1313-82-2Relevant articles and documents
Complex Hydroxides of Chromium: Na9[Cr(OH)6]2(OH)3 ? 6 H2O and Na4[Cr(OH)6]X ? H2O (X = Cl, (S2)1/2) - Synthesis, Crystal Structure, and Thermal Behaviour
Hinz, Dirk
, p. 1004 - 1011 (2000)
Green plate-like crystals of Na9[Cr(OH)6]2(OH)3 · 6H2O (triclinic, P1?, a = 872.9(1) pm, b = 1142.0(1) pm, c = 1166.0(1) pm, α = 74.27(1)°, β = 87.54(1)°, γ = 70.69(1)°) are obtained upon slow cooling of a hot saturated solution of CrIII in cone. NaOH (50 wt%) at room temperature. In the presence of chloride or disulfide the reaction yields green prismatic crystals of Na4[Cr(OH)6]Cl · H2O (monoclinic, C2/c, a = 1138.8(2) pm, b = 1360.4(1) pm, c = 583.20(7) pm, β = 105.9(1)°) or green elongated plates of Na4[Cr(OH)6](S2)1/2 · H2O (monoclinic, P21/c, a = 580.8(1) pm, b = 1366.5(3) pm, c = 1115.0(2) pm, β = 103.71(2)°), respeclively. The latter compounds crystallize in related structures. All compounds can be described as distorted cubic closest packings of the anions and the crystal water molecules with the cations occupying octahedral sites in an ordered way. The thermal decomposition of the compounds was investigated by DSC/TG or DTA/TG and high temperature X-ray powder diffraction measurements. In all cases the final decomposition product is NaCrO2.
Caldwell, W. E.,Krauskopf, F. C.
, p. 2936 - 2942 (1929)
Na3+xMxP1?xS4 (M = Ge4+, Ti4+, Sn4+) enables high rate all-solid-state Na-ion batteries Na2+2δFe2?δ(SO4)3|Na3+xMxP1?xS4|Na2Ti3O7
Rao, Rayavarapu Prasada,Chen, Haomin,Wong, Lee Loong,Adams, Stefan
, p. 3377 - 3388 (2017)
Electrolytes in current Na-ion batteries are mostly based on the same fundamental chemistry as those in Li-ion batteries-a mixture of flammable liquid cyclic and linear organic carbonates leading to the same safety concerns especially during fast charging. All-solid-state Na-ion rechargeable batteries utilizing non-flammable ceramic Na superionic conductor electrolytes are a promising alternative. Among the known sodium conducting electrolytes the cubic Na3PS4 phase has relatively high sodium ion conductivity exceeding 10?4 S cm?1 at room temperature. Here we systematically study the doping of Na3PS4 with Ge4+, Ti4+, Sn4+ and optimise the processing of these phases. A maximum ionic conductivity of 2.5 × 10?4 S cm?1 is achieved for Na3.1Sn0.1P0.9S4. Utilising this fast Na+ ion conductor, a new class of all-solid-state Na2+2δFe2?δ(SO4)3|Na3+xMxP1?xS4 (M = Ge4+, Ti4+, Sn4+) (x = 0, 0.1)|Na2Ti3O7 sodium-ion secondary batteries is demonstrated that is based on earth-abundant safe materials and features high rate capability even at room temperature. All-solid-state Na2+2δFe2?δ(SO4)3|Na3+xMxP1?xS4|Na2Ti3O7 cells with the newly prepared electrolyte exhibited charge-discharge cycles at room temperature between 1.5 V and 4.0 V. At low rates the initial capacity matches the theoretical capacity of ca. 113 mA h g?1. At 2C rate the first discharge capacity at room temperature is still 83 mA h per gram of Na2+2δFe2?δ(SO4)3 and at 80 °C it rises to 109 mA h per gram with 80% capacity retention over 100 cycles.
Aromatic hydrocarbon-catalyzed direct reaction of sulfur and sodium in a heterogeneous system: Selective and facile synthesis of sodium monosulfide and disulfide
Takata, Toshikazu,Saeki, Daisaku,Makita, Yoshimasa,Yamada, Nobuo,Kihara, Nobuhiro
, p. 3712 - 3714 (2003)
Sodium disulfide and monosulfide were selectively formed via the direct reaction of sulfur and an equimolar amount of sodium in 1,2-dimethoxyethane at 70 °C in the presence of a catalytic amount of aromatic hydrocarbons and ketone.
Preparation of alkali-metal hypothiophosphates in an alcoholic solution
Svirskaya,Lupeiko,Pakhomov,Medvedeva
, p. 762 - 765 (2011)
A procedure was developed for preparation of lithium and sodium hypothiophosphates from the corresponding alkali-metal and phosphorus sulfides in ethanol. The possibility was explored for preparation of tin(II) hypothiophosphate in an alcoholic solution by an exchange reaction between sodium hypothiophosphate and tin(II) chloride.
DETERMINATION OF GIBBS ENERGY OF THE EXCHANGE REACTION OF SULPHIDES USING BETA-ALUMINA SOLID ELECTROLYTE.
Itoh, Mitsuru,Kozuka, Tetsuya Yamamoto Zensaku
, (1988)
EMF measurements of the cell Na(l)/ beta prime -alumina/Na//2S plus Ag//2S plus Ag were carried out in the temperature range 463. 4 to 843. 7 K. The results are represented by the equation E/V ( plus or minus 0. 00057) equals 1. 75793( plus or minus 0. 00
Solvent-thermal preparation of nanocrystalline tin chalcogenide
Qian,Zhang,Wang,Wang,Xie,Qian
, p. 415 - 417 (1999)
Nanocrystalline β-SnS2 has been successfully prepared by the reaction between SnCl4 and anhydrous Na2S using a solvent-thermal method at 150 °C, which is similar to the well-known hydrothermal process except that toluene is substituted for water. X-ray diffraction analysis indicates that the product is the β-SnS2 phase, and no Sn-O vibrations are found in the IR spectra. Transmission electron microscopy shows that the average particle size is about 12 nm.
Topochemical anion metathesis routes to the Zr2N2S phases and the Na2S and ACL derivatives (A = Na, K, Rb)
Stoltz,Ramesha,Sirchio,Goenen,Eichhorn,Salamanca-Riba,Gopalakrishnan
, p. 4285 - 4292 (2003)
Anion metathesis reactions between ZrNCl and A2S (A = Na, K, Rb) in the solid state follow three different pathways depending on reaction temperature and reactant stoichiometry: (1) the reaction of ZrNCl with A2S in the 2:1 stoichiometry at 800 °C/72 h/in vacuo yields α-Zr2N2S with the expected layered structure of La2O2S. Above 850 °C, α-Zr2N2S (P3m1; a = 3.605(1) A, c = 6.421(3) A) neatly transforms to β-Zr2N2S (P63/mmc: a = 3.602(1) A, c = 12.817(1) A). The structures of the α- and β-forms are related by an a/2 shift of successive Zr2N2 layers. (2) The same reaction at low temperatures (300-400 °C) yields ACl intercalated phases of the formula AxZr2N2SClx (0 a ZrNCl-type structure. The S and Cl ions are disordered and the c lattice parameters are alkali dependent (R3m, a ~ 3.6 A, c ~ 28.4 (Na), 28.9 (K), and 30.5 A (Rb). AxZr2N2SClx phases are hygroscopic and reversibly absorb water to give monohydrates. (3) Reaction of ZrNCl with excess A2S at 400-1000 °C gives A2S intercalated phases of the formula A2xZr2N2S1+x (0 a ZrNCl type structure (R3m, a ~ 3.64 A, c ~ 29.48 A). Structural characterization of the new phases and implications of the results are described.
Selective and Facile Synthesis of Sodium Sulfide and Sodium Disulfide Polymorphs
El-Shinawi, Hany,Cussen, Edmund J.,Corr, Serena A.
, p. 7499 - 7502 (2018)
Na2S and Na2S2 were selectively synthesized using a microwave-assisted thermal treatment of a Na+/S solution in tetraglyme between 100 and 200 °C, considerably lower than that of current routes. This novel synthetic pathway yields the Na2S phase in high purity and allows for good selectivity between the polymorphs of Na2S2 (α and β phases). These materials show promising electrochemical properties and are particularly interesting for the continued development of Na-S batteries.
Flux Synthesis of LiAuS and NaAuS: Chicken-Wire-Like Layer Formation by Interweaving of (AuS)nn- Threads. Comparison with α-HgS and AAuS (A = K, Rb)
Axtell III, Enos A.,Liao, Ju-Hsiou,Kanatzidis, Mercouri G.
, p. 5583 - 5587 (1998)
From the reaction of Au with alkali metal polysulfide liquids, LiAuS and NaAuS were discovered. Orange crystals of LiAuS crystallize in the monoclinic space group C2/c, (no. 15), with a = 8.994(2) ?, b = 8.956(2) ?, c = 7.201(3) ?, β= 128.68(1)°, and Z = 8. Light-yellow planks of NaAuS crystallize in the orthorhombic space group Ccca, (no. 68), with a = 14.658(5) ?, b = 21.043(7) ?, c = 7.118(4) ?, and Z = 32. Both compounds contain infinite one-dimensional (AuS)nn- chains, featuring alternating sulfide anions and linear coordinated Au centers. In LiAuS, the chains are zigzag and fully extended and they pack in two mutually perpendicular sets. In NaAuS, the same chains coil in an unusual fashion so that they become interwoven to form layers reminiscent of chicken-wire . This novel coiling mode allows Au-Au contacts to form, which help to stabilize the structure. The structural relationships between LiAuS, NaAuS, Na7Au5S6, AAuQ (A = K, Rb, Cs; Q = S, Se), and α-HgS are explored.
Kinetics and Mechanism of the Reaction of the Ammoniated Electron with Sodium Thiosulfate in Liquid Ammonia
Lau, Nathanielo,Dewald, Robert R.
, p. 2348 - 2350 (1980)
The reaction of sodium with thiosulfate in liquid ammonia was found to be second order, first order with respect to both the sodium and thiosulfate concentration.The sodium ion concentration was found to have a dominant influence on the net reaction rate, and a mechanism involving ion-paired species is proposed.The stoichiometry and reaction products were also determined.
Synthesis in molten alkali metal polythiophosphate fluxes. The new quaternary bismuth and antimony thiophosphates ABiP2S7 (A = K, Rb), A3M(PS4)2 (A = K, Rb, Cs; M = Sb, Bi), Cs3Bi2(PS4)3, and Na0.16Bi1.28P2S6
McCarthy,Kanatzidis
, p. 70 - 85 (1996)
The molten alkali metal polychalcogenide flux method was used to prepare the new compounds ABiP2S7 (A = K, Rb), A3M(PS4)2 (A = K, Rb, Cs; M = Sb, Bi), Cs3Bi2 (PS4)3, and Na0.16Bi1.28P2S6. The structural diversity in this family of compounds ranges from the one-dimensional non-centrosymmetric chains of A3M(PS4)2 and the layered compounds, ABiP2S7 and Cs3Bi2 (PS4)2, to the dense three-dimensional framework of Na0.16Bi1.28P2S6. Their synthesis, structural characterization, optical absorption and thermal properties are reported.
Na2EuAs2S5, NaEuAsS4, and Na4Eu(AsS4)2: Controlling the valency of arsenic in polysulfide fluxes
Bera, Tarun K.,Kanatzidis, Mercouri G.
, p. 4293 - 4299 (2012)
The reactivity of europium with As species in Lewis basic alkali-metal polysulfide fluxes was investigated along with compound formation and the As3+/As5+ interplay vis-a-vis changes in the flux basicity. The compound Na2EuAs2S5 containing trivalent As3+ is stabilized from an arsenic-rich polysulfide flux. It crystallizes in the monoclinic centrosymmetric space group P21/c. Na2EuAs2S5 has [As2S 5]4- units, built of corner sharing AsS3 pyramids, which are coordinated to Eu2+ ions to give a two-dimensional (2D) layered structure. A sodium polysulfide flux with comparatively less arsenic led to the As5+ containing compounds NaEuAsS4 (orthorhombic, Ama2) and Na4Eu(AsS 4)2 (triclinic, P1) depending on Na2S/S ratio. The NaEuAsS4 and Na4Eu(AsS4)2 have a three-dimensional (3D) structure built of [AsS4]3- tetrahedra coordinated to Eu2+ ions. All compounds are semiconductors with optical energy gaps of ~2 eV.
Kingzett
, p. 456 - 456 (1873)
Kraus, C. A.,Ridderhof, J. A.
, p. 79 - 86 (1934)
Mixed thio/oxo orthovanadates Na3[VSxO4-x] (x = 2, 3): Synthesis - crystal structures - properties
Schnabel, Simone,R?hr, Caroline
, p. 479 - 490 (2005)
Mixed sodium thio/oxo orthovanadates(V), dark red Na3[VS 3O] and orange red Na3[VS2O2], were synthesized via reactions in the melt starting from V, Na, Na2S, Na2O and sulfur. The structure of the low temperature phase of Na3[VS3O] (space group Pnma, a = 589.5(3), b = 962.8(5), c = 1186.6(6) pm, Z = 4, R1 = 0.0494) contains anions [VS3O] 3- almost identical to those known from the high temperature form, β-Na3[VS3O] (space group Cmc21, a = 968.4(4), b = 1194.6(4), c = 590.5(2) pm, Z = 4, R1 = 0.0291). The second order phase transition between these two forms at 536°C was studied by temperature dependent powder diffraction and explained on the basis of a comparison of the anion packing in the two related structures. The packing of the dithiodioxovanadate anions in Na3[VS2O2] (space group Pbca, a = 1162.7(2), b = 592.71(12), c = 1766.7(4) pm, Z = 8, R1 = 0.0312) is also closely related. The chemical bonding in the anions [VS 3O]3- and [VS2O2]3- of approximately ideal C3v and C2v symmetry is discussed on the basis of FP-LAPW band structure calculations and force constants obtained from Raman spectroscopy. The decrease of the calculated band gaps with increasing S content x in Na3[VSxO4-x] is in accordance with the optical properties showing a gradually deepening of the crystal and solution colour. Discernible trends in the chemical bonding in this series of mixed thio-oxo anions also include the amount of π bonding of the V-O and V-S bonds and the corresponding variation of force constants and V-O/V-S distances.
An efficient method for synthesizing dimethylsulfonio-34S-propionate hydrochloride from 34S8
Wirth, Joseph S.,Whitman, William B.
, p. 52 - 58 (2019/01/04)
Dimethylsulfoniopropionate (DMSP, (2-carboxyethyl)dimethylsulfonium) is a highly abundant compound in marine environments. As a precursor to the climatically active gas, dimethylsulfide (DMS), DMSP connects the marine and terrestrial sulfur cycles. However, the fate of DMSP in microbial biomass is not well understood as only a few studies have performed isotopic labeling experiments. A previously published method synthesized 34S-labeled DMSP from 34S8, but the efficiency was only 26% and required five separate reactions, expensive reagents, and purification of the products of each reaction. In this study, a method of synthesizing 34S-labeled DMSP from 34S8 is described. Improvements include elemental steps, inexpensive reagents, purification of only one intermediate, and less time to complete. The efficiency of this method is 65% and results in pure DMSP with more than 98% isotope enrichment as determined by 1H-nuclear magnetic resonance (NMR) and gas chromatography–mass spectrometry (GC–MS).