Development of a low-temperature photoelectron spectroscopy instrument using an electrospray ion source and a cryogenically controlled ion trap

The ability to control ion temperatures is critical for gas phase spectroscopy and has been a challenge in chemical physics. A low-temperature photoelectron spectroscopy instrument has been developed for the investigation of complex anions in the gas phase, including multiply charged anions, solvated species, and biological molecules. The new apparatus consists of an electrospray ionization source, a three dimensional (3D) Paul trap for ion accumulation and cooling, a time-of-flight mass spectrometer, and a magnetic-bottle photoelectron analyzer. A key feature of the new instrument is the capability to cool and tune ion temperatures from 10 to 350 K in the 3D Paul trap, which is attached to the cold head of a closed cycle helium refrigerator. Ion cooling is accomplished in the Paul trap via collisions with a background gas and has been demonstrated by observation of complete elimination of vibrational hot bands in photoelectron spectra of various anions ranging from small molecules to complex species. Further evidence of ion cooling is shown by the observation of H2-physisorbed anions at low temperatures. Cold anions result in better resolved photoelectron spectra due to the elimination of vibrational hot bands and yield more accurate energetic and spectroscopic information. Temperature-dependent studies are made possible for weakly bonded molecular and solvated clusters, allowing thermodynamic information to be obtained.     

Instrument combining x-ray photoelectron spectroscopy and secondary ion mass spectrometry for surface studies

X-ray Photoelectron Spectroscopy (XPS) or (ESCA) and Secondary Ion Mass Spectrometry (SIMS) have been combined in the same ultrahigh vacuum system to facilitate a new approach to studying clean and reacted surfaces. The design philosophy is to connect two satellite vacuum systems via a set of magnetically driven sample transfer devices. The advantages and capabilities of this approach are discussed with respect to its flexibility and its ability to couple to other surface techniques. XPS and static SIMS spectra of an oxidized polycrystalline indium film are presented to exemplify the type of information which can be gleaned from a multitechnique investigation of surfaces. The additional ability to prepare sample surfaces in our system by ion implantation is demonstrated by a positive-ion SIMS analysis of a gold-implanted aluminum foil.     

An instrument for the investigation of actinides with spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy

A new system for spin resolved photoelectron spectroscopy and bremsstrahlung isochromat spectroscopy has been built and commissioned at Lawrence Livermore National Laboratory for the investigation of the electronic structure of the actinides. Actinide materials are very toxic and radioactive and therefore cannot be brought to most general user facilities for spectroscopic studies. The technical details of the new system and preliminary data obtained therein will be presented and discussed.     

A photoelectron velocity map imaging spectrometer for experiments combining synchrotron and laser radiations

A velocity map imaging/ion time-of-flight spectrometer designed specifically for pump-probe experiments combining synchrotron and laser radiations is described. The in-house built delay line detector can be used in two modes: the high spatial resolution mode and the coincidence mode. In the high spatial resolution mode a kinetic energy resolution of 6% has been achieved. The coincidence mode can be used to improve signal-to-noise ratio for the pump-probe experiments either by using a gate to count electrons only when the laser is present or by recording coincidences with the ion formed in the ionization process.     

Development of a versatile multiaperture negative ion source

A 60 kV ion source (9 beamlets of 15 mA each of H(-)) and plasma generators are being developed at Consorzio RFX and INFN-LNL, for their versatility in experimental campaigns and for training. Unlike most experimental sources, the design aimed at continuous operation. Magnetic configuration can achieve a minimum ∣B∣ trap, smoothly merged with the extraction filter. Modular design allows for quick substitution and upgrading of parts such as the extraction and postacceleration grids or the electrodes in contact with plasma. Experiments with a radio frequency plasma generator and Faraday cage inside the plasma are also described.     

Design and evaluation of a new bench-top instrument for laser-induced breakdown spectroscopy

A newly designed and developed bench-top instrument is reported for laser-induced breakdown spectroscopy offering compact size and relatively low cost. A miniature laser was designed in the laboratory with a small volume and a light weight. The spectrometer was controlled using laboratory-written software. The instrument is suitable for the direct and rapid analysis of solid samples after simple pretreatment. Good stability and accuracy were achieved for quantitative analysis. The performance of the instrument was evaluated by qualitative and quantitative analyses of nickel ore for Mn, Al, Fe, Cr, Zn, Mg, Si, and Ca. The quantitative analysis showed linear calibration graphs and small relative standard deviations. The results show that the new instrument is suitable for elemental analysis.     

Femtosecond time-resolved photoelectron spectroscopy with a vacuum-ultraviolet photon source based on laser high-order harmonic generation

A laser-based tabletop approach to femtosecond time-resolved photoelectron spectroscopy with photons in the vacuum-ultraviolet (VUV) energy range is described. The femtosecond VUV pulses are produced by high-order harmonic generation (HHG) of an amplified femtosecond Ti:sapphire laser system. Two generations of the same setup and results from photoelectron spectroscopy in the gas phase are discussed. In both generations, a toroidal grating monochromator was used to select one harmonic in the photon energy range of 20-30 eV. The first generation of the setup was used to perform photoelectron spectroscopy in the gas phase to determine the bandwidth of the source. We find that our HHG source has a bandwidth of 140 ± 40 meV. The second and current generation is optimized for femtosecond pump-probe photoelectron spectroscopy with high flux and a small spot size at the sample of the femtosecond probe pulses. The VUV radiation is focused into the interaction region with a toroidal mirror to a spot smaller than 100 × 100 μm(2) and the flux amounts to 10(10) photons/s at the sample at a repetition rate of 1 kHz. The duration of the monochromatized VUV pulses is determined to be 120 fs resulting in an overall pump-probe time resolution of 135 ± 5 fs. We show how this setup can be used to map the transient valence electronic structure in molecular dissociation.     

Development of a compact filament-discharge multi-cusp H- ion source

A 14 MeV medical cyclotron with the external ion source has been designed and is being constructed at China Institute of Atomic Energy. The H(-) ion will be accelerated by this machine and the proton beam will be extracted by carbon strippers in dual opposite direction. The compact multi-cusp H(-) ion source has been developed for the cyclotron. The 79.5 mm long ion source is 48 mm in diameter, which is consisting of a special shape filament, ten columns of permanent magnets providing a multi-cusp field, and a three-electrode extraction system. So far, the 3 mA∕25 keV H(-) beam with an emittance of 0.3 π mm mrad has been obtained from the ion source. The paper gives the design details and the beam test results. Further experimental study is under way and an extracted beam of 5 mA is expected.     

Advanced light ion source extraction system for a new electron cyclotron resonance ion source geometry at Saclay

One of the main goal of intense light ion injector projects such as IPHI, IFMIF, or SPIRAL2, is to produce high current beams while keeping transverse emittance as low as possible. To prevent emittance growth induced in a dual solenoid low energy transfer line, its length has to be minimized. This can be performed with the advanced light ion source extraction system concept that we are developing: a new ECR 2.45 GHz type ion source based on the use of an additional low energy beam transport (LEBT) short length solenoid close to the extraction aperture to create the resonance in the plasma chamber. The geometry of the source has been considerably modified to allow easy maintenance of each component and to save space in front of the extraction. The source aims to be very flexible and to be able to extract high current ion beams at energy up to 100 kV. A specific experimental setup for this source is under installation on the BETSI test bench, to compare its performances with sources developed up to now in the laboratory, such as SILHI, IFMIF, or SPIRAL2 ECR sources. This original extraction source concept is presented, as well as electromagnetic simulations with OPERA-2D code. Ion beam extraction in space charge compensation regime with AXCEL, and beam dynamics simulation with SOLMAXP codes show the beam quality improvement at the end of the LEBT.     

Generation of an ion beam in a glow-discharge source

A mechanism of ion extraction from a glow-discharge ion source based on a hollow cathode and used for elemental analysis of solids, is considered Experiments have shown that two oppositely directed ion flows are formed from ions produced in the region of negative glow-discharge fluorescence. One flow has an ion energy ≥ 100 eV, is directed to the cathode, and bombards and sputters the analyzed sample. The sputtered atoms diffuse into the negative-glow region and are ionized. The second flow (low-energy ions) is extracted from the same negative-glow region and transported from the cathode to the surface of the anode chamber owing to an ambipolar diffusion. These ions are extracted from a hole in the anode chamber of a standard ion source by an electric field and are used for mass-spectrum analysis. The energy-distribution width for these ions is ∼5 eV. The intensity of the ion beam extracted from the anode hole is an order of magnitude higher than the intensity of the ion beam extracted from the cathode region. Original Russian Text ? G.G. Sikharulidze, 2009, published in Pribory i Tekhnika Eksperimenta, 2009, No. 2, pp. 105–109.     

Design of a cavity ring-down spectroscopy diagnostic for negative ion rf source SPIDER

The rf source test facility SPIDER will test and optimize the source of the 1 MV neutral beam injection systems for ITER. Cavity ring-down spectroscopy (CRDS) will measure the absolute line-of-sight integrated density of negative (H(-) and D(-)) ions, produced in the extraction region of the source. CRDS takes advantage of the photodetachment process: negative ions are converted to neutral hydrogen atoms by electron stripping through absorption of a photon from a laser. The design of this diagnostic is presented with the corresponding simulation of the expected performance. A prototype operated without plasma has provided CRDS reference signals, design validation, and results concerning the signal-to-noise ratio.     

Development of a new bimodal imaging methodology: a combination of fluorescence microscopy and high-resolution secondary ion mass spectrometry

In this paper, we present a new experimental methodology to combine mass spectrometry (NanoSIMS) with fluorescence microscopy to provide subcellular information on the location of small molecules in cultured cells. We demonstrate this by comparing the distribution of 5-bromo-2-deoxyuridine in the same cells given by both NanoSIMS analysis and by fluorescence immunohistochemistry. Fiducial markers in the substrates ensured that the images formed by SIMS mapping of bromine ions could be co-registered exactly with images from fluorescence microscopy. The NanoSIMS was shown to faithfully reproduce the information from fluorescence microscopy, but at a much higher spatial resolution. We then show preliminary SIMS images on the distribution of ATN-224, a therapeutic copper chelator for which there is no fluorescent marker, co-registered with conventional Lysotracker and Hoechst stains on the same cells.     

Electron tomography combining ESEM and STEM: a new 3D imaging technique

This paper presents the development and the application of a new electron tomography technique based on STEM (Scanning Transmission Electron Microscopy) configuration in ESEM (Environmental Scanning Electron Microscopy). This combination provides a new approach for the characterization of the 3D structure of materials, as it optimizes a compromise between the resolution level of a few tens of nm and the large tomogram size due to the high thickness of transparency. The method is well adapted for non-conductive samples, and exhibits good contrast even for materials with low atomic number. The paper describes the development of a dedicated stage for this new tomography technique. Taking advantage of the size of the ESEM chamber, the range of tilt angles is not limited by the space around the sample. The performance of this device is illustrated through the three-dimensional characterization of samples issued from materials science and chosen to illustrate the results in resolution, contrast and thickness.     

The hyperspectral irradiometer, a new instrument for long-term and unattended field spectroscopy measurements

Reliable time series of vegetation optical properties are needed to improve the modeling of the terrestrial carbon budget with remote sensing data. This paper describes the development of an automatic spectral system able to collect continuous long-term in-field spectral measurements of spectral down-welling and surface reflected irradiance. The paper addresses the development of the system, named hyperspectral irradiometer (HSI), describes its optical design, the acquisition, and processing operations. Measurements gathered on a vegetated surface by the HSI are shown, discussed and compared with experimental outcomes with independent instruments.     

端部中空离子源的磁场测量

研究了端部中空离子源的磁路设计.在简要叙述端部中空离子源的基本原理及其对磁场要求的基础上,考虑了在设计离子源磁路时的关键问题和解决方法,并给出了实验结果和分析结论.     

现代X光电子能谱(XPS)分析技术

现代电子能谱仪有3个主要功能:单色XPS(Mono XPS)、小面积XPS(SAXPS)和成像XPS(iXPS),被认为是光电子能谱仪发展方向。本文介绍这3个功能突出的特点及在材料微分析方面的实际应用。     

Development of environmental scanning electron microscopy electron beam profile imaging with self-assembled monolayers and secondary ion mass spectroscopy

A method for demonstrating the scattering of the primary electron beam in the presence of a gas has been developed. A self-assembled decanethiol monolayer is damaged by primary beam electrons. The damaged portion of the mono-layer is exchanged with another thiol-containing molecule by immersion in solution. The resulting film is imaged using a secondary ion mass spectrometer. Three-dimensional reconstruction of the data yields a representation of scattered electrons in the gaseous environment of the environmental scanning electron microscope.     

Quantitative DNA measurements in an instrument combining scanning electron microscopy and light microscopy

An instrument for combined scanning electron microscopy (SEM) and light microscopy (LM) to which a photometer unit is attached is described. A special stage in the vacuum chamber of a scanning electron microscope incorporates light microscope optics (objective and condenser) designed for transmission and epi-illumination fluorescence LM. An optical bridge connects these optics to a light microscope, without objective and condenser. The possibility of performing quantitative DNA measurements in this combined microscope (the LM/SEM) was tested using preparations of either chicken erythrocytes, human lymphocytes, or mouse liver cells. The cells were fixed, brought on a cover-glass, quantitatively stained for DNA, dehydrated, and critical point dried (CPD). After mounting the cells were coated with gold. The specimens were brought into the vacuum chamber of the combined microscope and individual cells were studied with SEM and LM. Simultaneously DNA measurements were performed by means of the photometer unit attached to the microscope. It is shown in this study that DNA measurements of cells in the combined microscope give similar results when compared to DNA measurements of embedded cells performed with a conventional fluorescence microscope. Furthermore, it is shown that although the gold layer covering the LM/SEM specimens weakens the fluorescence signal, it does not interfere with the DNA measurements.     

Characteristics of a multidipole ion source

The properties of a steady-state, dc discharge multidipole ion source have been investigated. The plasma density in the source depends on the magnet geometries, the discharge voltage, and the bias voltage on the first extraction grid. Different schemes to reduce the loss of ions to the chamber wall are described. Hydrogen ion species in the extracted beam are studied by a mass analyzer.