Formative ceramics from the Andes and their production: A Mössbauer study

The potential of Mössbauer spectroscopy in the reconstruction of production techniques of early ceramics is demonstrated by the results of a study of a Formative kiln site at the Archaeological Park at Batán Grande, Perú, and of ceramics from the nearby settlement of Huaca Chólope.     

Chemical Far Infrared Spectroscopy

Abstract

A number of books, symposia, proceedings, special publications [1–9], and review papers in English covering catalytic surfaces [10, 11], solid surface characterization [12–191, thin film analysis [20–22], surface structure and bonding [23, 24], angular distribution of photoelectrons [25, 26], use of synchrotron radiation [27, 281, ion beam effects [29], different methods of surface study [30, 31], experimental and theoretical aspects of ultraviolet photoelectron spectroscopy (UPS) [32], and angle resolved UPS [33, 34] are available in literature. Reviews in other languages, namely Japanese [35–41], German [42–46], French [47–50], Italian [51], Russian [52], and Polish [53], are also available. But the present situation demands a thorough and up-to-date literature survey of the surface study by photoelectron spectroscopy in order to assess what has been done and what is left to be done. This paper is aimed at that goal.     

China rose petal as biotemplate to produce two-dimensional ceria nanosheets

China rose petal was used as robust biotemplate for the facile fabrication of novel ceria nanosheet with a thickness of about 7 nm via a continuous infiltration process. The presence of well-resolved peaks ([111], [200], [220], and [311]) for the products revealed the formation of the fluorite-structured CeO₂. The detailed characterization by field-emission scanning electron microscope (FESEM), field-emission transmission electron microscope (FETEM), and atomic force microscopy (AFM) exhibited the biomorphic structure of polycrystalline ceria film with the nanoparticle size of ca. 6.98 nm. Based on the surface chemistry and biochemistry processes, a possible mechanism for the formation of CeO₂ nanosheets is proposed. Furthermore, nitrogen adsorption–desorption measurement and photoluminescence spectrum (PL) were employed to characterize the samples. The ceria nanosheet showed the existence of mesopores (pores 2–4 nm diameter) on its surface and a broad emission ranging from 350 to 500 nm in photoluminescence spectrum. X-ray photoelectron spectroscopy analysis (XPS) confirmed that the mesoporous nanosheets possessed more surface vacancies than the bulk CeO₂; hence these hierarchical CeO₂ layers appear to be potential candidates for catalytic applications.     

On PbS nanoparticles formed in the compartments of water/AOT/n-heptane microemulsion

Colloidal nanodispersion of lead sulfide has been prepared in the aqueous compartments of water/AOT/n-heptane. Compartmentalization has prevented growth and coagulation of particles in the dispersion. The uv–vis and fluorescence spectral measurements of the colloidal PbS dispersion were taken. Particle size has been determined by laser light scattering, transmission electron microscopy and absorption spectroscopy. The effects of temperature, ω (water/AOT mole ratio), [AOT], and [PbS] on the particle size have been examined. The nanodispersed particles in microemulsion capped with thiophenol and dodecanethiol were isolated and characterized by the TEM and FTIR methods.     

On PbS nanoparticles formed in the compartments of water/AOT/n-heptane microemulsion

Colloidal nanodispersion of lead sulfide has been prepared in the aqueous compartments of water/AOT/n-heptane. Compartmentalization has prevented growth and coagulation of particles in the dispersion. The uv–vis and fluorescence spectral measurements of the colloidal PbS dispersion were taken. Particle size has been determined by laser light scattering, transmission electron microscopy and absorption spectroscopy. The effects of temperature, ω (water/AOT mole ratio), [AOT], and [PbS] on the particle size have been examined. The nanodispersed particles in microemulsion capped with thiophenol and dodecanethiol were isolated and characterized by the TEM and FTIR methods.This revised version was published online in August 2005 with a corrected issue number.     

Origin of the low-frequency band in Raman spectra of multi-walled carbon nanotubes synthesized by the CVD method

The origin of the low-frequency band (250–300 cm^?1) in the Raman spectra of multi-walled carbon nanotubes (MWCNTs) produced by the CVD method has been studied. The studies performed by Raman spectroscopy, transmission electron microscopy, Auger spectroscopy, and X-ray photoelectron spectroscopy after chemical and thermal treatments allow the assumption that this band belongs to radial vibrations of carbon atoms in internal walls of MWCNTs.     

Band Assignment in Ultraviolet Photoelectron Spectroscopy

A review of photoelectron spectroscopy, [1], a book containing a great number of experimental results [2], and the proceedings of an international conference [3] have appeared recently.     

Application of lasers in precision analytical measurements (review)

Conclusions The foregoing analysis does not exhaust the analytic methods of laser spectroscopy (see, e.g., [6–8, 142, 143]). The methods of traditional [8–10, 144, 145] resonance [8, 146], and active (or CARS) [8, 11, 147] Raman scattering spectroscopy are continuously being expanded. Newer, purely laser methods — optogalvanic spectroscopy [25, 148], optothermal spectroscopy [7, 149], the method of selective photoionization [6, 150], etc. — are also being developed.Further development of laser spectra analysis will primarily require going beyond narrow laboratory, purely research setups, and the development of commercial laser analytic devices. In this connection, in selecting a method as the basis for the device being constructed it is necessary to know not only the technical characteristics, such as sensitivity, selectivity, speed of operation, etc., but also the metrological characteristics, such as the random and systematic measurement errors; in addition, the measurement accuracy is a decisive factor. At the same time there are few works devoted to the questions of accuracy of the measurements performed with laser spectrometers; in the literature available to us there are no reviews and comparisons of analytic methods of laser spectroscopy from this viewpoint.Amongst the foregoing methods the direct absorption method has the highest accuracy. With a definite arrangement of the measurement process this method enables absolute measurements of the concentration of the analyte component, i.e., it does not require precalibration of the apparatus based on gas mixtures (for the gas analyzer). The minimum achievable error of such measurements is limited by the error of the premeasured absorption coefficient for radiation of the molecule being detected at the wavelength of the laser radiation and at the present time can equal 1–3%. Other methods studied are characterized by higher sensitivity, and they are also more accurate, difficult to calibrate, and less versatile. A comparative analysis of the methods and their errors will be performed in the future.Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 48, No. 1, pp. 7–26, January, 1988.We thank A. P. Voitovich for useful remarks and a discussion of this work.     

Coordination-dependent valence state of Sm adsorbed on Cu(1 0 0) and (1 1 0) studied by STM and XPS

Geometric and electronic structures of Sm adlayers on Cu(1 0 0) and (1 1 0) were studied by scanning tunneling microscopy (STM) and X-ray photoelectron spectroscopy (XPS). The present results, in addition to the previous results for Sm/Cu(1 1 1) [Y. Nakayama, H. Kondoh, T. Ohta, Surf. Sci. 552 (2004) 53], indicate that the valence state of Sm adsorbed on Cu surfaces is determined by Sm-Sm and Sm-Cu coordination numbers. We propose that the valence state of the adsorbed Sm atoms can be explained by a simple thermodynamic equation including the coordination numbers.     

光谱法测试瓜环与2-氨基苯丙噻唑的主客体作用

利用1H NMR技术,紫外吸收光谱法和荧光光谱法考察了七、八元瓜环(cucurbit[n]urilsn=7,8)与2-氨基苯并噻唑(g)的相互作用。实验结果表明:在2pH9范围内,利用不同的光谱方法均能观察到瓜环与客体的相互作用;Q[7]与客体作用形成物质的量比为1∶1的包结配合物,Q[8]与客体形成物质的量比为1∶2的包结配合物,并计算出包结常数,同时测试了超分子体系的热力学稳定性及熵变,焓变。     

Deposition of iron pyrite via pulsed electron ablation

Pulsed electron beam ablation is a relatively novel deposition technique with some unique advantages, such as ease for scale-up and low operating cost. In this work, we report on the preparation of iron pyrite (FeS₂) on 1.5-cm² glass substrates through the pulsed electron beam ablation of a single synthetic target. The 40–120-nm-thin films were deposited at a substrate temperature ranging from room temperature to 250 ^°C and under a background argon atmosphere of 3.5 mTorr. Different characterization techniques have been used to analyze the deposited films, such as grazing-angle x-ray diffraction (XRD), X-ray photon spectroscopy (XPS), visible Raman spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), and visible optical reflectance spectroscopy. The findings show that iron pyrite can be obtained at high temperature in association with other phases.     

Discovery of novel iron clusters in proteins by Mössbauer spectroscopy

Iron clusters are the catalytically active groups of many proteins. The basis building blocks of these clusters are few; they are all variants of three archetypal patterns: [Fe–O–Fe], [2Fe–2S], and [4Fe–4S]. Mössbauer spectroscopy, in conjunction with EPR spectroscopy, susceptometry and EXAFS, plays an important role in characterizing type, number, oxidation states and magnetic properties of such clusters in newly discovered proteins, and in detecting how valency and magnetism vary by passing through the catalytical cycle of these proteins. In this contribution we present the characterization of a novel iron cluster with unusual bridging and terminal ligands and metal coordinations.     

Influence of Shearing on Crystallization Behavior of Polyoxymethylene/Poly(Ethylene Oxide) Crystalline/Crystalline Blends

The effect of shearing on crystallization behavior of a crystalline/crystalline blend, polyoxymethylene [POM]/poly(ethylene oxide) [PEO], was investigated using polarized light microscopy connected with a CSS450 shearing hot-stage, scanning electron microscopy, differential scanning calorimetry [DSC], and x-ray diffraction [XRD]. The experimental results indicated that the shearing made POM and PEO disperse more evenly and increased the inclusion and entanglement effects between the molecular chains of POM and PEO and therefore enhanced the influence of PEO on the crystallization of POM. As a result, the blend sheared at a shear rate of 20 s^?1 for 10 min at 160°C formed shish–kebab crystals and produced more interlamellar structures compared with the formation of perforated spherulites in the unsheared blend. Moreover, a more obvious shoulder melting peak of POM appeared in the DSC heating trace and a new diffraction peak occurred at 2θ = 31.7° in the XRD pattern for the sheared POM/PEO [50/50] blend.     

Effects of gas pressure on the synthesis and photoluminescence properties of Si nanowires in VHF-PECVD method

Silicon nanowires (SiNWs) were grown on an Au-coated Si(111) substrate at various gas pressures by very high frequency plasma enhanced chemical vapor deposition via the vapor–liquid–solid mechanism. The synthesized SiNWs were characterized by field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, high-resolution transmission electron microscopy, Raman spectroscopy and photoluminescence (PL). The SiNWs were sharp needle-shaped and possessed highly crystalline core and oxide amorphous shell. As the gas pressure increases from 70 mtorr to 85 mtorr, the average diameter of the SiNWs decreases from 250 nm to 70 nm. Furthermore, the density of the nanowires increases with the gas pressure. The PL spectra revealed a peak at about 400 nm and a broadband emission at about 700 nm.     

Calibrating Multichannel Raman Spectrometers

Abstract

Although multichannel Raman spectroscopy has a history of more than a decade [I], it was only recently that the real potential of this technique became fully appreciated. The use of advanced optical multichannel detectors (OMDs) is now bringing about a substantial change in Raman spectroscopy. For example, the application of this technique to short-lived transient species has established a new frontier of Raman spectroscopy known as transient and time-resolved Raman spectroscopy [2]. The technique has made it possible to measure the spectrum even from an extremely weak scatterer like a monolayer film deposited on a substrate [3, 41. A recent experiment on an intact mouse lens [5] demonstrated that only 1 mW laser power with 1 s exposure time is enough to obtain a good quality Raman spectrum of the lens protein, which is of clinical importance for the prevention of cataract formation. A number of stimulating reports are also notable in a variety of fields including chemistry, physics, biology, medicine, and engineering. The advantages of multichannel Raman spectroscopy are manifold.     

A novel precursor for synthesis of metallic copper nanocrystals by thermal decomposition approach

[Bis(2-hydroxy-1-naphthaldehydato)copper(II)] complex, as a novel precursor, was employed in thermal decomposition process to synthesize metallic copper nanoparticles using oleylamine (C₁₈H₃₇N) as capping agent. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and ultraviolet-visible (UV-vis) spectroscopy. The synthesized copper nanoparticles have a fcc structure with average size 20-35 nm.     

An electron paramagnetic resonance study of the tetragonally distorted [Formula: see text] ion in [Formula: see text] and [Formula: see text

Chromium-doped [Formula: see text] and [Formula: see text] have been studied by both EPR and ENDOR spectroscopy. [Formula: see text] ions enter the fluorite structure in distorted substitution cation sites. In both matrices the distortion observed is tetragonal. X- and Q-band EPR measurements at temperatures between 4 and 300 K allowed us to determine the ion symmetry and the following spin-Hamiltonian parameters: [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text] and [Formula: see text] for [Formula: see text]; and [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text], [Formula: see text] and [Formula: see text] for [Formula: see text]. For [Formula: see text], the weak superhyperfine interaction of [Formula: see text] with the surrounding [Formula: see text] ions has been studied by both EPR and ENDOR techniques for [Formula: see text]. No ENDOR signals were detected for [Formula: see text]. The results are tentatively explained in terms of a Jahn - Teller effect corresponding to [Formula: see text] coupling strongly stabilized by lattice stresses, although other possible origins for the distortion cannot be completely ruled out.     

Wave-function mapping of InAs quantum dots by scanning tunneling spectroscopy

Scanning tunneling spectroscopy is used to investigate the single-electron states and the corresponding squared wave functions of single and freestanding strain-induced InAs quantum dots grown on GaAs(001). Several peaks are found in dI/dV curves, which belong to different single-electron states. Spatially resolved dI/dV images reveal (000), (100), (010), (200), and (300) states, where the numbers describe the number of nodes in [11;0], [110], and [001] directions, respectively. The total number and energetic sequence of states is different for different dots. Interestingly, the (010) state is often missing, even when (200) and (300) states are present. We interpret this anisotropy in electronic structure as a consequence of the shape asymmetry of the dots.     

Tin-doped indium oxide nanobelts grown by carbothermal reduction method

This communication discusses the formation of doped nanobelts produced by a simple route. Tin-doped indium oxide (ITO) nanobelts were obtained by a carbothermal reduction method. The nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) and wavelength-dispersive X-ray spectroscopy (WDX). The results show that the nanobelts have a cubic structure, are single crystalline and doped with tin and grow in the [400] direction. PACS 81.07.-b; 61.46.+w; 68.37.Hk; 68.37.Lp     

Template-free preparation and characterization of nanocrystalline ZnO in aqueous solution of [EMIM][EtSO4] as a low-cost ionic liquid using ultrasonic irradiation and photocatalytic activity

A fast, template-free, and environmentally benign green route for the preparation of nanocrystalline ZnO in aqueous solution of 1-ethyl-3-methylimidazolium ethyl sulfate, [EMIM][EtSO₄], room-temperature ionic liquid (RTIL), via ultrasonic irradiation is proposed. The X-ray diffraction (XRD) studies display that the products are excellently crystallized in the form of wurtzite hexagonal. Energy-dispersive X-ray spectroscopy (EDX) investigations reveal the products are extremely pure. The morphology of as-prepared nanocrystalline ZnO was characterized by scanning electron microscopy (SEM). Diffuse reflectance spectra (DRS) of the products with absorption maxima at 359 nm show blue shift relative to the bulk ZnO with absorption at 384 nm that can be attributed to quantum confinement effect of nanocrystalline ZnO. A possible formation mechanism of the nanocrystalline ZnO using ultrasonic irradiation in aqueous solution of the RTIL is presented. The results demonstrate that photocatalytic activity of the nanocrystalline ZnO prepared in the presence of the RTIL is higher than the prepared sample in water.