Synthesis and characterization of iron silicon boron (Fe5Si2B) and iron boride (Fe3B) nanowires

Single-crystal iron silicon boron (Fe(5)Si(2)B) and iron boride (Fe(3)B) nanowires were synthesized by a chemical vapor deposition (CVD) method on either silicon dioxide (SiO(2)) on silicon (Si) or Si substrates without introducing any catalysts. FeI(2) and BI(3) were used as precursors. The typical size of the nanowires is about 5-50 nm in width and 1-20 mum in length. Different kinds of Fe-Si-B and Fe-B structures were synthesized by adjusting the ratio of FeI(2) vapor to BI(3) vapor. Single-crystal Fe(5)Si(2)B nanowires formed when the FeI(2) sublimator temperature was kept in the range of 540-570 degrees C. If the FeI(2) sublimator temperature was adjusted in the range of 430-470 degrees C, single-crystal Fe(3)B nanowires were produced. Fe(3)B nanowires grow from polycrystalline Fe(5)SiB(2) particles, while Fe(5)Si(2)B nanowires grow out of the Fe(5)Si(2)B layers, which are attached to triangle shaped FeSi particles. Both the ratio of FeI(2) vapor to BI(3) vapor and the formation of the particles (Fe(5)SiB(2) particles for the growth of Fe(3)B nanowires, FeSi particles for the growth of Fe(5)Si(2)B nanowires) are critical for the growth of Fe(3)B and Fe(5)Si(2)B nanowires. The correct FeI(2) vapor to BI(3) vapor ratio assures the desired phase form, while the particles provide preferential sites for adsorption and nucleation of Fe(3)B or Fe(5)Si(2)B molecules. Fe(3)B or Fe(5)Si(2)B nanowires grow due to the preferred growth direction of <110>.     

Preparation of Gd2O3:Yb,Er and Gd2O2S:Yb,Er infrared-to-visible conversion phosphor ultrafine particles using an emulsion liquid membrane system

Upconverting phosphor fine particles (Gd2O3:Yb,Er and Gd2O2S:Yb,Er) have been prepared, using an emulsion liquid membrane (ELM, water-in-oil-in-water (W/O/W) emulsion) system. The composite Gd-Yb-Er oxalate particles obtained in the ELM system were mainly 20-60 nm in size, together with a smaller amount of submicrometer-sized spherical particles. Nanometer-sized Gd2O3:Yb,Er and Gd2O2S:Yb,Er particles were obtained by calcination in air and in sulfur atmosphere, respectively, of the precursor oxalate particles prepared in the ELM system. Upconversion emissions (red and green) were obtained from the Gd2O3:Yb,Er and Gd2O2S:Yb,Er particles prepared in the ELM system under infrared excitation (lambdaex=980 nm) via a two-photon process. Upconversion phosphor fine particles, about 50 nm in diameter, may be applied to the luminescent reporter material for the detection of the targeted analyte in immunoassays or DNA assays.     

Nanoparticles from the Vapor Phase: Synthesis and Characterization of Si, Ge, MoO3, and WO3Nanocrystals

In this paper, we present two studies of nanocrystals prepared by the pulsed laser vaporization–controlled condensation (LVCC) technique. In the first study, we present a comparison between the surface oxidation, morphology and the photoluminescence (PL) properties of Si and Ge nanocrystals. In the second study, we compare the photochromic properties of Mo and W oxides nanoparticles with the properties of the corresponding bulk materials. We also present evidence for a novel photoreduction of the white WO₃ nanoparticles into the blue W₂O₅ following the irradiation of the particles with the second harmonic of the Nd:YAG laser in air. These studies illustrate the novel properties of the nanoscale particles, which could lead to significant practical and technological applications.     

Phase-controlled growth of metastable Fe5Si3 nanowires by a vapor transport method

We report the synthesis of single-crystalline nanowires (NWs) of metastable Fe5Si3 phase via an iodide vapor transport method. Free-standing Fe5Si3 NWs are grown on a sapphire substrate placed on a Si wafer without the use of any catalyst. The typical size of the Fe5Si3 nanowires is 5-15 microm in length and 100-300 nm in diameter. Synthesis of the metastable phase is induced by composition-dependent nucleation from the gas-phase reaction. Depending on the concentration ratio of FeI2(g) to SiI4(g), different phases of iron silicides are formed. The growth of nanowires is facilitated by the initial nucleation of silicide particles on the substrate and further self-seeded growth of the NWs. The present work not only provides a method for the synthesis of metastable Fe5Si3 nanowires but also suggests that the phase controlled synthesis can be further optimized to produce other metal-rich silicide nanostructures for future spintronic devices.     

Size distribution and characteristics of chemical components in ambient particulate matter.

Ambient particulate matter and gas in Kyoto were investigated by gravimetric analysis, X-ray fluorescence spectrometry, and ion chromatography in order to clarify their behavior and origin. The size distribution and characteristics of the chemical components in ambient particulates collected on PTFE membrane filters using an Andersen air sampler were examined from August 2001 to April 2004. A four-stage filter pack method was used to sample the atmosphere for the determination of gas (SO2, HNO3, HCl, NH3) and particulate matter (SO42, NO3, Cl-, Na+, K+, Ca2+, Mg2+, NH4+) concentrations from October 2002 to April 2004. The concentration of SPM mass was in the range of 6.7 - 80.2 microg/m3. The size distributions of SPM mass were bimodal, peaking at around 0.65 - 1.1 and 3.3 - 4.7 microm, and 40 - 85% of SPM mass was fine particles (< 2.1 microm). Na, Mg, Al, Si, Ca, Cl, and Fe were mainly present in coarse particles (2.1 to 11.0 microm), while S was present in fine particles. The concentrations of Al, Si, Ca, Mg, and Fe in fine particles increased from March to April in 2002, and those in coarse particulates increased in November 2002 and from March to April in 2004. This may be the effect of the continental yellow sand "Kosa." The differences in the size distributions of Al, Si, Ca, Mg, and Fe in particles may depend on differences in their place of occurrence and course of transport from China to Japan. The concentration of HCl gas was higher than that of particulate chloride ion in summer. Nitric acid gas existed at higher concentrations in summer, but fine particulate nitrate ion was observed in winter. The gaseous-to-fine aerosol nitrate fraction became higher at warmer temperatures. Coarse sulfate was below 10%, and SO2 gas and fine particulate sulfate were above 90%.     

O／W微乳液中聚邻甲苯胺超微粒子的制备

聚邻甲苯胺具有较高的电导率、较好的贮存电荷的能力和良好的环境稳定性，因而具有较大的应用价值［’－‘j，其合成方法主要有电化学合成法和化学合成法［‘·’J．化学会成法所得聚邻甲苯肢的粒子一般大于100urn．近年来，以表面活性剂聚集体微乳液、溶致液晶为介质，制备超微粒子材料已为人们所关注「’－’］．以微乳液为介质进行聚合反应亦引起重视，但大部分微乳液聚合都是在四组分微乳液（表面活性剂、助表面活性剂、单体和水）中进行‘”·“‘．近年来，某些油溶性单体已成功地在无助表面活性剂的三组分微乳液中聚合［‘’·‘’1…     

Dimerization of A-alpha-[SiNb(3)W(9)O(40)](7-) by pH-controlled formation of individual Nb-mu-O-Nb linkages

The reversible, stepwise formation of individual Nb-mu-O-Nb linkages during acid condensation of 2 equiv of A-alpha-[SiNb(3)W(9)O(40)](7-) (1) to the tri-mu-oxo-bridged structure A-alpha-[Si(2)Nb(6)W(18)O(77)](8-) (4) is demonstrated by a combination of X-ray crystallography and variable-pD solution (183)W and (29)Si NMR spectroscopy. Addition of DCl to a pD 8.4 solution of 1 (Li(+) salt in D(2)O) results in formation of a mono-Nb-mu-O-Nb-linked dimer, A-alpha-[Si(2)Nb(6)W(18)O(79)](12-) (2; pD = 3.0-1.3). At pD values between 1.6 and 0.3, two isomers (syn and anti) of the di-mu-oxo-bridged dimer, A-alpha-[Si(2)Nb(6)W(18)O(78)](10-) (3), are observed by (183)W NMR (C(2v) and C(2h) symmetry for the syn and anti isomers, respectively; 5 (183)W NMR signals for each isomer in the ratio 2:2:2:2:1). X-ray-quality crystals of syn-3 were isolated in 53% yield (syn-A-alpha-Cs(8)H(2)[Si(2)Nb(6)W(18)O(78)].18H(2)O, orthorhombic, Cmcm, a = 40.847(2), b = 13.2130(7), and c = 16.8179(9) A at 173K, Z = 4, final R(1) = 0.0685). At the low-pD limit of -0.08 (1.2 M DCl), 4 alone is observed. Additional supporting data are provided by variable-pD (29)Si NMR spectroscopy. Reversibility of the above processes was subsequently demonstrated by acquisition of (183)W NMR spectra after incremental additions of LiOH to D(2)O solutions of 4 to effect its stepwise hydrolysis to 2 equiv of 1.     

Microstructural and Mechanical Properties of Al-20%Si Containing Cerium

In this paper the effect of cerium addition in hypereutectic Al-Si alloys was studied. Casting method was used to produce Al-20Si with variation of Ce contents. The sample characterization studied was investigated by Optical Microscope, X-ray fluorescence and X-ray Diffraction. Vickers microhardness and wear test was carried out to study the influence of Ce towards the Al-20Si alloys. The addition of Ce in the Al-20Si alloys refined the Si primary phase as the Ce content increases. The results showed that the addition of 0.46 to 2.24 wt.% of cerium in Al-20Si alloys led to the formation of fine cells dispersed in the Al-matrix. These fine cells consist of a mixture of eutectic Si particles and intermetallic Al3Ce and CeAl1.2Si0.8 phase in Al matrix. The amount of rod- like intermetallic Al3Ce and CeAl1.2Si0.8 phase increases with increasing Ce content. The microhardness of Al-20Si alloys increases with the increase in Ce content. Addition of Ce up to 1.61 wt.% Ce improve the wear properties of Al-20Si alloy.     

Si(SiMe3)3]3Ge9M(CO)3(-) (M=Cr, Mo, W): coordination chemistry with metalloid clusters

Very recently it was shown that the metalloid cluster compound {Ge(9)[Si(SiMe(3))(3)](3)}(-)1 can be used for subsequent reactions as the shielding of the cluster core is rather incomplete. So the reaction of 1 with Cr(CO)(3)(CH(3)CN)(3) leads to a cluster enlargement where the chromium atom is incorporated into the cluster core. Here further applications of 1 as a flexible ligand in coordination chemistry are presented where the reaction of 1 with Mo(CO)(3)(EtCN)(3) and W(CO)(3)(CH(3)CN)(3) leads to [(CO)(3)MoGe(9)R(3)](-)4 and [(CO)(3)WGe(9)R(3)](-)5 respectively (R = Si(SiMe(3))(3)), showing that 1 can indeed be used as a flexible ligand in coordination chemistry. Structural and electronic properties of the Ge(9)M clusters 4 and 5 are discussed as well as mechanistic aspects of their formation.     

Synthesis,Structure of Organophosphonyl Polyoxotungstates of Formula [C_6H_(11)P(O)]_2 X~(n )W_(11)O_(39)~((8-n)-) (X~(n )=P~(5 ), Si~(4 ), B~(3 ), Ga~(3 ))

Derivatizedp0ly0x0metalates(POMs)havereceivedincreasingattenti011tbrthelas1twentyyearsowingtotheirpotentialinbifunctionalcatalysis'.Ithasbeenrec0gnizedforal0ngtimethattheversatiIityofthepoly0x0metalatesandtheircatalyticapplicati0ncanbesignificantlyincreasedbygraftingorganicand0rgan0metalIicgroup0ntothepoIyoxometalatesurface.Organophosph0nylderivatives0fheter0polyanionshavebeenreportedpreviously=.Asthecontinuation,werep0rtthesynthesisandcharacterizationofthetitlec0mpounds.Sodiumandpotassiums…     

[μ‐(Me3SiCH2Sb)5–Sb1,Sb3–{W(CO)5}2] und [{(Me3Si)2CHSb}3Fe(CO)4] – zwei cyclische Komplexe mit Antimon‐Liganden

Syntheses and Crystal Structures of [μ‐(Me₃SiCH₂Sb)₅–Sb¹,Sb³–{W(CO)₅}₂] and [{(Me₃Si)₂CHSb}₃Fe(CO)₄] – Two Cyclic Complexes with Antimony Ligands cyclo‐(Me₃SiCH₂Sb)₅ reacts with [(THF)W(CO)₅] (THF = tetrahydrofuran) to form cyclo‐[μ‐(Me₃SiCH₂Sb)₅–Sb¹,Sb³–{W(CO)₅}₂] ( 1 ). The heterocycle cyclo‐ [{(Me₃Si)₂CHSb}₃Fe(CO)₄] ( 2 ) is formed by an insertion reaction of cyclo‐[(Me₃Si)₂CHSb]₃ and [Fe₂(CO)₉]. The crystal structures of 1 and 2 are reported.     

Die Kristallstruktur von U2Cr3Si,U4Mn5Si3 und U2Co3Si

Zusammenfassung In den Dreistoffen: Uran–T (Ti,V,Cr,Mn,Co,Nb,W)–{Si,Al} werden Legierungen auf dem Schnitt U(T,Si)₂ bzw. U(T,Al)₂ aus den Komponenten hergestellt und röntgenographisch identifiziert^*. Es bestehen die ternären Verbindungen U₂Cr₃Si, U₄Mn₅Si₃ und U₂Co₃Si, die sich als mit MgZn₂ isotyp erweisen.     

RAPID SEPARATION OF FINE PARTICLES FROM DILUTE SUSPENSIONS

A potential rapid solid/liquid separation process of fine particles from dilute aqueous suspensions is introduced (tumbling method). This process involves the separation of one or two types of fine particles in aqueous suspension by heterocoagulation phenomena and is conducted by tumbling suspensions with a macroscopic collector such as glass beads which leads to the settling of particles with the collector. Particularly, it was found that silica (Si0₂: 0.12 μm) particles could effectively be collected by glass beads (80 μ.m) through a bridging effect of hematite (α-Fe₂0₃ : 0.10 μm ) particles. The results were explained in terms of the DLVO theory and the efficient movement of the glass beads collector

A chromatographic separation between silica and hematite particles is also proposed.     

UV-Induced Formation of [Fe(bpy)3]2+ Complex and its Confinement into Silica Fine Particles

Silica fine particles in a single or sub-micrometer regime, containing FeCl₃ and 2,2-bipyridine (bpy), were prepared by utilizing reverse micellar method. Formation of tris-bpy iron(II) ([Fe(bpy)₃]²⁺) complex was induced in the silica fine particles by UV irradiation at 365 nm. The starting micellar solution was obtained by an injection of 0.04 cm³ HCl aqueous solution into 5 cm³ tetraethyl orthosilicate (TEOS)/cyclohexane (2 cm³/3 cm³) mixed solution containing 4–14 vol% of nonionic surfactant, polyoxyethylene(5) nonylphenyl ether (NP-5). Size of the silica particles was regulated by the concentration of NP-5.     

气流粉碎分子筛性质和催化性能的研究

微颗粒分子筛的合成研究 ,已得到人们的充分重视 .用合成法可以得到粒径在 1 μm以下的微颗粒分子筛 ,它对于一些特征反应具有许多独特的性能 ,然而由于合成工艺的复杂性 ,还难以将其应用于工业生产 .气流粉碎又称流能磨 ,或称喷射磨 .与传统的机械粉碎机原理不同 ,它是利用高压气体通过喷嘴产生的高速气流所孕育的巨大动能 ,使物料颗粒发生互相冲击碰撞 ,或与固定板 (例如冲击板 )冲击碰撞 ,从而达到粉碎的目的 .其粉碎强度大 ,粉碎产品细、颗粒规整 ,颗粒在高速旋流中分级 ,成品粒度分布狭窄 .气流粉碎已在工业生产的诸多领域发挥了巨大作…     

Control of optical properties of gel-derived oxide coating films containing fine metal particles

Control of the optical properties of gel-derived oxide films containing fine metal particles is described. The duration of the aging of Si(OC₂H₅)₄-derived sols and the amount of water for hydrolyzing Si(OC₂H₅)₄ were found to greatly affect the size and the shape of Au particles formed in the silica matrix, and accordingly the optical absorption of the Au/SiO₂ composite films. Employing dielectric media with high refractive indices like TiO₂ was shown to shift the absorption peak of Au particles to longer wavelengths. Pd/TiO₂ and Pt/TiO₂ composite films showed absorption in the visible region.     

Transition‐Metal Complexes [(PMe3)2Cl2M(E)] and [(PMe3)2(CO)2M(E)] with Naked Group 14 Atoms (E=C–Sn) as Ligands; Part 2: Complexation with W(CO)5

Density functional calculations at the BP86/TZ2P level were carried out to understand the ligand properties of the 16‐valence‐electron(VE) Group 14 complexes [(PMe₃)₂Cl₂M(E)] ( 1ME ) and the 18‐VE Group 14 complexes [(PMe₃)₂(CO)₂M(E)] ( 2ME ; M=Fe, Ru, Os; E=C, Si, Ge, Sn) in complexation with W(CO)₅. Calculations were also carried out for the complexes (CO)₅W–EO. The complexes [(PMe₃)₂Cl₂M(E)] and [(PMe₃)₂(CO)₂M(E)] bind strongly to W(CO)₅ yielding the adducts 1ME–W(CO)₅ and 2ME–W(CO)₅ , which have C_2v equilibrium geometries. The bond strengths of the heavier Group 14 ligands 1ME (E=Si–Sn) are uniformly larger, by about 6–7 kcal mol^?1, than those of the respective EO ligand in (CO)₅W‐EO, while the carbon complexes 1MC–W(CO)₅ have comparable bond dissociation energies (BDE) to CO. The heavier 18‐VE ligands 2ME (E=Si–Sn) are about 23–25 kcal mol^?1 more strongly bonded than the associated EO ligand, while the BDE of 2MC is about 17–21 kcal mol^?1 larger than that of CO. Analysis of the bonding with an energy‐decomposition scheme reveals that 1ME is isolobal with EO and that the nature of the bonding in 1ME–W(CO)₅ is very similar to that in (CO)₅W–EO. The ligands 1ME are slightly weaker π acceptors than EO while the π‐acceptor strength of 2ME is even lower.     

原位反应合成Mo-Si化合物系复合材料

采用反应烧结法原位合成了Mo Si系化合物复合材料，利用X射线衍射仪、扫描电镜和电子探针等考察了材料的显微结构和相组成.结果表明，随原料粉中Mo含量的增加， Mo Si系反应生成物依次向MoSi2→Mo5Si3→Mo3Si变化；各相分布较为均匀，组织致密，晶粒细小.     

磁性Fe_3O_4微粒表面有机改性

在分散聚合法制备复合磁性微球过程中 ,采用硅烷偶联剂 KH- 570对磁性 Fe_3O_4微粒进行表面改性 .红外光谱 (FTIR)、光电子能谱 (XPS)分析结果表明 ,偶联剂与磁性微粒表面以化学键形式结合 .改性后 ,Fe_3O_4微粒与单体及其聚合物之间具有良好的亲和性 ,采用改性后的磁性微粒可以显著改善磁性微球的性能指标 .     

磁性Fe3O4微粒表面有机改性

在分散聚合法制备复合磁性微球过程中,采用硅烷偶联剂KH 570对磁性Fe3O4微粒进行表面改性.红外光谱(FTIR)、光电子能谱(XPS)分析结果表明,偶联剂与磁性微粒表面以化学键形式结合.改性后,Fe3O4微粒与单体及其聚合物之间具有良好的亲和性,采用改性后的磁性微粒可以显著改善磁性微球的性能指标.