四取代4-异丙苯基苯氧基酞菁铅复合凝胶玻璃的结构及光限幅性能研究

采用溶胶-凝胶(Sol-gel)湿化学工艺将四取代4-异丙苯基苯氧基酞菁铅PbPc(CP)₄掺入二氧化硅(SiO₂)凝胶玻璃基质,制备均匀掺杂的PbPc(CP)₄复合凝胶玻璃,并通过紫外-可见(UV-Vis)吸收光谱和透射电镜(TEM)图像对PbPc(CP)₄在复合凝胶玻璃中的存在状态及结构进行了表征。对PbPc(CP)₄在液相体系和固相体系中的光限幅性能分别进行了测试及对比研究。结果表明PbPc(CP)₄以团簇形式存在于复合凝胶玻璃中,并由于钢性结构固相基质的保护作用使其在复合凝胶玻璃相对于液相体系中表现出较强的光限幅特性。     

Synthesis and characterization of graphenated carbon nanotubes on IONPs using acetylene by chemical vapor deposition method

The graphenated carbon nanotubes (G-CNTs) were synthesized on monodisperse spherical iron oxide nanoparticles (IONPs) using acetylene as carbon precursor by simple chemical vapor deposition method. The reaction parameters such as temperature and flow of carbon source were optimized in order to achieve G-CNTs with excellent quality and quantity. Transmission electron microscopy (TEM) clearly illustrated that the graphene flakes are forming along the whole length on CNTs. The degree of graphitization was revealed by X-ray diffraction (XRD) analysis and Raman spectroscopic techniques. The intensity of D to G value was less than one which confirms the obtained G-CNTs have high degree of graphitization. The optimum reaction temperature for the IONPs to form metallic clusters which in turn lead to the formation of G-CNTs with high carbon deposition yield is at 900 °C. The TEM shows the CNTs diameter is 50 nm with foiled graphene flakes of diameter around 70 nm. Our results advocate for IONPs as a promising catalytic template for quantitative and qualitative productivity of nanohybrid G-CNTs. The produced G-CNTs with high degree of graphitization might be an ideal candidate for nanoelectronic application like super capacitors and so on.     

Different W cluster deposition regimes in pulsed laser ablation observed by in situ scanning tunneling microscopy

We report on how different cluster deposition regimes can be obtained and observed by in situ scanning tunneling microscopy by exploiting deposition parameters in a pulsed laser deposition process. Tungsten clusters were produced by nanosecond pulsed laser ablation in Ar atmosphere at different pressures and deposited on Au(1 1 1) and HOPG surfaces. Deposition regimes including cluster deposition-diffusion-aggregation, cluster melting and coalescence and cluster implantation were observed, depending on background gas pressure and target-to-substrate distance which influence the kinetic energy of the ablated species. These parameters can thus be easily employed for surface modification by cluster bombardment, deposition of supported clusters and growth of films with different morphologies. The variation in cluster mobility on different substrates and its influence on aggregation and growth mechanisms has also been investigated.     

Surface microstructure and magnetic behavior in FeSiB amorphous ribbons from magneto-optical Kerr effect

The magneto-optical Kerr effect (MOKE) completed by other surface sensitive methods as integral low-energy and conversion electron Mössbauer spectroscopy, scanning and transmission electron microscopy and by X-ray diffraction have been used with the aim to trace the surface microstructure and magnetic properties of FeSiB amorphous ribbons prepared by planar flow casting. The general composition of studied samples is Fe₈₀Si_xB_20−x, where x=4, 6, 8, 10 at.%.It is shown that MOKE used for magnetization, hysteresis loop, and domain structure determination is highly beneficial in a detection of both surface crystallization and local ordering of atoms into magnetically different clusters of amorphous structure. Moreover, a combination of blue and red laser with different penetration depths yields unique results concerning the surface anisotropy and depth sensitivity. In the case of samples with 4, 6, and 8 at.% Si MOKE detects two magnetically different phases diverging in coercivity values H_c, however, not varying with the sample composition. These phases have been identified by Mössbauer measurements as FeSi and FeB clusters. Their relationship changes with Si concentration. On the other hand, a strong increase in the surface H_c found for the sample with 10 at.% Si has indicated a nanocrystallization. It was confirmed by electron microscopy, Mössbauer and X-ray diffraction results. The size of nanocrystals has varied between 200 nm and 500 nm.     

Polysulfone as polymer matrix for a novel polymer-dispersed liquid crystals system

We report the preparation and thermotropic characterization of a novel polymer-dispersed liquid crystal (PDLC) system based on the polysulfone (PSU) UDEL-1700 as a polymer matrix and on 4-[4-(n-butyloxy)phenylene-imino-methylidene]benzonitrile as a liquid crystal. PDLC films have been prepared using the thermal-induced phase separation (TIPS) technique, with different compositions in the two components. A detailed optical polarized microscopy and differential scanning calorimetry study has been carried out to evaluate a correlation between the composite composition and the PDLC formation. We found that PSU could be a good matrix for the formation of PDLC systems.     

Hierarchical nanoparticle morphology for platinum supported on SrTiO3 (0 0 1): A combined microscopy and X-ray scattering study

The morphology of metal nanoparticles supported on oxide substrates plays an important role in heterogeneous catalysis and in the nucleation of thin films. For platinum evaporated onto SrTiO₃ (0 0 1) and vacuum annealed we find an unexpected growth formation of Pt nanoparticles that aggregate into clusters without coalescence. This hierarchical nanoparticle morphology with an enhanced surface-to-volume ratio for Pt is analyzed by grazing incidence small-angle X-ray scattering (GISAXS), X-ray fluorescence (XRF), atomic force microscopy (AFM) and high-resolution scanning electron microscopy (SEM). The nanoparticle constituents of the clusters measure 2-4 nm in size and are nearly contiguously spaced where the average edge-to-edge spacing is less than 1 nm. These particles make up the clusters, which are 10-50 nm in diameter and are spaced on the order of 100 nm apart.     

Preparation and characterization of “green” hybrid clay-dye nanopigments

We obtained a low cost and abundant nanopigment material composed of Rhodamine B (Rh-B) organic dye compound and Unye bentonite (UB) clay from Turkey. The characterization of the nanopigment was investigated using scanning electron microscopy (SEM), particle size distribution, powder X-ray diffraction (PXRD), Fourier transformed infra-red spectroscopy (FT-IR) and thermal analysis techniques. According to the result of texture analyses, we showed that the particle size distribution (d: 0.5-mean distribution) of Rh-B/UB nanopigment material was around 100 nm diameter. It was also demonstrated that the samples had a particle size around nm diameter in SEM images. As seen in the PXRD and thermal analysis, there is a difference in basal spacing by 1.46° (2θ) and a higher mass loss by 7.80% in the temperature range 200–500 °C compared to the raw bentonite.     

Nanometer-scale spatial inhomogeneities of the chemical and electronic properties of an ion implanted Mn-Ge alloy

Electron energy loss spectroscopy maps using a transmission electron microscope were used to investigate with nanometer spatial resolution the Mn distribution of a Mn_xGe_1−x ion implanted alloy (x ? 4%). Mn is fully diluted in the Ge matrix in a subsurface implanted layer, showing concentration inhomogeneities at the nm scale. In the deep implanted layers the presence of Mn rich clusters—either amorphous or in the Mn₅Ge₃ phase—is directly evidenced. Scanning Tunneling Microscopy/Spectroscopy directly shows that the Mn₅Ge₃ clusters are metallic, while those smaller and amorphous are semiconducting with 0.45 ± 0.05 eV band gap. The Ge matrix with Mn dilution is semiconducting with 0.60 ± 0.05 eV gap. Electronic structure results are compared with ab-initio calculations.     

Thickness-dependent magnetic domain structures of Co ultra-thin film investigated by scanning transmission X-ray microscopy

Thickness-dependent magnetic domain structure of ultrathin Co wedge films (0.3 nm–1.0 nm) sandwiched by Pt layers was investigated by scanning transmission x-ray microscopy (STXM) employing X-ray magnetic circular dichroism (XMCD), utilizing elliptically polarized soft x-rays and electromagnetic fields, with a spatial resolution of 50 nm. The magnetic domain images measured at the Co L₃ edge showed the evolution of the magnetic domain structures from maze-like form to the bubble-like form as the perpendicular magnetic field was applied. The asymmetric domain expansion of a 500 nm-scale bubble domain was also measured when the in-plane and perpendicular external magnetic field were applied simultaneously.     

Ge在Si(111)7×7表面的选择性吸附

利用超高真空扫描隧道显微镜研究了室温条件下Ge在Si(111)7×7表面上初期吸附过程.在Ge所形成团簇中存在一个临界核.这些Ge团簇的吸附中心总是在三个增原子所围成的区域中.它们的电子结构具有类似半导体的性质,即其局域态密度在远离费米面的能级处很大,而在费米面附近的能级处非常小. 关键词： 扫描隧道显微镜 Si(111)7×7表面 Ge团簇     

Fluorescence confocal polarizing microscopy: Three-dimensional imaging of the director

Much of the modern understanding of orientational order in liquid crystals (LCs) is based on polarizing microscopy (PM). A PM image bears only two-dimensional (2D) information, integrating the 3D pattern of optical birefringence over the path of light. Recently, we proposed a technique to image 3D director patterns by fluorescence confocal polarizing microscopy (FCPM). The technique employs the property of LC to orient the fluorescent dye molecules of anisometric shape, added in small quantities to the LC. In LC, smooth director deformations do not alter mass density of the material. Thus the density of dye is also uniform across the sample, except, perhaps, near the surfaces or at the cores of topological defects. In polarized light, the measured fluorescence signal is determined by the spatial orientation of the molecules rather than by dye concentration (as in regular biological samples stained with tissue-specific dyes). The contrast is enhanced when both excitation and detection of fluorescence light are performed in polarized light. This short review describes the essence of FCPM technique and illustrates some of its applications, including imaging of Frederiks electric-field induced effect in a nematic LC and defects such as dislocations in cholesteric LCs.     

Morphology and electronic structure of bcc Co(1 1 0) and fcc/hcp Co(1 1 1) on Fe(1 1 0) investigated by STM and STS

We report on the growth of ultrathin epitaxial Co films on Fe(1 1 0) examined by scanning tunneling microscopy and spectroscopy (STM and STS). At room temperature Co forms pseudomorphic, ideally ordered body-centered cubic (bcc) layers for the first two monolayers as confirmed by atomically resolved STM images. This is in contrast to the related case of Co/Cr(1 1 0) where a superstructure occurs in the second layer. The third monolayer forms a close-packed structure and causes a transformation of the buried second monolayer into a close-packed structure. The Fe(1 1 0) substrate strongly influences the electronic structure of the first Co monolayer as concluded from the dI/dU spectra. This influence is less important for the second monolayer. The measured local density-of-states function for the bcc Co double layer is in agreement with theoretical predictions for bcc Co.     

Coexisting electron emission mechanisms in small metal particles observed in fs-laser excited PEEM

Silver cluster films deposited on Si(1 1 1) were investigated by spectroscopic photoelectron microscopy using fs-laser excitation tuneable between hν = 1.45-1.65 eV and 2.9-3.3 eV. With increasing coverage the films grown as stepped wedges first exhibit clusters of few nanometers diameter with narrow size distributions that later agglomerate forming larger islands up to about 100 nm diameter. The cluster films have been characterized by SEM, AFM and HR-TEM. In the 3.1 eV range the small clusters emit more effectively and the dependence of electron yield on laser power follows a quadratic power law. Microspectroscopy reveals that the Fermi level onset is sharp(<150 meV width) and shifts by 2hν when the quantum energy is increased, thus confirming the predominance of two-photon-photoemission (2PPE). Under 1.6 eV excitation the situation is different: The power dependence is non-integer and the slope varies between 2.9 and 3.7 for different points on the sample. The Fermi edge appears smeared out and shifted by several hundred meV to lower final state energies. We attribute this deviation from pure 3PPE to thermally assisted nPPE of electrons from a transient “hot electron” gas in the nanoparticles.     

Heavy ion induced damage in MgAl2O4, an inert matrix candidate for the transmutation of minor actinides

Magnesium aluminum spinel (MgAl₂O₄) is a material selected as a possible matrix for transmutation of minor actinides by neutron capture or fission in nuclear reactors. To study the radiation stability of this inert matrix, especially against fission product impact, irradiations with heavy energetic ions or clusters have been performed. The high electronic energy losses of the heavy ions in this material led to the formation of visible tracks as evidenced by transmission electron microscopy for 30 MeV C₆₀-Buckminster fullerenes and for ions of energy close to or higher than fission energy (²⁰⁹Bi with 120 MeV and 2.38 GeV energy). The irradiations at high energies showed a pronounced degradation of the spinel. Additionally, MgAl₂O₄ exhibited a large swelling for irradiation at high fluences with fission products of fission energy (here I-ions of 72 MeV) and at temperatures ≤ 500 °C. These observations are discussed from the technological point of view in the frame of using MgAl₂O₄ as an inert matrix for the transmutation of minor actinides.     

Growth of Co nanoparticles on a nanostructured θ-Al2O3 film on CoAl(1 0 0)

We have investigated the growth of Co nanoparticles on θ-Al₂O₃/CoAl(1 0 0) by means of Auger electron spectroscopy (AES), high-resolution electron energy loss spectroscopy (EELS), low energy electron diffraction (LEED) and scanning tunneling microscopy (STM). Due to Volmer-Weber growth, Co forms particles with a mean diameter of approximately 2.5 nm and height of 0.8 nm. Even on the entirely covered oxide, there is no Ostwald ripening and Co particles stay structurally isolated. The nanoparticles exhibit a small size distribution and tend to form chains, as predetermined by the streak structure of the oxide template. For sufficient high coverages Co-core-CoO-shell nanoparticles may be evidenced, which is explained as a result of surfactant oxygen. The nanostructured particles may open the door to numerous applications, such as in catalysis and magnetoelectronic applications, where large areas of ordered nanodots are desired.     

Interpretation of initial stage of 3C-SiC growth on Si(1 0 0) using dimethylsilane

The initial stage of cubic silicon carbide (3C-SiC) growth on a Si(0 0 1) surface using dimethylsilane (DMS) as a source gas was observed using scanning tunneling microscopy (STM) and reflection high-energy electron diffraction (RHEED). It was found that the dimer vacancies initially existing on the Si(0 0 1)-(2 × 1) surface were repaired by the Si atoms in DMS molecules, during the formation of the c(4 × 4) surface. From the STM measurement, nucleation of SiC was found to start when the Si surface was covered with the c(4 × 4) structure but before the appearance of SiC spots in the RHEED pattern. The growth mechanism of SiC islands was also discussed based on the results of RHEED, STM and temperature-programmed desorption (TPD).     

Systematic studies of tunneling magnetoresistance in granular films made from well-defined Co clusters

The tunneling magnetoresistance (TMR) of granular films prepared by the co-deposition of well-defined ferromagnetic Co clusters and insulating inert-gas matrix atoms has been studied as function of matrix atoms (Kr, Xe), cluster volume fraction, temperature (4–40 K) and cluster size (4.2–5.2 nm). Tunneling samples with resistivities that differ by about five orders of magnitude have a TMR that is found to be independent of matrix and cluster volume fraction, i.e. is independent of both tunneling barrier height and width. All samples show a characteristic TMR(T)-dependence that can be explained by a model which takes into account that magnetic moments at the cluster surface are becoming misaligned with increasing temperature. The fraction of misaligned moments at a fixed temperature is increasing with decreasing clusters size.     

Reactively sputtered Ni, Ni(N) and Ni3N films: Structural, electrical and magnetic properties

Nickel thin films were deposited on glass substrates at different N₂ gas contents using a dc triode sputtering deposition system. Triode configuration was used to deposit nanostructured thin films with preferred orientation at lower gas pressure and at lower substrate temperature compared to the dc diode sputtering system. A gradual evolution in the composition of the films from Ni, Ni(N), to Ni₃N was found by X-ray diffraction analysis. The preferred growth orientation of the nanostructured Ni films changed from (1 1 1) to (1 0 0) for 9% N₂ at 100 °C. Ni₃N films were formed at 23% N₂ with a particle size of about 65 nm, while for 0% and 9% of nitrogen, the particles sizes were 60 nm, and 37 nm, respectively, as obtained by atomic force microscopy. Magnetic force microscopy imaging showed that the local magnetic structure changed from disordered stripe domains of about 200 nm for Ni and Ni(N) to a structure without a magnetic contrast, indicating the paramagnetic state of this material, which confirmed the structural transformation from Ni to Ni₃N.     

Three-dimensional growth characteristics of antimony aggregates on graphite

The growth of antimony aggregates on the basal plane of graphite via diffusion and aggregation of Sb₄ clusters has been investigated with scanning electron microscopy, and in 3-dimensions with atomic force microscopy. The aggregate morphologies depend critically on the deposition conditions. It is shown that a transition from compact to branched morphologies with increasing aggregate size, depends on the particle flux. Also, the aggregate heights are strongly influenced by flux, with higher fluxes producing flatter aggregates. The heights of individual island branches are also shown to depend on the local diffusion field.     

Transmission electron microscopy and X-ray diffraction study of microstructural evolution in magnetoresistive Cu–Fe–Ni ribbons

The evolution of the microstructure of a granular Cu₈₀Fe₁₀Ni₁₀ (at%) melt-spun ribbon is studied by transmission electron microscopy (TEM), energy-filtered transmission electron microscopy (EFTEM) and X-ray diffraction. This system is interesting as large giant magnetoresistance (GMR) values have been measured for this composition. We have shown the presence of two face-centred cubic phases, an (Fe,Ni)-rich phase and a Cu-rich phase. The lattice parameters of these two phases are close and no diffraction or elastic contrast is involved in displaying the two phases in TEM bright-field mode. With EFTEM imaging, we have shown the presence of a fine-scale (Fe,Ni)-rich precipitation inside the Cu-rich fcc matrix. The precipitates are 2–4 nm in the as-spun state and 4–6 nm after annealing for 2 h at 400°C. The lattice parameter of the Cu-rich phase in the as-spun sample is 0.3608 nm and 0.3610 nm for the (Fe,Ni)-rich phase. After a 24-h annealing treatment at 600°C, the mean diameter of the particle is 20 nm and the lattice parameter of the (Fe,Ni)-rich phase has decreased to 0.3600 nm, while that of the Cu-rich phase has increased to 0.3613 nm, which is consistent with a segregation of Fe and Ni in the precipitates. The composition and volume fraction of the two phases measured for this annealed sample are in good agreement with the Thermocalc® predictions.