)(C6H19N4)]SbS 4 (I) and [Mn(C6H14N2) 3]2-[Mn(C6H14N2) 2(SbS4)2]·6H2O (II) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in the stoichiometric ratio in 5 ml tris(2-aminoethyl)amine (tren) at 140°C or chxn (trans-1,2-diaminocyclohexane, aqueous solution 50%) at 130°C. Compound I crystallises in the triclinic space group P1, a = 9.578(2), b = 11.541(2), c = 12.297(2) A, α = 62.55(1), β = 85.75(1), γ = 89.44(1)°, V = 1202.6(4) A3, Z = 2, and II in the monoclinic space group C2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1) A, β = 117.237(5)°, V = 7931.7(8) A3, Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS 4]3- anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn2+ ion is coordinated by two chxn ligands and two monodentate [SbS4] 3- units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods.
- Schaefer, Michael,Engelke, Lars,Bensch, Wolfgang
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- Large-scale growth of hollow Sb microspheres
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Uniform hollow antimony micron spheres were synthesized on a large scale using SbCl3 and dithizone as starting reagents in ethylenediamine at 140°C for 72 h. XRD and Raman results reveal that the as-obtained final product is pure Sb. FE-SEM and TEM observation reveals that the prepared hollow microspheres are composed of nanoparticles. The possible formation mechanism was briefly discussed.
- Zhang, Wanqun,Xu, Liqiang,Xi, Guangchen,Yu, Weichao,Qian, Yitai
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- Thermal properties and ion mobility in the antimony(III) fluoride complexes with DL–valine (C5H12NO2)SbF4·H2O and DL–serine (C3H8NO3)Sb2F7. Crystal structure of (C5H12NO2)SbF4·H2O compound
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Fluoride complexes of antimony(III) with amino acids (DL–valine and DL–serine) of the compositions (C5H12NO2)SbF4·H2O (I) and (C3H8NO3)Sb2F7 (II) have been synthesized. The crystal structure of the (C5H12NO2)SbF4·H2O compound (monoclinic syngony, Z = 4, space group P21/c) has been determined for the first time. The structure of I is composed of cations of DL-valinium ((C5H12NO2)+), complex [SbF4]nn– anions having a polymeric chain structure, and crystallization water molecules. Thermal properties and ionic mobility in fluoroantimonates I and II were studied by the DSC and NMR (1H, 19F) methods. It has been established that irreversible endo-effects on DSC curves at 351 and 385 K for the compounds I and II, respectively, are related to formation of X-ray-amorphous phases. In the complex I, ionic mobilities in fluoride and proton sublattices with frequencies above 104 Hz are absent in the studied temperature range (150–420 K), whereas the ions diffusion is observed in both sublattices of II at 320 K. The mechanisms of emergence of ions diffusion in sublattices of the compound II were suggested.
- Kavun, V.Ya.,Udovenko,Slobodyuk,Makarenko,Kovaleva,Zemnukhova
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- Shrinking nanowires by kinetically controlled electrooxidation
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Nanowires composed of antimony, gold, and bismuth telluride (Bi 2Te3) were reduced in diameter by electrooxidation in aqueous solutions. When electrooxidation was carried out using low current densities (Jox -2), the mean wire diameter decreased in direct proportion to the oxidation time, as expected for a kinetically controlled process. Under these conditions, the diameter uniformity of nanowires remained constant as wires were shrunk from initial diameters of more than 120 nm to less than 40 nm, for Sb and Bi 2Te3, and less than 60 nm for Au. Oxidized nanowires remained continuous for more than 100 μm. Electrooxidation at higher current densities rapidly introduced breaks into these nanowires. Electrochemical wire growth and shrinking by electrooxidation were integrated into a single electrochemical experiment that allowed the final mean diameter of nanowires to be specified with a precision of 5-10 nm.
- Thompson,Menke,Martens,Penner
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- Synthesis of the new metastable skutterudite compound NiSb3 from modulated elemental reactants
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A new metastable binary compound with the skutterudite crystal structure has been synthesized from modulated elemental reactants, through an amorphous intermediate, using a novel low-temperature synthesis technique. The amorphous reaction intermediate undergoes nucleation at 87 °C, an extremely low temperature for solid-state reactions. When heated above 350 °C, the metastable phase NiSb3 disproportionates into the thermodynamically stable phases NiSb2 and Sb. Also, if the sum of the individual elemental layer thicknesses is greater than 30 A, a mixture of different phases forms. Simulation of the high-angle powder X-ray diffraction spectrum confirms that NiSb3 is isostructural with CoSb3.
- Williams, Joshua R.,Johnson, David C.
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- A triphosphete and a spirocyclic cation with a PP4 skeleton and a 10e spiro P atom
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The first triposphete 1a and its arsenic analog 1b are the products of the reactions of PCl3 and AsCl3, respectively, with Li[C(PPh2)2- (SiMe3)]. The side product Ph2(Cl)P=C(PPh2)(SiMe3) 2 reacts further with 1a and NaBPh4 by chloride abstraction to yield the spirocyclic ten-electron cation 3 with a pseudo-trigonal-bipyramidal PP4 skeleton.
- Karsch,Witt,Hahn
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- Solvothermal Syntheses, Crystal Structures, and Thermal Properties of New Manganese Thioantimonates(III): The First Example of the Thermal Transformation of an Amine-Rich Thioantimonate into an Amine-Poorer Thioantimonate
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Two new neutral thioantimonates(III) were first prepared by the reaction of elemental manganese, antimony, and sulfur in tren (tren = tris(2-aminoethyl)amine, C6H18N4) at 140 °C. In the amine-rich compound [Mn(tren)]2Sb2S 5 (1) the trigonal SbS3 pyramids are connected via common corners (S(3)) into the tetradentate [Sb2S5]4- anion. Four S atoms have bonds to the manganese atoms of the [Mn(tren)2+] cations. A special structural feature is the large Sb-S(3)-Sb(a) angle of 134°. Density functional calculations clearly demonstrate that this large angle results from the steric interactions between the two Mn(tren) subunits. In the crystal structure of the amine-poorer compound [Mn(tren)] 2Mn2Sb4S10 (2), MnS4 tetrahedra and SbS3 pyramids are linked via common corners and edges to form a new heterometallic [Mn2Sb4S10] core. The [Mn(C6H18N4)2+] cations are located at the periphery of the core and are bound to the [Mn2Sb 4S10] unit via two S atoms. The thermal behavior of both compounds was investigated using simultaneous thermogravimetry (TG), differential thermoanalysis, and mass spectroscopy. The amine-richer compound 1 decomposes in three steps upon heating. After the first TG step an intermediate phase is formed, which was identified as the amine-poorer compound 2 by X-ray diffraction. Reaction of compound 2 at 140 °C with an excess of tren forms the amine-rich compound 1.
- Schaefer, Michael,Naether, Christian,Lehnert, Nicolai,Bensch, Wolfgang
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- Preparation of nanocrystalline antimony powders by using γ-ray radiation method
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Pure nanocrystalline antimony powders have been prepared by using γ-ray radiation method in ambient pressure and room temperature. Transmission electron micrographs and X-ray powder diffraction patterns show that the smallest average particle size is 8 nm and the particle size distribution of this sample is from 5 to 25 nm.
- Liu,Qian,Wang,Zhang,Zhang
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- Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films
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Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III) (1), a precursor for Sb2S3 thin films synthesized from an acidified aqueous solution of SbCl3 and KS2COCH2CH3, was monitored by simultaneous thermogravimetry, differential thermal analysis and evolved gas analysis via mass spectroscopy (TG/DTA-EGA-MS) measurements in dynamic Ar, and synthetic air atmospheres. 1 was identified by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) measurements, and quantified by NMR and elemental analysis. Solid intermediates and final decomposition products of 1 prepared in both atmospheres were determined by X-ray diffraction (XRD), Raman spectroscopy, and FTIR. 1 is a complex compound, where Sb is coordinated by three ethyldithiocarbonate ligands via the S atoms. The thermal degradation of 1 in Ar consists of three mass loss steps, and four mass loss steps in synthetic air. The total mass losses are 100% at 800?°C in Ar, and 66.8% at 600?°C in synthetic air, where the final product is Sb2O4. 1 melts at 85?°C, and decomposes at 90–170?°C into mainly Sb2S3, as confirmed by Raman, and an impurity phase consisting mostly of CSO22? ligands. The solid-phase mineralizes fully at ≈240?°C, which permits Sb2S3 to crystallize at around 250?°C in both atmospheres. The gaseous species evolved include CS2, C2H5OH, CO, CO2, COS, H2O, SO2, and minor quantities of C2H5SH, (C2H5)2S, (C2H5)2O, and (S2COCH2CH3)2. The thermal decomposition mechanism of 1 is described with chemical reactions based on EGA-MS and solid intermediate decomposition product analysis.
- Adamson, Jasper,Eensalu, Jako S.,Krunks, Malle,Oja Acik, Ilona,T?nsuaadu, Kaia
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- Comprehensive Study on Reactions of Group 13 Diyls with Tetraorganodipentelanes
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L1Ga {L1 = HC[C(Me)N(2,6-iPr2C6H3)]2} reversibly reacts with E2Ph4 (E = Sb, Bi) in a temperature-dependent equilibrium reaction with insertion into the E-E bond and formation of L1Ga(EPh2)2 (E = Sb 1, Bi 2). Analogous findings were observed in the reactions of L2Ga {L2 = (C6H11)2NC[N(2,6-iPr2C6H3)]2} with E2R4 (R = Ph, Et), yielding L2Ga(EPh2)2 (E = Sb 3, Bi 4) and L2Ga(EEt2)2 (E = Sb 5, Bi 6). 1-3 and 5 were isolated by fractional crystallization at low temperature, whereas 4 and 6 could not be isolated in their pure form even at low temperature. In contrast, reactions of [Cp?Al]4 (Cp? = C5Me5) with Sb2R4 (R = Ph, Et) and Bi2Et4 did not proceed with insertion into the E-E bonds but with formation of (Cp?Al)3E2 (E = Sb, 7; Bi, 8), whereas the reaction with Bi2Ph4 yielded metallic bismuth. 8 was also formed in the reaction of [Cp?Al]4 and BiEt3 at ambient temperature, whereas the analogous reaction of [Cp?Al]4 with SbEt3 did not yield 7 even under drastic reaction conditions (120 °C, 3 days). In contrast, Cp?Ga and Sb2R4 (R = Ph, Et) were found to react only at elevated temperature (120 °C) with formation of antimony metal.
- Ganesamoorthy, Chelladurai,Krüger, Julia,Gl?ckler, Eduard,Helling, Christoph,John, Lukas,Frank, Walter,W?lper, Christoph,Schulz, Stephan
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p. 9495 - 9503
(2018/08/17)
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- Highly reversible Na-ion reaction in nanostructured Sb2Te3-C composites as Na-ion battery anodes
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Sb2Te3 and its amorphous carbon-modified nanocomposite (Sb2Te3-C) are synthesized by simple solid-state synthetic methods, and their potential as anode materials for rechargeable Na-ion batteries (NIBs) is evaluated. Ex situ X-ray diffraction and high-resolution transmission electron microscopy clearly demonstrate the sodiation/desodiation reaction mechanism of the Sb2Te3 and Sb2Te3-C nanocomposite electrodes. In both electrodes, Sb2Te3 is converted into Na3Sb and Na2Te during Na insertion. However, Na3Sb and Na2Te in only the Sb2Te3-C nanocomposite electrode recombine into the original Sb2Te3 phase after full Na extraction. As a consequence of its interesting conversion/recombination reaction during sodiation/desodiation reaction, the Sb2Te3-C nanocomposite electrode exhibits a long cycle life with highly reversible gravimetric and volumetric capacity (373 mAh g-1 and 765 mAh cm-3 over 50 cycles) and fast rate capability (1 C: 391 mAh g-1 and 802 mAh cm-3; 2 C: 377 mAh g-1 and 773 mAh cm-3).
- Nam, Ki-Hun,Choi, Jeong-Hee,Park, Cheol-Min
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p. A2056 - A2064
(2018/02/28)
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- Solvothermal synthesis of wire-like SnxSb2Te3+x with an enhanced thermoelectric performance
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Nanostructured tellurides have attracted increasing attention in thermoelectric applications for waste heat recovery and cooling devices. Here, we report on the synthesis of wire-like SnxSb2Te3+x (x = 0, 0.02 and 0.05) nanoparticles using elemental precursors in EG. The enhanced thermoelectric performance was achieved in alloyed samples due to the increase of carrier population in heavy valence band valleys by incorporating Sn2+ at the Sb3+ sublattice, enabling the simultaneous realization of low electrical resistivity along with a high Seebeck coefficient as well as the decline of thermal conductivity. Thus a boosted power factor and low thermal conductivity lead to the highest ZT value of 0.58 at 150 °C in the Sn0.02Sb2Te3.02 sample. Our research offers a general wet-chemical route for the preparation of one-dimensional nanomaterials and probably promotes the practical thermoelectric applications of Sb2Te3-based materials at low temperatures.
- Yang, Heng Quan,Miao, Lei,Liu, Cheng Yan,Wang, Xiao Yang,Peng, Ying,Zhang, Ai Juan,Zhou, Xiao Yuan,Wang, Guo Yu,Li, Chao,Huang, Rong
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supporting information
p. 7483 - 7491
(2016/06/01)
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- Salt-Free Reduction of Nonprecious Transition-Metal Compounds: Generation of Amorphous Ni Nanoparticles for Catalytic C-C Bond Formation
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A salt-free procedure for the generation of a wide variety of metal(0) particles, including Fe, Co, Ni, and Cu, was achieved using 2,3,5,6-tetramethyl-1,4-bis(trimethylsilyl)-1,4-diaza-2,5-cyclohexadiene (1), which reduced the corresponding metal precursors under mild conditions. Notably, Ni particles formed in situ from the treatment of Ni(acac)2 (acac=acetylacetonate) with 1 in toluene exhibited significant catalytic activity for reductive C-C bond-forming reactions of aryl halides in the presence of excess amounts of 1. By examination of high-magnification transmission electron microscopy images and electron diffraction patterns, we concluded that amorphous Ni nanoparticles (Ni aNPs) were essential for the high catalytic activity.
- Yurino, Taiga,Ueda, Yohei,Shimizu, Yoshiki,Tanaka, Shinji,Nishiyama, Haruka,Tsurugi, Hayato,Sato, Kazuhiko,Mashima, Kazushi
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supporting information
p. 14437 - 14441
(2016/01/25)
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- Properties of fluoroantimonates(III) complexes with amino acids
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Crystalline complex fluoroantimonates(III) with amino acids (glycine, β-alanine, DL-serine, DL-valine, L-leucine, and L-phenylalanine) have been prepared. The complexes stability in aqueous solutions has been studied with the cementation method. 1/s
- Zemnukhova,Babushkina,Klimova,Makarenko,Kovaleva
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p. 918 - 922
(2014/07/22)
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- Antimonato polyoxovanadates with structure directing transition metal complexes: Pseudopolymorphic{Ni(dien)2}3[V 15Sb6O42(H2O)]·nH 2O compounds and {Ni(dien)2}4[V 16Sb4O42(H2O)]
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Three new poloxovanadates were synthesized under solvothermal conditions and were structurally characterized. The two compounds with composition {Ni(dien)2}3[V15Sb6O 42(H2O)]·nH2O (n = 12 and 8; dien = bis(2-aminoethyl)amine or diethylenetriamine) are pseudopolymorphs crystallizing in different space groups. The compounds were obtained by applying identical reaction slurries but using different reaction temperatures. Both compounds feature the [V15Sb6O42(H2O)] 6- anion which is the antimony analogue to the single molecule magnet [V15As6O42(H2O)]6-. Crystal data: 1 tetragonal space group P4, a = 46.9378(3), c = 16.51300(10) A and V = 36380.7(4) A3. 2 rhombohedral space group R3c with a = 23.0517(4), c = 28.6216(5) A and V = 13171.3(4) A3. In 1 several unusual short inter-cluster Sb...O contacts lead to the formation of three different super-clusters with composition V60Sb24O168. The 12 unique {Ni(dien)2}2+ complexes adopt all three possible configurations. In 2 the special arrangement of the {Ni(dien)2} 2+ complexes around the cluster anion prevents inter-cluster Sb...O contacts. The main structural motif of the third compound {Ni(dien)2}4[V16Sb4O 42(H2O)] (3) is the [V16Sb4O 42(H2O)]8- cluster anion consisting of two perpendicular eight-membered rings of VO5 pyramids. Two additional VO5 polyhedra are located on opposite sides. Crystal data: 3 triclinic space group P1, a = 13.5159(4), b = 14.2497(5), c = 14.9419(4) A, α = 98.322(2), β = 114.080(2), γ = 110.130(2)°and V = 2326.35(12) A3.
- Antonova, Elena,Naether, Christian,Bensch, Wolfgang
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p. 1338 - 1344
(2012/03/07)
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- Solution synthesis of nanoparticular binary transition metal antimonides
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The preparation of nanoengineered materials with controlled nanostructures, for example, with an anisotropic phase segregated structure or a regular periodicity rather than with a broad range of interparticle distances, has remained a synthetic challenge for intermetallics. Artificially structured materials, including multilayers, amorphous alloys, quasicrystals, metastable crystalline alloys, or granular metals, are mostly prepared using physical gas phase procedures. We report a novel, powerful solution-mediated approach for the formation of nanoparticular binary antimonides based on presynthesized antimony nanoparticles. The transition metal antimonides M-Sb (M = Co, Ni, Cu 2, Zn) were obtained with sizes ranging from 20 and 60 nm. Through careful control of the reaction conditions, single-phase nanoparticular antimonides were synthesized. The nanophases were investigated by powder X-ray diffraction and (high resolution) electron microscopy. The approach is based on activated metal nanoparticles as precursors for the synthesis of the intermetallic compounds. X-ray powder diffraction studies of reaction intermediates allowed monitoring of the reaction kinetics. The small particle size of the reactants ensures short diffusion paths, low activation barriers, and low reaction temperatures, thereby eliminating solid-solid diffusion as the rate-limiting step in conventional bulk-scale solid-state synthesis.
- Kieslich, Gregor,Birkel, Christina S.,Stewart, Andrew,Kolb, Ute,Tremel, Wolfgang
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p. 6938 - 6943
(2011/10/10)
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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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- Thermoelectric properties of A0.05Mo3Sb 5.4Te1.6 (A = Mn, Fe, Co, Ni)
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Mo3Sb7-xTex was earlier reported to be a promising p-type thermoelectric material for high temperature applications, with Ni0.06Mo3Sb5.4Te1.6 achieving a ZT of 0.93 at 1023 K. In order to investigate the effect of using different transition metal atoms and to further improve the thermoelectric properties, a variety of transition metal atoms (Mn, Fe, Co and Ni) were intercalated into the voids of empty Sb atom cubes. Our results indicate that Fe 0.05Mo3Sb5.4Te1.6 and Ni 0.05Mo3Sb5.4Te1.6 exhibit a higher power factor than Mo3Sb5.4Te1.6. Fe 0.05Mo3Sb5.4Te1.6 demonstrates the highest ZT value at 673 K (ZT = 0.31), significantly higher than Mo 3Sb5.4Te1.6. Thermal analysis proves Ni 0.05Mo3Sb5.4Te1.6 to be phase stable at least until 1250 K in an inert atmosphere, an important prerequisite for high temperature applications.
- Xu, Hong,Kleinke, Katja M.,Holgate, Tim,Rossouw, David,Botton, Gianluigi,Tritt, Terry M.,Kleinke
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p. 314 - 319
(2011/01/11)
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- Synthesis, crystal structure, and spectral analysis of antimony thiourea tetra chloride
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The synthesis of antimony thiourea tetra chloride (ATTC) single crystals by solution technique at room temperature is reported. The complex crystallizes in the orthorhombic space group Pnma with four formula units ofSb[CS(NH 2)2]2Cl3·Cl in the unit cell. The structure has been solved by direct methods and refined to a final-R value of 0.0393. The synthesized crystals are characterized by FT-IR, UV-visible and TGA-DTA techniques. Copyright Taylor & Francis Group, LLC.
- Upadhya, K. Mahesha,Udayashankar
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p. 812 - 820
(2011/02/23)
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- Kinetics of mechanochemical synthesis of Me/FeS (Me = Cu, Pb, Sb) nanoparticles
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The mechanochemical synthesis of Cu/FeS, Pb/FeS and Sb/FeS nanoparticles was investigated with the regard to solid-state kinetics. Experiments were performed in a planetary mill and in an eccentric vibratory mill by a high-energy milling of Cu2
- Balá?,Dutková,?korvánek,Gock,Kovac,Satka
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p. 484 - 487
(2010/03/01)
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- Reduction of PbS and Sb2S3 with elemental Fe and Mg in dusty plasma environment created during electrical discharge assisted mechanical milling (EDAMM)
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The newly developed synthesis technique of electrical discharge assisted mechanical milling (EDAMM) is used to reduce Pb and Sb sulfides using Fe and Mg as reduction agents. It is demonstrated that both Fe and Mg can successfully be used to fully reduce P
- Calka,Mosbah,Stanford,Balaz
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p. 477 - 484
(2009/04/13)
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- Thermodynamic properties of tetraphenylantimony benzophenoxymate in the region of 0-450 K
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Heat capacity of tetraphenylantimony benzophenoxymate Ph 4SbONCPh2 is measured for first time using adiabatic calorimeter in the range from 6K to 350K and differential scanning calorimeter in the range from 330 K to 450 K. In the ran
- Smirnova,Letyanina,Markin,Larina,Sharutin,Molokova
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p. 717 - 723
(2009/09/26)
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- Electrodeposition of SbTe phase-change alloys
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Electrodeposition of SbTe thin films was investigated at room temperature, where amorphous deposits were obtained. The electrodeposition of Sb was found to be induced by Te, while the latter was not affected by the Sb. Detailed studies on this induced deposition were carried out by varying the Sb(III) and Te(IV) concentrations, pH, and agitation. The Sb deposition rate was found to be independent of the concentrations of both species but dependent on the pH and agitation. A phase transition from amorphous films into crystalline Sb2 Te3 at 120°C was observed for the plated SbTe.
- Huang,Kellock,Raoux
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p. D104-D109
(2008/10/09)
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- Electrodeposition of Sb, Bi, Te, and their alloys in AlCl3-NaCl-KCl molten salt
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The Electrochemistry of Sb, Bi, and Te in AlCl3-NaCl-KCl molten salt containing SbCl3, BiCl3, and/or TeCl4 at 423 K was investigated by voltammetry, and electrodeposition of the three metals was performed under constant potential control in the melt. The voltammogram on a glassy carbon (GC) electrode in a melt containing 0.025 mol dm-3 [M] SbCl3 showed a couple of redox peak corresponding to the Sb/Sb(III) redox reaction, and a stable layer of pure Sb was deposited under the constant potential control. The voltammograms in the melt containing 0.025 M BiCl3 or 0.025 M TeCl4 showed several redox couples. Stable deposit layers of pure Bi and Te were not obtained under the constant potential control, as the deposited layers detached from the electrode and immediately dissolved into the molten salt. Binary alloy deposition was possible in a melt containing BiCl3 and SbCl3, and also with BiCl3 and TeCl4. A stable Bi-Sb alloy deposit of metallic Sb and Bi-Sb solid solution was obtained at 0.8 and 0.9 V versus Al/Al(III) in the melt containing BiCl3 and SbCl3. The atomic ratio of Bi in the deposit was 37% at 0.9 V and 57% at 0.8 V. A stable Bi-Te alloy deposit was also obtained with the molten salt containing BiCl3 and TeCl4. The deposited Bi-Te alloy consisted of a mixture of Bi2Te3, BiTe, and Bi2Te. The alloy deposit had good crystallinity and the preferential orientation was the (1 1 0) plane.
- Ebe, Hirofumi,Ueda, Mikito,Ohtsuka, Toshiaki
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p. 100 - 105
(2008/10/09)
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- Diamidonaphthalene-stabilized N-heterocyclic pnictogenium cations and their cation-cation solid-state interactions
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The synthesis and comprehensive characterization of a new series of N-heterocyclic phosphine, arsine, and stibine compounds is presented. The diamidochloropnictines ClPn(NR)2C10H6 (Pn = P, As, Sb) were prepared via the dehydrohalide coupling reactions of N,N′-diisopropyl-1,8-diaminonaphthalene, (iPrNH) 2C10H6, or N,N′-diphenyl-1,8- diaminonaphthalene, (PhNH)2C10H6, with the appropriate pnictogen trichloride. Reaction of these pnictines with appropriate halide abstraction agents yielded the corresponding phosphenium and arsenium salts. These planar pnictogenium cations {Pn(NR)2C10H 6}+ (Pn = P, As; R = iPr, Ph) display dicoordinate pnictogen centers that are stabilized by an electron-rich diamidonaphthalene framework and represent rare examples of six-membered N-heterocyclic pnictogenium cations possessing a π-conjugated carbon backbone. The related stibenium salts could not be prepared via this route; however, the reaction of the new heteroleptic triamidostibene, (Me 2N)Sb(iPrN)2C10H6, with triflic acid does generate the base-stabilized stibenium cation, [Sb( iPrN)2C10H6·(Me 2NH)]+. The phosphenium and arsenium salts exhibit different modes of packing in their solid-state structures depending upon the identity of the nitrogen substituents. The two phenyl substituted compounds display an interaction between the pnictogen center and the π-system of an adjacent naphthyl moiety. In contrast, the isopropyl substituted species undergo metastable dimerization through naphthyl π-stacking. These dimers are bound by strong dipole-dipole and dispersion interactions as revealed through computational studies.
- Spinney, Heather A.,Korobkov, Ilia,DiLabio, Gino A.,Yap, Glen P. A.,Richeson, Darrin S.
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p. 4972 - 4982
(2008/10/09)
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- Thermoelectric properties and microstructure of Mg3Sb2
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Mg3Sb2 has been prepared by direct reaction of the elements. Powder X-ray diffraction, thermal gravimetric, differential scanning calorimetery, and microprobe data were obtained on hot pressed samples. Single phase samples of Mg
- Condron, Cathie L.,Kauzlarich, Susan M.,Gascoin, Franck,Snyder, G. Jeffrey
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p. 2252 - 2257
(2008/10/09)
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- Zinc reaction with diphenylantimony and diphenylbismuth chlorides in aprotic solvents
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Products of zinc oxidation with diphenylantimony and diphenylbismuth chlorides in aprotic solvents are established. The effective adsorption constants of the reagents on the metal surface and the rate constants and activation energies of the processes und
- Losev,Klement'eva,Maslennikov,Spirina
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p. 1581 - 1583
(2008/02/07)
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- Oxidation of magnesium with diphenylbismuth and diphenylantimony chlorides in polar solvents
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The intermediate and final products of the reactions of magnesium with diphenylantimony and diphenylbismuth chlorides were identified, and the formal kinetic relationships of the process were elucidated. The apparent equilibrium constants, enthalpies, and
- Maslennikov,Klement'eva,Losev, Ya. V.,Spirina,Maslennikov
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- Synthesis, characterization and thermal decomposition of thiourea complexes of antimony and bismuth triiodide
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The thiourea complexes of antimony and bismuth triiodide were synthesized by a direct reaction of antimony and bismuth triiodide with thiourea powder at room temperature. The formula of the complex is MI3[SC(NH 2)2]3(M=Sb, Bi). The crystal structure of the complexes belongs to monoclinic system and the lattice parameters are a=1.4772 nm, b=1.6582 nm, c=2.0674 nm and β=90.81° for SbI 3(SC(NH2)2)3 and a=1.4009 nm, b=2.0170 nm, c=2.0397 nm and β=90.84° for BiI3[SC(NH 2)2]3. The infrared spectra reveal that the trivalent antimony or bismuth ion is coordinated by the nitrogen atom, not the sulfur atom of the thiourea. Thermal analysis shows that there are two times structure rearrangements or phase transformation in the complexes from 100 to 170°C. Springer-Verlag 2006.
- Zhong,Luan,Wang,Guo,Chen,Jia
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p. 775 - 781
(2008/10/09)
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- Interaction of oxides with supercritical isopropanol
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The interaction of Group I-VIII oxides with isopropanol (i-C 3H7OH; i-PrOH) in the supercritical fluid (SCF) region has been studied. Simple oxides can be divided into three groups: (a) oxides that are completely reduced to a metal (CuO, CdO, PbO, TeO2, Sb 2O3, Bi2O3, Co2O 3, ReO3, PtO2), (b) polyvalent metal oxides reducible to intermediate (lower) oxidation states (V2O5, Fe 2O3, MnO2, Mn2O3, MoO3) and (c) ones irreducible by SCF-/-PrOH (UO2, Ga 2O3, SnO2, ZnO, In2O3, Nd2O3, Cr2O3, WO3, ZrO2, NiO, CeO2, SiO2, GeO2). It has been found that in the cases of MnO2 and Nd2O3 the oxides can be hydrogenated to yield hydroxides. For the reactions of C 3H7OH with bismuth and manganese oxides, it has been shown that the process is heterogeneous during its entire duration.
- Kargin,Buslaeva,Kravchuk,Gubin
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p. 103 - 106
(2008/10/08)
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