Untersuchungen zur Umsetzung von [Lithium(trimethylsilyl)amido]-methyl-trimethylsilylamino-silan Me(Me3SiNLi)(Me3SiNH)SiH mit verschiedenen Elektrophilen

Investigations of the Reaction between the [Lithium(trimethylsilyl)amido]-methyl-trimethyl-silylamino-silane Me(Me₃SiNLi)(Me₃SiNH)SiH and different Electrophiles The lithium silylamide Me(Me₃SiNLi)(Me₃SiNH)SiH 1 reacts with chlorotrimethylsilan in the nonpolar solvent n-hexane to the N-substitution product Me[(Me₃Si)₂N](Me₃SiNH)SiH 2 and to the cyclodisilazane [Me(Me₃SiNH)Si—N(SiMe₃)]₂ 3 nearly in same amounts. The reaction of 1 with chlorotrimethylstannane gives besides small amounts of the cyclodisilazane 3 the N-substitution product Me[(Me₃Si)(Me₃Sn)N](Me₃SiNH)SiH 4 . By the reaction of 1 with trimethylsilyltriflate the cyclodisilazane 3 is obtained as the main product. Furthermore 2 and the cyclodisilazane 5 are formed. Ethylbromide shows no reaction with 1 under the same conditions. These results indicate the existence of an equilibrium of the lithium silylamide 1 , the silanimine Me(Me₃SiNH)Si?N(SiMe₃) and lithium hydride.     

Highly chemoselective coupling of allenylstannanes with organic iodides promoted by Pd(PPh3)4/LiCl: an efficient method for the synthesis of substituted allenes

An efficient method for the preparation of various monosubstituted arylallenes, disubstituted allenes and alkenylallenes via palladium-catalyzed coupling of allenylstannanes with aryl iodides or alkenyl iodides is described. The coupling reaction was carried out in the presence of Pd(PPh₃)₄ and LiCl using DMF as solvent. The possible role of LiCl in this coupling process is discussed based on the ¹¹⁹Sn NMR studies.     

Li2Br(NH2): Das erste ternäre Alkalimetallamidhalogenid

Li₂Br(NH₂): The First Ternary Alkali Metal Amide Halide The pseudobinary system LiNH₂/LiBr was investigated by X-ray methods. The crystal structure of the compound Li₂Br(NH₂) was solved by single crystal data: Li₂Br(NH₂): Pnma, Z = 8, a = 12.484(2) Å, b = 7.959(1) Å, c = 6.385(1) Å, Z(F_o) with (F_o)² ≧ 3σ(F_o)² = 348, Z (parameter) = 51, R/R_w = 0.019/0.021 Li₂Br(NH₂) crystallizes in a new type of structure. To one another isolated chains of [Li₂Li_4/2(NH₂)₂²⁺] show the motif of closest rod packing. They are connected via bromide ions in a distorted cubic primitive arrangement.     

多步法制备纳米钛酸钡

采用醋酸钡、碳酸钾、钛酸丁酯等为初始反应物，通过多步反应的方法，制得了纳米钛酸钡。所得产品采用XRD、TEM和SEM等进行了表征，并对生长机理进行了分析。研究结果表明，得到的碳酸钡为直径约100 nm的纳米棒，再经室温下钛酸丁酯水解产生二氧化钛对碳酸钡纳米棒进行包覆，可得到一维核-壳结构的碳酸钡/二氧化钛，最后于700 ℃下经固相反应而得到钛酸钡的纳米颗粒。这种制备纳米钛酸钡的方法可以有效地控制产品形貌及粒径。     

The investigation of the (p,ρ,T) and (ps,ρs,Ts) properties of {(1−x)CH3OH + xLiBr} for the application in absorption refrigeration machines and heat pumps

The (p,ρ,T) and (p_s,ρ_s,T_s) properties of {(1−x)CH₃OH + xLiBr} over a wide range of state parameters are reported for the first time. The experiments were carried out in a constant volume piezometer over a temperature range from 298.15 K to 398.15 K, at 0.08421, 0.13617, 0.19692, 0.23133 and 0.26891 mole fractions and from atmospheric pressure up to 60 MPa. The experimental uncertainties are ΔT=±3 mK for temperature, Δp=±5·10⁻² MPa for high pressure and Δp=±5·10⁻⁴ MPa for atmospheric pressure, Δρ=±3·10⁻² kg · m⁻³ for density. An equation of state was derived for correlation of the experimental data of the solutions.     

Novel siloxane polymers as polymer electrolytes for high energy density lithium batteries

A variety of disubstituted (double-comb) polysiloxane polymers have been prepared containing linear, branched, and cyclic oligoethyleneoxide units, –(OCH₂CH₂)_n–, in the side chains and as part of the siloxane backbone. Copolymers, using mixtures of linear ethylene oxide side chains, were also synthesized. These polymers were doped with LiN(SO₂CF₃)₂ (LiTFSI, 1) and conductivities of the polymer-salt complexes were determined as a function of temperature and doping level. The maximum conductivity of these polymers at 25 ° C was 2.99 ×10^–4, for a copolymer containing equimolar amounts of side chains with n = 5 and 6.     

尖晶石构造LiCu0.5Mn1.5O4的合成及其在水溶液中对Li^＋的抽出／嵌入反应

尖晶石构造ＬｉＣｕ０．５Ｍｎ１．５Ｏ４的合成及其在水溶液中对Ｌｉ＋的抽出／嵌入反应董殿权钟杰柳敦雷刘亦凡＊（青岛化工学院化学工程系青岛２６６０４２）关键词尖晶石，Ｌｉ－Ｃｕ－Ｍｎ复合氧化物，合成，锂离子交换１９９７－０９－１７收稿，１９９７－１２－２...     

Vibrational Spectroscopic Study on Ion Solvation and Association of Lithium Perchlorate in 4-Methoxymethyl-ethylene Carbonate

Solvation interaction and ion association in solutions of lithium perchlorate/4-methoxymethyl-ethylene carbonate （MEC） have been studied by using Infrared and Raman spectra as a function of concentration of lithium perchlorate. The splitting of ring deformation band and ring ether asymmetric stretching band, and the change of carbonyl stretching band suggest that there should be a strong interaction between Li^＋ and the solvent molecules, and the site of solvation should be the oxygen atom of carbonyl group. The apparent solvation number of Li^＋ was calculated by using band fitting technique. The solvation number was decreased from 3.3 to 1.1 with increasing the concentration of LiClO4/MEC solutions. On the other hand, the band fitting for the ClO4^- band revealed the presence of contact ion pair, and free ClO4^- anion in the concentrated solutions.     

Investigation of the Crystallisation Behaviour of Lead Titanate (PT), Lead Zirconate (PZ) and Lead Zirconate Titanate (PZT) by EXAFS-Spectroscopy and X-Ray Diffraction

Two solid solutions of lead zirconium titanates PbZr _x Ti_{1 – x} O₃ (x = 0.1 and 0.35) as well as the reference compounds lead titanate and lead zirconate were prepared from zirconium and titanium n-propoxide, dissolved in 2-methoxyethanol, by sol-gel process. The amorphous products after pyrolysis of the dried gels and the crystalline phases were studied by EXAFS spectroscopy to monitor the structural changes from the amorphous oxide mixture to the crystalline ceramics after calcination. Additionally, the crystalline phases were identified by X-ray diffraction (XRD).It follows from the analysis of the EXAFS data that the local order of the amorphous phases seems to be completely different from that of the crystalline phase. There is no indication of a preformation of the local order of the perovskite structure. The analysis of our EXAFS spectra can be interpreted very consistently with the assumption that in the amorphous samples a segregation exists on molecular level and the low crystallisation temperatures are a consequence of very short diffusion paths.     

Zwei neue Silicat-Chloride mit zweiwertigem Europium: LiEu3[SiO4]Cl3 und Li7Eu8[SiO4]4Cl7

Two New Silicate-Chlorides with Divalent Europium: LiEu₃[SiO₄]Cl₃ and Li₇Eu₈[SiO₄]₄Cl₇ LiEu₃[SiO₄]Cl₃ was prepared by reaction of LiCl with Eu₂SiO₄ and Li₇Eu₈[SiO₄]₄Cl₇ from Li with Eu₂O₃, SiO₂ and LiCl. The crystal structures of LiEu₃[SiO₄]Cl₃ (Pmna, a = 946.95(13); b = 699.52(8); c = 1 368.0(2) pm; Z = 4; R1 = 0.0325, R2_w = 0.0642) and Li₇Eu₈[SiO₄]₄Cl₇ (P2₁/c; a = 851.85(5); b = 948.62(7); c = 1 679.0(2) pm; β = 96.221(8)°; Z = 2; R1 = 0.0352, R2_w = 0.0744) were determined from four-circle diffractometer data. LiEu₃[SiO₄]Cl₃ contains [Li(SiO₄)₂] units and LiCl₆ octahedra while in Li₇Eu₈[SiO₄]₄Cl₇ larger ?lithosilicate”? groups are found. In both structures, the Eu²⁺ ions are coordinated mostly eightfold by O^2? and Cl^? ligands.