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7440-36-0Relevant articles and documents
A facile route to fabricate single-crystalline antimony nanotube arrays
Li, Liang,Xiao, Yanhe,Yang, Youwen,Huang, Xiaohu,Li, Guanghai,Zhang, Lide
, p. 930 - 931 (2005)
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
Thermal behavior of antimony nanowire arrays embedded in anodic aluminum oxide template
Zhang,Ding,Zhang,Hao,Meng,Zhang
, p. 493 - 497 (2007)
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.
Solution synthesis of a new thermoelectric Zn1+ xSb nanophase and its structure determination using automated electron diffraction tomography
Birkel, Christina S.,Mugnaioli, Enrico,Gorelik, Tatiana,Kolb, Ute,Panthoefer, Martin,Tremel, Wolfgang
, p. 9881 - 9889 (2010)
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.
Cohn, G.,Goodeve, C. F.
, p. 433 (1940)
Antimony film electrode for direct cathodic measurement of sulfasalazine
Nigovi?, Biljana,Hocevar, Samo B.
, p. 523 - 527 (2011)
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.
Chalcogenolato Complexes of Bithmuth and Antimony. Syntheses, Termolysis Reactions, and Crystal Structure of Sb(SC6H2(i-Pr)3-2,4,6)3
Bochmann, Manfred,Song, Xuejing,Hursthouse, Michael B.,Karaulov, Alexander
, p. 1649 - 1652 (1995)
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.
Phase stability and thermoelectric properties of Cu10.5Zn1.5Sb4S13 tetrahedrite
Harish, Subramaniam,Sivaprahasam, Duraisamy,Battabyal, Manjusha,Gopalan, Raghavan
, p. 323 - 328 (2016)
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.
Thermoelectric properties of the Ru2Ni2Sb 12 ternary skutterudite
Navratil, Jiri,Laufek, Frantisek,Plechacek, Tomas,Drasar, Cestmir
, p. 2 - 7 (2012)
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.
Synthesis and Structural Evolution of RuSb3, a New Metastable Skutterudite Compound
Smalley, Arwyn L. E.,Jespersen, Michael L.,Johnson, David C.
, p. 2486 - 2490 (2004)
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.
Nanoscale electrocrystallisation of Sb and the compound semiconductor AlSb from an ionic liquid
Aravinda,Freyland
, p. 1703 - 1705 (2006)
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
Hovorka, F.,Chapman, G. H.
, p. 955 - 2024 (1941)
Thermally stable thermoelectric Zn4 Sb3 by zone-melting synthesis
Pedersen,Iversen
, (2008)
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.
A rational complexing-reduction route to antimony nanotubes
Hu, Hanmei,Mo, Maosong,Yang, Baojun,Shao, Mingwang,Zhang, Shuyuan,Li, Qiaowei,Qian, Yitai
, p. 1161 - 1163 (2003)
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).
Cohn, G.,Hedvall, J. A.
, p. 603 - 607 (1943)
Soft-Chemical Method for Synthesizing Intermetallic Antimonide Nanocrystals from Ternary Chalcogenide
Jiang, Yilan,Yuan, Long,Xu, Yanyan,Ma, Jiaojiao,Sun, Yu,Gao, Xia,Huang, Keke,Feng, Shouhua
, p. 15131 - 15136 (2019)
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.
Thermal reduction of mechanically activated cinnabar (HgS) and stibnite (Sb2S3)
Balaz,Godocikova
, p. 51 - 57 (2001)
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.
Mechanism of formation and electronic structure of semiconducting ZnSb nanoclusters electrodeposited from an ionic liquid
Mann, Olivier,Freyland, Werner
, p. 518 - 524 (2007)
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.
Konopik, N.,Werner, E.
, (1950)
Characterization of CuSbSe2 crystallites synthesized using a hot injection method
Hsiang, Hsing-I.,Yang, Chang-Ting,Tu, Jui-Huan
, p. 99297 - 99305 (2016)
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.
In situ TEM observation of synergistic electronic-excitation-effects of phase stability in III-V binary compound nanoparticles
Yasuda,Tanaka,Usui,Mori,Lee
, p. 177 - 180 (2007)
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.
Large-scale growth of hollow Sb microspheres
Zhang, Wanqun,Xu, Liqiang,Xi, Guangchen,Yu, Weichao,Qian, Yitai
, p. 1476 - 1477 (2004)
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.
Shrinking nanowires by kinetically controlled electrooxidation
Thompson,Menke,Martens,Penner
, p. 36 - 41 (2006)
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.
Langstroth, G. O.,McRae, D. R.
, p. 282 - 282 (1938)
Price, S. J. W.,Trotman-Dickenson, A. F.
, p. 1630 - 1637 (1958)
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
Schaefer, Michael,Naether, Christian,Lehnert, Nicolai,Bensch, Wolfgang
, p. 2914 - 2921 (2004)
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.
Thermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III)—a single-source precursor for antimony sulfide thin films
Adamson, Jasper,Eensalu, Jako S.,Krunks, Malle,Oja Acik, Ilona,T?nsuaadu, Kaia
, (2021/06/25)
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.
