20859-73-8Relevant articles and documents
In Search of Aluminum Hexathiohypodiphosphate: Synthesis and Structures of ht-AlPS4, lt-AlPS4, and Al4(P2S6)3
Kuhn, Alexander,Eger, Roland,Ganter, Pirmin,Duppel, Viola,Nuss, Jürgen,Lotsch, Bettina V.
, p. 2663 - 2668 (2016/02/23)
We report the high-pressure synthesis and the structure of aluminum hexathiohypodiphosphate, Al4(P2S6)3, along with the redetermination of the structures of two modifications of AlPS4. Al4(P2S6)3 crystallizes in the monoclinic space group C2 with a = 17.584(3), b = 10.156(2), c = 6.698(1) ?, β = 106.93(1) in a superstructure of the layered FePS3 structure type with tripled a axis. Hereby, Al3+ occupies 2/3 of the Fe2+ sites in an ordered fashion. The structure model obtained from single-crystal X-ray diffraction was corroborated by TEM-PED. The low-temperature modification of AlPS4 with platelet-like morphology shows tetragonal symmetry [space group P bar42c, a = b = 5.6572(9), c = 9.220(2) ?]. The orthorhombic high-temperature modification with fibrous needle-like morphology of AlPS4 is isotpyic with BPS4 [space group I222, a = 5.660(2), b = 5.759(2), c = 9.189(2) ?].
The phase transition of ZrP induced by Si in Al-Si melts
Bao, Guoju,Li, Dakui,Nie, Jinfeng,Liu, Xiangfa
, p. 45 - 50 (2012/06/30)
In this article, the reaction process of ZrP in Al-Si melts was investigated, and by the results of XRD, EDS and FESEM, the AlP and (Al, Zr, Si) phases were observed, indicating that the phase transition of ZrP phase has carried out in Al melts induced by Si. Detailed investigation confirmed that the finer particle of (Al, Zr, Si) phase is the type of ZrAl3 doped with trace Si and the coarser block is the type of ZrSi2 doped with trace Al. Furthermore, it is found that when the ZrP phase was added into Al-Si melts, Si atoms accumulated around ZrP phase, forming Si deficiency-layer and Si enrichment-layer. The concentration gradient of Si leads to two types of transition process of the ZrP phase in Al melt. Finally, the reaction mechanism of ZrP with Al-Si alloys was analyzed.
Preparation of Al, Cr, Nb, Mo, and W monophosphides from a lithium metaphosphate melt
Lesnyak,Stratiichuk,Sudavtsova,Slobodyanik
, p. 1274 - 1277 (2007/10/03)
Synthesis of a series of phosphides (AlP, CrP, NbP, MoP, and WP) by reactions of powdered metals with a melt of lithium metaphosphate LiPO3 was studied. Thermodynamic parameters (ΔH2980, ΔS2980, ΔG2980, and ΔG12730) of the reactions were calculated and their temperature modes were optimized on the basis of the standard thermodynamic characteristics of the initial substances and the reaction products. X-ray patterns of the powders of the obtained compounds are presented.
Electrical Discharge-Assisted Production of a bcc Aluminum Phosphide Phase
Rybachenko,Kazbanov,Trofimov,Olado
, p. 481 - 484 (2008/10/08)
A bcc aluminum phosphide phase was produced with the assistance of a low-power spark discharge. This phase is isostructural to high-pressure Si(II) (which exists under pressures above 20 GPa). X-ray powder diffraction, gravimetric, and chemical analysis evidence concerning samples dissolved in HCl and NaOH and thermally oxidized is reported. The silicon, iron, and nickel concentrations found by emission spectroscopy are also reported.
Reactions of H3Al-NMe3 with E(SiMe3)3 (E = P, As). Structural Characterization of the Trimer [H2AIP(SiMe3)2]3 and Base-Stabilized Adduct [H2AIAs(SiMe3)2]-NMe3 and Their Thermal Decomposition toward Nanocrystalline AIP and AIAs, Respectively
Janik, Jerzy F.,Wells, Richard L.,White, Peter S.
, p. 3561 - 3566 (2008/10/08)
Dehydrosilylation reactions in diethyl ether between H3Al-NMe3 and E(SiMe3)3 afforded for E = P a high yield of the trimer [H2AlP(SiMe3)2]3 (1), while for E = As a monomeric base-stabilized adduct [H2AlAs(SiMe3)2]NMe3 (2) as well as its degradation solid product were obtained. No reaction occurred for E = N. The singlecrystal X-ray structure determination for 1 yielded a planar six-membered ring of alternating four-coordinated Al and P centers. The structural solution for 2 revealed the monomeric unit [H2AlAs(SiMe3)2] stabilized by coordination of NMe3 at the Al site. Pyrolysis of 1 at 450 °C promoted further dehydrosilylation and yielded a product which by XRD spectroscopy showed the onset of AlP crystallinity while at 950 °C afforded nanocrystalline AlP with 5 nm average panicle size. Pyrolysis of 2 at 450 °C resulted in the formation of nanocrystalline AlAs with 2 nm average particle size. Under applied pyrolysis conditions for 1 and 2, the target elimination-condensation pathway via dehydrosilylation was accompanied by other decomposition side reactions and retention of some contaminant residues.
Synthesis of III-V semiconductors by solid-state metathesis
Treece, Randolph E.,Macala, Gerald S.,Rao, Lin,Franke, Deanna,Eckert, Hellmut,Kaner, Richard B.
, p. 2745 - 2752 (2008/10/08)
Solid-state precursor reactions have been investigated as a general synthetic route to binary III-V (13-15) compounds. The generic reaction scheme MX3 + Na3Pn → MPn + 3 NaX (M = Al, Ga, In; X = F, Cl, I; Pn = pnictogen = P, As, Sb) has been used to prepare crystalline powders of the III-V semiconductors. The reaction mixtures can be either heated in sealed tubes or ignited with a hot filament, and the byproduct salts are simply removed by washing with an appropriate solvent. The ignited reactions are self-propagating and highly exothermic, owing to the formation of 3 mol of sodium halide. Products from both types of reactions have been characterized by powder X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, and solid-state NMR. In some cases, the products of the ignited solid-state metathesis (SSM) reactions differ from those of the sustained heating reactions. These differences provide clues as to reaction pathways in the solid-state precursor reactions.
Synthesis and characterization of phosphinosilylalanes from [(CH3)3Si]3Al. Crystal and molecular structure determinations of {[(CH3)3Si]2AlP(C6H 5)2}2, {[(CH3)3Si]2AlP(C6H 5)[Si(CH ...
Janik, Jerzy F.,Duesler, Eileen N.,McNamara, William F.,Westerhausen, Matthius,Paine, Robert T.
, p. 506 - 514 (2008/10/08)
Full title: Synthesis and characterization of phosphinosilylalanes from [(CH3)3Si]3Al. Crystal and molecular structure determinations of {[(CH3)3Si]2AlP(C6H 5)2}2, {[(CH3)3Si]2AlP(C6H 5)[Si(CH3)3]}2, {[(CH3)3Si]2AlP(H)(c-C6H 11)}3, and [{[(CH3)3Si]2N}(C6H 5)P]2. The reactions of [(CH3)3Si]3Al·O(C2H 5)2 with phosphines (C6H5)2PCl, PCl3, {[(CH3)3Si]2N}(C6H5)PCl, (C6H5)2PH, [(CH3)3Si](C6H5)PH, (C6H5){[(CH3)3Si]2N}PH, (C-C6H11)PH2, and PH3 were surveyed. Reactions of the chlorophosphines led to formation of di- or polyphosphines, and the molecular structure of [{[(C-H3)3Si]2N}(C6H 5)P]2 was determined by single-crystal X-ray diffraction analysis. The compound crystallized in the tetragonal space group I41/a with a = 24.379 (9) A?, c = 10.778 (3) A?, Z = 8, V = 6405.8(4) A?, and ρcalcd = 1.11 g cm-3. Least-squares refinement gave RF = 6.3% and RwF = 5.3% on 1613 reflections with F ≥ 4σ(F). The diphosphine has C1 symmetry, and each phosphorus atom has pseudotetrahedral geometry: P-P = 2.270 (3) A? and P-N = 1.724 (4) A?. The remaining phosphines form Lewis acid-base complexes with [(CH3)3Si]3Al and/or undergo elimination/condensation chemistry resulting in production of phosphinoalane ring compounds or polymers. The molecular structures of three additional compounds have been determined by single-crystal X-ray diffraction analysis. The compound {[(CH3)3Si]2AlP(C6H 5)2}2 crystallized in the triclinic space group P1 (No. 2) with a = 10.989 (3) A?, 6 = 20.576 (5) A?, c = 21.000 (5) A?, α = 101.52 (2)°, β = 102.17 (2)°, γ = 100.86 (2)°, Z = 4, V = 4414 (2) A?3, and ρcalcd = 1.08 g cm-3. Least-squares refinement gave RF = 11.3% and RwF = 9.6% on 7466 reflections with F > 3σ(F). The compound {[(CH3)3Si]2AlP(C6H 5)[Si(CH3)3]}2 crystallized in the monoclinic space group P21/n with a = 11.360 (8) A?, b = 12.215 (7) A?, c = 16.673 (12) A?, β = 102.13 (5)°, Z = 2, V = 2261 (2) A?3, and ρcalcd = 1.04 g cm-3. Least-squares refinement gave RF = 9.9% and RwF = 7.7% on 2718 reflections with F ≥ 3σ(F). The compound {[(CH3)3Si]2AlP(H)(c-C6H 11)}3 crystallized in the triclinic space group P1 (No. 2) with a = 12.564 (2) A?, b = 12.935 (3) A?, c = 19.149 (4) A?, α = 83.66 (2)°, β = 88.64 (2)°, γ = 66.65 (1)°, Z = 2, V = 2839 (1) A?3, and ρcalcd = 1.01 g cm-3. Least-squares refinement gave RF = 11.3% and RwF = 8.6% and 5213 reflections with F ≥ 3σ(F). The first two compounds contain planar four-membered (ALP)2 rings with C1 symmetry and average Al-P distances of 2.455 and 2.466 A?, respectively. The third compound forms a six-membered skew-boat cyclohexane-like (AlP)3 ring with an E, E, A conformation and an average Al-P distance of 2.444 A?. Pyrolysis of a polymeric product obtained from reactions involving PH3 and [(C-H3)3Si]3Al·O(C2H 5)2 resulted in formation of aluminum phosphide, AlP.
Organometallic Chemical Vapor Deposition of III/V Compounds Semiconductors with Novel Organometallic Precursors
Cowley, Alan H.,Benac, Brian L.,Ekerdt, John G.,Jones, Richard A.,Kidd, Kenneth B.,et al.
, p. 6248 - 6249 (2007/10/02)
We have found that compounds of type 1 are excellent single source precursors for the preparation of III/V compound semiconductor materials such as GaAs and InP under relatively mild conditions.
SYNTHESIS AND REACTIVITY OF METALLOPHOSPHANES
Paine, Robert T.,McNamara, William F.,Janik, Jerzy Fr.,Duesler, Eileen N.
, p. 241 - 244 (2007/10/02)
Aspects of the reactivity of metallophosphanes are presented along with the synthesis and structure determinations for new aluminophosphanes.
