Channeling‐enhanced EDX for polarity resolved crystal orientation determination

Using channeling‐enhanced energy‐dispersive X‐ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non‐centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling‐enhanced, angle‐dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non‐centrosymmetric point group. The method shown here overcomes the limitation of a reduced point‐group sensitivity of electron backscatter diffraction patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections.     

Synthesis and optical properties of Ce-doped ZnO hexagonal nanoplatelets

Single crystalline Ce-doped ZnO hexagonal nanoplatelets are successfully synthesized. Zinc acetate, cerium nitrate, potassium hydroxide and poly vinyl alcohol were mixed together and transferred to a 100 mL Teflon-lined stainless steel autoclave kept at 150 °C for 24 h. The obtained precipitant is calcined at 600 °C. The morphology and microstructure were determined by field emission scanning electron microscopy (FE-SEM), X-ray diffraction transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and photoluminescence (PL) spectroscopy. The investigation confirmed that the products were of the wurtzite structure of ZnO. The doped hexagonal nanoplatelets have edge length 25 nm and thickness 11 nm. EDX result showed that the amount of Ce in the product is about 15%. Photoluminescence of these doped hexagonal nanoplatelets exhibits a blue shift and weak ultraviolet (UV) emission peak, compared with pure ZnO, which may be induced by Ce-doping. The growth mechanism of the doped hexagonal nanoplatelets was also discussed.     

The Al nano-crystallization process in amorphous Al85Ni8Y5Co2

The primary nano-crystallization of fcc Al in initially amorphous Al₈₅Ni₈Y₅Co₂ has been studied by differential scanning calorimetry (DSC), transmission electron microscopy (TEM) in combination with energy electron loss spectroscopy (EELS), high-resolution transmission electron microscopy (HRTEM) and X-ray diffractometry (XRD). TEM in combination with EELS after both isochronal and isothermal annealing allowed the determination of the change of the crystalline particle density and particle density/size distribution. The crystallization in Al₈₅Ni₈Y₅Co₂ was found to take place in three sequences. In the first step of the first sequence spherical fcc Al nano-particles develop with a very high particle density. In the second step of the first sequence the more or less spherical Al particles develop protrusions without significant further nucleation of fcc Al particles. In the second sequence nucleation of new fcc Al particles takes place. Comparing the crystallization behavior of Al₈₅Ni₈Y₅Co₂ with that of Al₈₅Ni₅Y₈Co₂ it follows that the yttrium solute level has a strong influence on the nucleation and growth behavior during the fcc Al primary nano-crystallization.     

Extended fine structure analysis using electron beams

Appearance potential spectroscopy has found use primarily as a core level probe of the electronic structure of solid surfaces. The observation of extended fine structure above appearance potential edges, analogous to that observed above X-ray adsorption edges, gives promise that atomic spacings in the surface region may also be determined. Most previous studies of appearance potentials have depended on observing changes in the soft X-ray yield. Poor detection efficiencies and low flourescence yields have limited the usefulness of this approach. Using the secondary electron yield, however, we have recently succeeded in observing fine structure extending more than 400 eV above appearance potential edges. We are currently employing this approach to study the structure of SiO₂ films on Si substrates. Initial attempts at Fourier inversion and problems due to diffraction of the incident electron beam and multiple scattering effects will be discussed.     

Structural,microchemical and superconducting properties of ultrathin NbN films on silicon

Structural, chemical and superconducting properties of thin NbN films used for development of fast and sensitive hot‐electron bolometer (HEB) detectors for wide spectra range are reported. The thin NbN films with a thickness between 4 and 10 nm were deposited on the (001)Si substrates by magnetron sputtering. In order to investigate the film morphology and microchemistry, diffraction‐contrast and high‐resolution transmission electron microscopy (TEM) in combination with scanning TEM and electron energy loss spectroscopy (EELS) were performed. In addition, the zero‐resistance critical temperature of the NbN films was measured and correlated to their thickness. The interrelations between fabrication conditions, crystalline and superconducting properties of the differently thick NbN films are discussed. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

氯化亚铁催化制备硼碳氮纳米管

采用固相反应法,以无定型硼粉为原料,氯化亚铁为催化剂,在无水乙醇和氨气气氛中高温热处理3 h成功制得大量竹节状的三元硼碳氮(BCN)纳米管.利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)以及X射线光电子能谱仪(XPS)等手段对所得纳米管进行了表征.结果显示,纳米管的直径在60~90 nm之间,纳米管由B、C、N三种元素组成,其原子比为9.77∶1∶8.65.纳米管的生长机理属于气-液-固(VLS)机制.同时初步探讨了反应温度对纳米管的影响.     

Surface and interfacial structure of epitaxial SrTiO3 thin films on (0 0 1) Si grown by molecular beam epitaxy

Effects of relaxation of interfacial misfit strain and non-stoichiometry on surface morphology and surface and interfacial structures of epitaxial SrTiO₃ (STO) thin films on (0 0 1) Si during initial growth by molecular beam epitaxy (MBE) were investigated. In situ reflection high-energy electron diffraction (RHEED) in combination with X-ray diffraction (XRD), atomic force microscopy (AFM), X-ray photoelectron spectrometry (XPS) and transmission electron microscopy (TEM) techniques were employed. Relaxation of the interfacial misfit strain between STO and Si as measured by in situ RHEED indicates initial growth is not pseudomorphic, and the interfacial misfit strain is relaxed during and immediately after the first monolayer (ML) deposition. The interfacial strain up to 15 ML results from thermal mismatch strain rather than lattice mismatch strain. Stoichiometry of STO affects not only surface morphology but interfacial structure. We have identified a nanoscale Sr₄Ti₃O₁₀ second phase at the STO/Si interface in a Sr-rich film.     

La,Pr,Nd掺杂对纳米TiO2光催化性能的影响

采用水解共沉淀法制备了稀土元素(La, Pr, Nd)掺杂量为0.5wt;～1.5wt;的TiO2光催化剂样本,并对其进行了XRD、TG-DTA、TEM、BET和UV-Vis表征.结果表明,所制备的TiO2光催化剂是以锐钛矿晶型为主的纳米颗粒,掺杂抑制了TiO2晶型由锐钛矿向金红石的转变,同时减小了晶粒尺寸、增大了比表面积、提高了吸光度,且使TiO2半导体的吸光范围发生了红移.将制得的TiO2光催化剂应用于溶液中草酸的降解反应,用K2MnO4滴定法分析降解效率,发现经掺杂改性后的TiO2样本光催化效率均有提高.其中,以掺杂量为1.0wt;的La掺杂样本具有最高的降解效率,与纯TiO2样本相比对草酸的降解率提高了近45;.     

Tetragonal tungsten oxide nanobelts synthesized by chemical vapor deposition

Tungsten trioxide (WO₃) nanobelts in tetragonal structure were grown on Si substrates by a hot-wall chemical vapor deposition (CVD) method without using catalysts. The products were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, and photoluminescence (PL) spectrum. The width of the nanobelts is in the range of 50–100 nm with width-to-thickness ratios of 5–10 and lengths of up to tens of micrometers. These nanobelts grew along the [0 0 1] direction and can be identified as the tetragonal WO₃ structures. Raman and PL measurements indicate the high quality of the nanobelts. The vapor–solid growth mechanism could be applicable in our experiment.     

SnSxSe2-x单晶纳米片的可控制备与表征

锡二硫族化合物可以通过改变硫和硒的含量来连续调控三元合金材料的带隙、载流子浓度等物理化学性质,在电子和光电子器件应用上具有巨大的潜力。本文采用化学气相沉积(CVD)技术可控地制备了不同元素组分的SnS_xSe_2-x(x=0,0.2,0.5,0.8,1.0,1.2,1.5,1.8,2.0)单晶纳米片。采用扫描电子显微镜(SEM)、原子力显微镜(AFM)、能量色散X射线光谱(EDS)、透射电子显微镜(TEM)以及拉曼光谱等手段对SnS_xSe_2-x纳米片进行了综合表征。结果表明本方法成功实现了元素百分比可调的SnS_xSe_2-x单晶纳米片的可控制备。重点研究了依赖于元素百分比的SnS_xSe_2-x的拉曼特征谱,实验结果与基于密度泛函理论(DFT)的第一性原理计算得到的SnS_xSe_2-x的拉曼仿真谱高度吻合,理论计算结果较好地诠释了实验拉曼光谱发生变化的原因。本研究提供了一种元素百分比可调的三元SnS_xSe_2-x单晶纳米片的可控制备方法,同时对锡二硫族化合物的明确、无损识别提供了方案。     

Structural and optical properties of vapour‐etching based porous silicon

The structural and optical properties of porous silicon (PS) layers prepared by Vapour‐Etching (VE) of moderately and heavily boron‐doped Si substrates are investigated. The VE technique produces rough PS layers that are essentially formed of interconnected cluster‐like structures. Optical investigations indicate that this surface roughness enables the PS layers to be used as antireflection coatings in silicon based devices. These optical characteristics are investigated by optical reflectivity and light scattering. The local chemical state and the microstructure of the PS layers are studied by electron energy loss spectroscopy (EELS) in transmission electron microscopy (TEM), and are correlated to the red photoluminescence (PL). TEM studies point out that the cluster‐like interconnected structures are composed of luminescent nanocrystallites. PL measurements display that both quantum confinement and surface passivation determine the electronic states of the silicon nanocrystallites. The complex dielectric function is calculated from the experimental single‐scattering distribution spectrum using a Kramers Kronig analysis. The first resonance peak in the imaginary part is observed at 2.3 eV; two other broadened features appear at 4.7 and 8.8 eV. The latter is generally related to an interface plasmon resulting from the silicon‐silicon oxide interface. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of amorphous carbon nanotubes using attapulgite as template and furfuryl alcohol as carbon source

Amorphous carbon nanotubes were synthesized by vapor deposition polymerization (VDP) method using attapulgite as template and furfuryl alcohol as carbon source. The morphology and microstructure analysis of the as-prepared samples showed that highly pure amorphous carbon nanotubes were obtained, and determined by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SEAD) and energy dispersive X-ray (EDX) spectrum. The Brunauer–Emmett–Teller (BET) surface area analysis indicated that the specific surface area of the as-prepared amorphous carbon nanotubes reaches up to 503.1 m²/g. A hypothesis about the formation mechanism of the amorphous carbon nanotubes was also proposed accordingly.     

Optimal crystal growth conditions of thin films of Bi2Te3 semiconductors

Crystal growth conditions of Bi₂Te₃ narrow bandgap semiconductors have been studied using molecular beam epitaxy method. It was applied to the growth of Bi₂Te₃ on Bridgman single-crystal substrate Sb₂Te₃. Substrate ingots were taken from the natural cleavage along the (0001) plane. The deposited conditions have been studied as a function of substrate temperature (T_s) and flux ratio (F_R=F(Te)/F(Bi)). The quality of deposited layers was controlled by X-ray diffraction, scanning electron microscope (SEM), secondary ion mass spectroscopy (SIMS) depth profiling and energy-dispersive X-ray (EDX) microanalyser. The sticking coefficients K_s(Te) and K_s(Bi) of the elements that compose Bi₂Te₃ were determined. It was found that the stoichiometry of deposited layers depended on substrate temperature and flux ratio. It was observed that all deposited layers were single-crystal in the orientation of their substrates with a small shift due to the stress in layer.     

Synthesis and morphology of nanosized zeolite L

AFM is a powerful tool for imaging nanoscale surface features; it provides two and three dimensional crystal structure images and other information about actual surface of zeolite crystallites. In this paper, nanosized zeolite L is synthesized in different crystallization times and a study of crystal growth of zeolite L is reported using atomic force microscopy (AFM). X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) techniques are used for characterization of the as synthesized samples. TEM and two‐dimensional AFM images indicate that the zeolite particles are in a nano‐range and they have hexagonal structure. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Use of different rapid mixing devices for controlling the properties of magnetite nanoparticles produced by precipitation

Magnetite nanoparticles were precipitated by the classic Massart's method in a 2.5 L stirred tank reactor where the injection of reagent solutions was effectuated by different micro-mixers (T-tube and Hartridge-Roughton rapid mixing devices). The specific surface area, the average particle size and the particle size distribution were highly influenced by changing operating parameters. Laser Diffraction, BET adsorption, Energy-Dispersive X-ray Spectroscopy (EDX), Raman spectroscopy and Transmission Electron Microscopy (TEM) were used for characterizing magnetite nanoparticles. Especially, Hartridge-Roughton micromixer appears to be the most efficient mixing device for producing magnetite nanoparticles. The average particle size of magnetite nanoparticles prepared by Hartridge-Roughton rapid mixing device was less than 10 nm and the EDX and Raman spectroscopy shows that the particle purity is quite high.     

TEM investigation on the structure of amorphous silicon monoxide

Commercially available powder samples of silicon monoxide have been investigated by methods of transmission electron microscopy: electron scattering, electron energy-loss spectroscopy (EELS) and electron spectroscopic imaging (ESI). Pair distribution functions (PDFs) as well as EEL spectra can be shown to be a composition of the PDF and EEL spectra of elemental silicon and amorphous SiO₂. The distribution of the elements silicon and oxygen calculated from ESI images proof the silicon monoxide to be inhomogeneous, i.e. it consists of amorphous silicon and amorphous SiO₂. The phase separated regions measure ≈3–4 nm. One maximum in the PDF at 2.95 Å does not stem from either a-Si or a-SiO₂, and it is assigned to atomic configurations at the interphase boundary layer between Si and SiO₂. The portion of the interphase domain in the total composite material is estimated to be between 20% and 25%.     

Synthesis and structure of iron zirconium phosphate Fe1/3[Zr2(PO4)3]

Iron zirconium phosphate Fe_1/3 [Zr₂(PO₄)₃] is synthesized by heat treatment of gels with the stoichiometric composition of components. The compound prepared is characterized using electron probe microanalysis, X-ray diffraction, and IR spectroscopy. The crystal structure of the Fe_1/3[Zr₂(PO₄)₃] phosphate is refined in space group P2₁/n by the Rietveld method in the isotropic approximation for atomic displacements of all elements.     

Accurate X-ray diffraction studies of KTiOPO<Subscript>4</Subscript> single crystals doped with niobium

Single crystals of potassium titanyl phosphate doped with 4% of niobium (КТР:4%Nb) and 6% of niobium (KTP:6%Nb) are studied by accurate X-ray diffraction at room temperature. The niobium atoms are localized near the Ti1 and Ti2 atomic positions, and their positions are for the first time refined independent of the titanium atomic positions. Maps of difference electron density in the vicinity of K1 and K2 atomic positions are analyzed. It is found that in the structure of crystal КТР:4%Nb, additional positions of K atoms are located farther from the main positions and from each other than in КТР and KTP:6%Nb crystals. The nonuniform distribution of electron density found in the channels of the КТР:4%Nb structure is responsible for ~20% increase in the signal of second harmonic generation.     

Elektronenmikroskopische Beobachtung von Zonenachsen-Interferenzmustern in verbogenen Molybdänfolien

The paper reports on many beam patterns at 150 and 200 kV observed in saucershaped single crystal molybdenum foils if the incident electron beam is parallel to a low index zone axis. Feasible applications are discussed.     

A novel sonochemical synthesis and nanostructured assembly of polyvinylpyrrolidone-capped CdS colloidal nanoparticles

Nanoparticles of cadmium sulfide (nano-CdS) have been successfully prepared from an aqueous solution of cadmium chloride and sodium sulfide by a novel sonochemical method. Through adding polyvinylpyrrolidone K30 (PVP) as the dispersant, a yellow translucent colloidal solution of cadmium sulfide which was considerably stable within at least one month was obtained. The characterizations of nanoparticles by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope (SEM) and FT-IR spectroscopy showed good properties of small size, high surface area and crystal structure. The size of the prepared nanoparticles was about 3–5 nm according to XRD spectra and TEM images. Poly(diallyldimethylammonium chloride) (PDDA) has been employed to fabricate multilayer films on quartz wafer and indium tin oxide (ITO) electrode in a layer-by-layer manner. Atomic force microscopy (AFM) displayed the dense coverage of the substrate surface by the nanoparticles. UV–vis absorption spectroscopy confirmed the consecutive growth of PDDA/nanoparticles layer pairs. The photoelectrochemical and the electrochemical behaviors of the prepared CdS particle were examined as well.