An experimental setup for high resolution 10.5 eV laser-based angle-resolved photoelectron spectroscopy using a time-of-flight electron analyzer

We present an experimental setup for laser-based angle-resolved time-of-flight photoemission. Using a picosecond pulsed laser, photons of energy 10.5 eV are generated through higher harmonic generation in xenon. The high repetition rate of the light source, variable between 0.2 and 8 MHz, enables high photoelectron count rates and short acquisition times. By using a time-of-flight analyzer with angle-resolving capabilities, electrons emitted from the sample within a circular cone of up to ±15° can be collected. Hence, simultaneous acquisition of photoemission data for a complete area of the Brillouin zone is possible. The current photon energy enables bulk sensitive measurements, high angular resolution, and the resulting covered momentum space is large enough to enclose the entire Brillouin zone in cuprate high-T(c) superconductors. Fermi edge measurements on polycrystalline Au shows an energy resolution better than 5 meV. Data from a test measurement of the Au(111) surface state are presented along with measurements of the Fermi surface of the high-T(c) superconductor Bi(2)Sr(2)CaCu(2)O(8 + δ) (Bi2212).     

Sialolith characterization by scanning electron microscopy and X-ray photoelectron spectroscopy

The objective of this study has been to characterize sialolith, a calcium phosphate deposit that develops in the human oral cavity, by high-resolution field emission scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The morphological and chemical data obtained helped in the determination of their formation mechanism in salivary glands. Sialoliths in the submandibular salivary glands may arise secondary to sialodenitis, but not via a luminal organic nidus. We believe this is the first study that characterizes a sialolith by XPS.     

Note: binding energy scale calibration of electron spectrometers for photoelectron spectroscopy using a single sample

The feasibility of calibrating the binding energy scale for photoelectron spectroscopy using a single sample without sputter cleaning was investigated. By measuring the Fermi level of a Au film with both monochromatic Al Kα (hν = 1486.7 eV) and He Iα (hν = 21.22 eV), the binding energy scale was simply and accurately calibrated. This method is found to yield binding energy values for the Cu 2p(3/2), Ag 3d(5/2), and Au 4f(7/2) peaks that agree with the standard tabulated values defined in International Organization for Standardization 15472 to within ±0.02 eV.     

Estimates of the maximum likelihood of parameters of weak optical signals during photodetecting by means of recording photoelectron emission moments

A likelihood function is obtained for estimating parameters of weak optical signals during detecting by means of recording emission moments of each photoelectron. Likelihood equations are derived and solved by an example of optimal estimates of a Gaussian pulse. Expressions for compatible and incompatible estimates of all three unknown parameters of the pulse are obtained. Analytical expressions for the Kramer-Rao bounds determining the quality of the estimates obtained are also derived. The variances of compatible estimates of the signal amplitude are demonstrated to be three times those of incompatible estimates, while the variances of the estimates of all parameters are inversely proportional to the product of the signal amplitude and its duration.     

Development of a new photoelectron spectroscopy instrument combining an electrospray ion source and photoelectron imaging

A new apparatus has been constructed that combines electrospray ionization with a quadrupole mass filter, hexapole ion trap, and velocity-map imaging. The purpose is to record photoelectron images of isolated chromophore anions. To demonstrate the capability of our instrument we have recorded the photodetachment spectra of isolated deprotonated phenol and indole anions. To our knowledge, this is the first time that the photodetachment energy of the deprotonated indole anion has been recorded.     

The transfer of polytetrafluoroethylene studied by x-ray photoelectron spectroscopy

A polytetrafluoroethylene (PTFE) sphere of radius 4.8 mm was rubbed against nickel and S-Monel at speeds from 0.94 to 94 mm s^?1 and at loads from 0.19 to 3.9 N. The transfer film of PTFE on the metal was examined with X-ray photoelectron spectroscopy. In all cases the film was found to be indistinguishable from bulk PTFE. A trace of metal fluoride was observed whether the rubbing took place on oxidized or atomically clean metal. The film was of the order of a molecule thick for the entire range of loads and did not increase with repeated passes over the same rubbed area. An erratic increase in thickness at rubbing speeds above 10 mm s^?1 was taken as evidence of random transfer of bulk material.     

紫外分光光度法测抗辐康中的红景天甙

抗辐康主要是由红景天和碳酸钙等成分组成,用于抗辐射、疲劳等。本文建立了紫外分光光度测定红景天甙的含量。红景天甙的最大吸收峰在290nm处。红景天甙的线性范围在20～60μg/mL,相关系数为0.9999。平均回收率为95.68％。本法测定抗辐康中的红景天甙需要提取和分离,结果可靠,可用于抗辐康中红景天甙的含量测定。     

The impact of surface and retardation losses on valence electron energy-loss spectroscopy

The inelastic scattering of fast electrons transmitting thin foils of silicon (Si), silicon nitride (Si(3)N(4)), gallium arsenide (GaAs), gallium nitride (GaN) and cadmium selenide (CdSe) was analyzed using dielectric theory. In particular, the impact of surface and bulk retardation losses on valence electron energy-loss spectroscopy (VEELS) was studied as a function of the foil thickness. It is shown that for the materials analyzed, surface and retardation losses can cause a systematic, thickness-dependent modulation of the dielectric volume losses, which can hamper the determination of the bulk dielectric data as well as the identification of band-gap and interband transition energies by VEELS. For Si and GaAs, where the dielectric function is strongly peaked with high absolute values, retardation losses lead to additional intensity maxima in the spectrum. For thin films of these materials (below approximately 100 nm), the additional intensity maxima are related to retardation effects due to the finite size of the sample leading to the excitation of guided light modes. For thicker films, exceeding about 200 nm, the intensity maxima are caused by bulk retardation losses, i.e., Cerenkov losses. Although thickness-dependent modulations were observed for Si(3)N(4), GaN and CdSe, the form of the dielectric functions and their lower maxima, means that for TEM samples < 100 nm thick, the band-gap energies of these materials can be accurately identified by VEELS. Guidelines are given that allow for forecasting the impact of surface and retardation losses on VEELS.     

Determination of oxygen in acid-treated high-purity niobium by X-ray photoelectron spectroscopy

High-purity niobium was immersed in nitric acid and hydrofluoric acid for two minutes and the resulting product was characterized. Scanning electron microscopy was employed to characterize the morphology of the acid treated product. Inert gas fusion was used for determination of oxygen in the high-purity niobium. X-ray photoelectron spectroscopy was employed to characterize the surface ratio of oxygen to niobium. The oxygen concentration was 30 ppm in the acid-treated material and 70 ppm in the untreated material. X-ray photoelectron spectroscopy was employed to characterize the reduction of oxygen at the surface. The ratio of oxygen to niobium decreased from 9.75 to 2.60 without treatment compared to acid treatment for two minutes. The concentrations of adsorbed water and niobium oxide decreased following etching. The acid-treated high-purity niobium was characterized by argon ion bombardment; adsorbed water molecules and niobium oxides were not present but non-lattice oxygen was observed.     

Assessment of electron irradiation damage to biomolecules by electron diffraction and electron energy-loss spectroscopy

Electron radiation damage is one of the most severe problems in high resolution electron microscopy of biomolecules. The techniques of electron diffraction and electron energy-loss spectroscopy were applied to gain a better understanding of radiation damage in amino acids and nucleic acid bases. The results when compared with G-values for the release of ammonia and hydrogen sulphide from amino acids seem to indicate that bond scission is an important cause of radiation damage at moderate doses of irradiation. High resolution structural disorder in nucleic acid bases was found to involve loss of atoms peripheral to the main ring structure.     

Analysis of ceramic materials by electron spectroscopy

The basic principles of X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy are described and their relative advantages as analysis methods for ceramic materials are reviewed. Their application in ceramics technology is illustrated by examples taken from the fields of catalysis and mineralogy. In particular, attention is drawn to recent developments of XPS which make it especially attractive for the study of ceramic materials. These include quantitative application of the X-ray photoelectron diffraction effect to layered, single crystal minerals; the development of higher energy X-ray sources for XPS, and the attendant study of the Sils–KLL Auger parameter as a probe of molecular and crystalline structure; and the analysis of small (?250 μm) surface features by XPS.     

Remote focusing in confocal microscopy by means of a modified Alvarez lens

Alvarez lenses are actuated lens‐pairs which allow one to tune the optical power by mechanical displacement of subelements. Here, we show that a recently realized modified Alvarez lens design which does not require mechanical actuation can be integrated into a confocal microscope. Instead of mechanically moving them, the sublenses are imaged onto each other in a 4f‐configuration, where the lateral image shift leading to a change in optical power is created by a galvo‐mirror. The avoidance of mechanical lens shifts leads to a large speed gain for axial (and hence also 3D) image scans compared to classical Alvarez lenses. We demonstrate that the suggested operation principle is compatible with confocal microscopy. In order to optimize the system, we have drawn advantage of the flexibility a liquid‐crystal spatial light modulator offers for the implementation. For given specifications, dedicated diffractive optical elements or freeform elements can be used in combination with resonant galvo‐scanners or acousto‐optic beam deflectors, to achieve even faster z‐scans than reported here, reaching video rate.     

Anisotropic oxidation of MoS2 crystallites studied by angle-resolved X-ray photoelectron spectroscopy

The oxidation behavior of the solid lubricant MoS₂ was studied using X-ray photoelectron spectroscopy. MoS₂-containing slip ring brushes were used to take advantage of anisotropic orientation of the plate-shaped MoS₂ crystallites occurring during fabrication of the brushes. Because oxidation occurs preferentially at the edges of the crystallites, greater oxidation fractions are measured when the edges are oriented toward the photoelectron energy analyzer. These results indicate a novel method for separately probing the chemistry on the edge and (lubricious) basal surfaces of MoS₂.     

Measurement of local thickness by electron energy-loss spectroscopy

We review various methods which can be used to derive the thickness of an electron-microscope specimen from its transmission energy-loss spectrum. We have applied a sum-rule technique to various kinds of specimen, using a variety of electron-optical conditions, and estimate its accuracy to be typically ±10% (or±2nm if larger) over the thickness range 10–150 nm. This method requires no knowledge of the physical or chemical properties of the specimen other than its refractive index (∞ for metal). It involves only a low radiation dose, allowing good lateral resolution (<10 nm) to be achieved even by selected-area techniques.     

Measurement of radiation damage by electron energy-loss spectroscopy

Inner shell ionization edges in the energy-loss spectrum were used to measure the loss of gaseous elements from thin samples of nitrocellulose, polyvinyl formal, copper phthalocyanine, graphite bisulphate and sodium chloride during exposure to 80 keV electrons. The irradiation kinetics were measured for electron doses up to 10⁴ C m^?2 and for dose rates up to 10 mA m^?2. The energy-loss technique is discussed in relation to other methods for assessing radiation damage.     

RLVIP技术制备Ge1-xCx薄膜的X射线光电子能谱

应用低压反应离子镀(RLVIP)技术在Ge基底上沉积了Get1-xCx薄膜.制备过程中,低压等离子源作为辅助等离子源,Ge作为蒸发材料,CH4作为反应气体,在相同的沉积条件下以不同的沉积速率制备了C含量(x)从0.23到0.78的Ge1-xCx薄膜.X射线衍射测试表明制备的Ge1-xCx薄膜为无定形结构.用X射线光电子能谱研究了不同C含量下Ce1-xCx薄膜中C的化学键合变化.研究结果表明;当x>0.78时,成键为C-H键;当x为0.53～0.62时,成键为C-C键;当x<0.47时,成键为Ge-C键.     

Application of transmission electron microscopes to nanometre-sized fabrication by means of electron beam-induced deposition

Electron beam‐induced deposition was carried out using a scanning transmission electron microscope with a field emission gun to fabricate nanometre‐sized structures. A small amount of a metal–organic gas was introduced near the substrate in the microscope chamber, and focused electron beams were irradiated. Two‐ and three‐dimensional structures were fabricated by scanning the beam position. The minimum line width of the freestanding structures was 8 nm at a constant gas flux used. This line width of 8 nm is considered to be achieved by employing a high accelerating voltage, which leads to a small probe size, and the optimum scanning speed.     

Demonstration of lanthanum in liver cells by energy-dispersive X-ray spectroscopy, electron energy loss spectroscopy and high-resolution transmission electron microscopy

The appearance of lanthanum in liver cells as a result of the injection of lanthanum chloride into rats is investigated by advanced transmission electron microscopy techniques, including electron energy loss spectroscopy and high‐resolution transmission electron microscopy. It is demonstrated that the lysosomes contain large amounts of lanthanum appearing in a granular form with particle dimensions between 5 and 25 nm, whereas no lanthanum could be detected in other surrounding cellular components.     

Determination of the electron density in plasma by means of a floating double probe

Investigations are performed in a microwave plasma expansion containing argon-nitrogen gas mixture. The purpose of this work is to measure accurate electron density values by means of a floating double probe. We check the accuracy of the different methods developed for the double probe under different experimental conditions in Ar-N2 gas mixture, comparing results to single probe measurements. On the basis of previous works, we propose a simple way to determine the electron density without the knowledge of the plasma potential.     

A flexible apparatus for attosecond photoelectron spectroscopy of solids and surfaces

We describe an apparatus for attosecond photoelectron spectroscopy of solids and surfaces, which combines the generation of isolated attosecond extreme-ultraviolet (XUV) laser pulses by high harmonic generation in gases with time-resolved photoelectron detection and surface science techniques in an ultrahigh vacuum environment. This versatile setup provides isolated attosecond pulses with photon energies of up to 140 eV and few-cycle near infrared pulses for studying ultrafast electron dynamics in a large variety of surfaces and interfaces. The samples can be prepared and characterized on an atomic scale in a dedicated flexible surface science end station. The extensive possibilities offered by this apparatus are demonstrated by applying attosecond XUV pulses with a central photon energy of ～125 eV in an attosecond streaking experiment of a xenon multilayer grown on a Re(0001) substrate.