A differentially pumped low-energy ion beam system for an ultrahigh-vacuum atom-probe field-ion microscope

An ultrahigh-vacuum (UHV) differentially pumped low-energy (50-3000 eV) ion beam system for the in situ irradiation of specimens in a UHV atom-probe field-ion microscope (FIM) was designed and constructed. The ion beam system consisted of a Finkelstein-type ion source, an Einzel lens, and a magnetic mass analyzer. The ion source was connected to the analyzer chamber by small apertures which resulted in differential pumping between the ion source and the analyzer chamber; during a typical in situ irradiation of a specimen in the atom-probe FIM the total pressure was maintained at approximately 10(-7) Torr. In the case of helium ion irradiation the optimum ion-current density was approximately 0.5 microA cm(-2) for 300-eV He+ ions at the atom-probe FIM specimen. After the completion of a helium ion irradiation the pumpdown time from 5 x 10(-7) to approximately 3 x 10(-10) Torr in the atom-probe FIM chamber was 0.5 h.     

Mirrorlike pulsed laser deposited tungsten thin film

Mirrorlike tungsten thin films on stainless steel substrate deposited via pulsed laser deposition technique in vacuum (10(-5) Torr) is reported, which may find direct application as first mirror in fusion devices. The crystal structure of tungsten film is analyzed using x-ray diffraction pattern, surface morphology of the tungsten films is studied with scanning electron microscope and atomic force microscope. The film composition is identified using energy dispersive x-ray. The specular and diffuse reflectivities with respect to stainless steel substrate of the tungsten films are recorded with FTIR spectra. The thickness and the optical quality of pulsed laser deposition deposited films are tested via interferometric technique. The reflectivity is approaching about that of the bulk for the tungsten film of thickness ～782 nm.     

Electron beam-induced thickening of the protective oxide layer around Fe nanoparticles

There are many circumstances in science where the process of measuring the properties of a system alters the system. An imaging process can exert an inadvertent effect on the object being observed. Consequently, what we observe does not necessarily represent what had been present before the observation. Normally, this effect can be ignored if the consequence of such a change is believed not to be significant. The expansion of nanostructured materials has made high-resolution transmission electron microscopy one of the indispensable tools for probing the characteristics of nanomaterials. Modification of nanoparticles by the electron beam during their imaging has been widely noticed and this is generally believed to be due to electron beam-induced heating effect, defect formation in the particles, charging of the particle, or excitation of surrounding gases. However, an explicit experimental identification of which process dominates is often very hard to establish. We report the thickening of native oxide layer on iron nanoparticle under electron beam irradiation. Based on atomic level imaging, electron diffraction, and computer simulation, we have direct evidence that the protecting oxide layer formed on Fe nanoparticle at room temperature in air or oxygen continues to grow during an electron beam bombardment in the vacuum system typical of most TEM systems. Typically, the oxide layer increases from approximately 3 to approximately 6 nm following approximately 1h electron beam exposure typically with an electron flux of 7 x 10(5)nm(-2)s(-1) and an vacuum of approximately 3 x 10(-5)Pa. Partial illumination of a nanoparticle and observation of the shell thickening conclusively demonstrates that many of the mechanisms postulated to explain such processes are not occurring to a significant extent. The observed growth is not related to the electron beam-induced heating of the nanoparticle, or residual oxygen ionization, or establishment of an electrical field, rather it is related to electron beam-facilitated mass transport across the oxide layer (a defect-related process). The growth follows a parabolic growth law.     

A technique for recording polycrystalline structure and orientation during in situ deformation cycles of rock analogues using an automated fabric analyser

Two in situ plane-strain deformation experiments on norcamphor and natural ice using synchronous recording of crystal c-axis orientations have been performed with an automated fabric analyser and a newly developed sample press and deformation stage. Without interrupting the deformation experiment, c-axis orientations are determined for each pixel in a 5 × 5 mm sample area at a spatial resolution of 5 μm/pixel. In the case of norcamphor, changes in microstructures and associated crystallographic information, at a strain rate of ～2 × 10(-5) s(-1), were recorded for the first time during a complete in situ deformation-cycle experiment that consisted of an annealing, deformation and post-deformation annealing path. In the case of natural ice, slower external strain rates (～1 × 10(-6) s(-1)) enabled the investigation of small changes in the polycrystal aggregate's crystallography and microstructure for small amounts of strain. The technical setup and first results from the experiments are presented.     

An efficient magneto-optical trap of metastable krypton atoms

We report a magneto-optical trap of metastable krypton atoms with a trap loading rate of 3×10(11) atoms/s and a trap capture efficiency of 3×10(-5). The system starts with an atomic beam of metastable krypton produced in a liquid-nitrogen cooled, radio-frequency driven discharge. The metastable beam flux emerging from the discharge is 1.5×10(14) atoms/s/sr. The flux in the forward direction is enhanced by a factor of 156 with transverse laser cooling. The atoms are then slowed inside a Zeeman slower before captured by a magneto-optic trap. The trap efficiency can be further improved, possibly to the 10(-2) level, by gas recirculation. Such an atom trap is useful in trace analysis applications where available sample size is limited.     

Dependence of surface morphology on molecular structure and its influence on the properties of OLEDs

Most organic light-emitting diodes (OLEDs) have a multilayer structure composed of organic layers such as a hole injection layer (HIL), a hole transport layer (HTL), an emission layer (EML), an electron transport layer (ETL) and an electron injection layer (EIL) sandwiched between two electrodes. The organic layers are thin solid films with a thickness from a few nano meters to a few tenths nano meter, respectively. Surface morphology of an organic thin solid film in OLEDs depends on the molecular structure of the organic material and has an affect on device performance. To analyze the effect of surface morphology of an organic thin solid film on fluorescence and electroluminescence (EL) properties, thin solid films of 4-(dicyanomethylene)-2-methyl-6-(julolidin-4-yl-vinyl)-4H-pyran (DCM2) and new red fluorophores, (2E,2′E)-3,3′-[4,4″-bis(dimethylamino)-1,1′:4′,1″-terphenyl-2′,5′-diyl]bis[2-(2-thienyl)acrylonitrile] (ABCV-Th) and (2Z,2′Z)-3,3′-[4,4″-bis(dimethylamino)-1,1′:4′,1″-terphenyl-2′,5′-diyl]bis(2-phenylacrylonitrile) (ABCV-P) were investigated by atomic force microscopy (AFM). The samples for EL and AFM measurement were fabricated by the high-vacuum thermal deposition (8×10⁻⁷ Torr) of organic materials onto the surface of indium tin oxide (ITO)-coated glass substrate, in which the layer structures of samples for AFM measurement and those for EL measurement were ITO/NPB (40 nm)/red emitters (80 nm) and ITO/NPB (40 nm)/red emitters (80 nm)/BCP (30 nm)/Liq (2 nm)/Al (100 nm), respectively. The analysis based on AFM measurements well supported that the photoluminescence properties and the device performance were very much dependent upon surface morphology of an organic thin layer.     

Formation of pentacene wetting layer on the SiO2 surface and charge trap in the wetting layer

We studied the early-stage growth of vacuum-evaporated pentacene film on a native SiO(2) surface using atomic force microscopy and in-situ spectroscopic ellipsometry. Pentacene deposition prompted an immediate change in the ellipsometry spectra, but atomic force microscopy images of the early stage films did not show a pentacene-related morphology other than the decrease in the surface roughness. This suggested that a thin pentacene wetting layer was formed by pentacene molecules lying on the surface before the crystalline islands nucleated. Growth simulation based on the in situ spectroscopic ellipsometry spectra supported this conclusion. Scanning capacitance microscopy measurement indicated the existence of trapped charges in the SiO(2) and pentacene wetting layer.     

IMPACT: a facility to study the interaction of low-energy intense particle beams with dynamic heterogeneous surfaces

The Interaction of Materials with Particles and Components Testing (IMPACT) experimental facility is furnished with multiple ion sources and in situ diagnostics to study the modification of surfaces undergoing physical, chemical, and electronic changes during exposure to energetic particle beams. Ion beams with energies in the range between 20 and 5000 eV can bombard samples at flux levels in the range of 10(10)-10(15) cm(-2) s(-1); parameters such as ion angle of incidence and exposed area are also controllable during the experiment. IMPACT has diagnostics that allow full characterization of the beam, including a Faraday cup, a beam imaging system, and a retarding field energy analyzer. IMPACT is equipped with multiple diagnostics, such as electron (Auger, photoelectron) and ion scattering spectroscopies that allow different probing depths of the sample to monitor compositional changes in multicomponent and/or layered targets. A unique real-time erosion diagnostic based on a dual quartz crystal microbalance measures deposition from an eroding surface with rates smaller than 0.01 nm/s, which can be converted to a sputter yield measurement. The monitoring crystal can be rotated and placed in the target position so that the deposited material on the quartz crystal oscillator surface can be characterized without transfer outside of the vacuum chamber.     

Efficient and inexpensive glass circulating pump

An efficient and inexpensive pump has been developed for the circulation of gaseous mixtures in a closed system. A continuous unidirectional flow of gas at rates of 0-40 l min(-1) was produced over an operating range of 10(-5)-10(-3) Torr.     

High-pressure scanning tunneling microscopy: tip reactions

Scanning tunneling microscopy (STM) is an ideal tool to image conducting and semiconducting surfaces with atomic resolution. The technique provides high-resolution images in vacuum or even high-pressure environments. Since STM can be operated at elevated pressures and temperatures, images can be collected in situ under catalytic conditions. In this work, we demonstrate that artifacts can be observed when imaging in situ since reactions can occur on the tip, and care should be taken when analyzing the data obtained.     

A high-pressure atomic force microscope for imaging in supercritical carbon dioxide

A high-pressure atomic force microscope (AFM) that enables in situ, atomic scale measurements of topography of solid surfaces in contact with supercritical CO(2) (scCO(2)) fluids has been developed. This apparatus overcomes the pressure limitations of the hydrothermal AFM and is designed to handle pressures up to 100 atm at temperatures up to ～350 K. A standard optically-based cantilever deflection detection system was chosen. When imaging in compressible supercritical fluids such as scCO(2), precise control of pressure and temperature in the fluid cell is the primary technical challenge. Noise levels and imaging resolution depend on minimization of fluid density fluctuations that change the fluid refractive index and hence the laser path. We demonstrate with our apparatus in situ atomic scale imaging of a calcite (CaCO(3)) mineral surface in scCO(2); both single, monatomic steps and dynamic processes occurring on the (1014) surface are presented. This new AFM provides unprecedented in situ access to interfacial phenomena at solid-fluid interfaces under pressure.     

An atomic beam source for fast loading of a magneto-optical trap under high vacuum

We report on a directional atomic beam created using an alkali metal dispenser and a nozzle. By applying a high current (15 A) pulse to the dispenser at room temperature we can rapidly heat it to a temperature at which it starts dispensing, avoiding the need for preheating. The atomic beam produced is capable of loading 90% of a magneto-optical trap (MOT) in less than 7 s while maintaining a low vacuum pressure of <10(-11) Torr. The transverse velocity components of the atomic beam are measured to be within typical capture velocities of a rubidium MOT. Finally, we show that the atomic beam can be turned off within 1.8 s.     

A Zeeman slower design with permanent magnets in a Halbach configuration

We describe a simple Zeeman slower design using permanent magnets. Contrary to common wire-wound setups, no electric power and water cooling are required. In addition, the whole system can be assembled and disassembled at will. The magnetic field is however transverse to the atomic motion and an extra repumper laser is necessary. A Halbach configuration of the magnets produces a high quality magnetic field and no further adjustment is needed. After optimization of the laser parameters, the apparatus produces an intense beam of slow and cold (87)Rb atoms. With typical fluxes of (1-5) × 10(10)?atoms/s at 30 m s(-1), our apparatus efficiently loads a large magneto-optical trap with more than 10(10) atoms in 1 s, which is an ideal starting point for degenerate quantum gas experiments.     

Plasma ion source for in situ ion bombardment in a soft x-ray magnetic scattering diffractometer

A new plasma ion source for in situ keV He ion bombardment of solid state samples or thin films was designed and built for ion fluences between 1 × 10(12) and 1 × 10(17) ions/cm(2). The system was designed to be mounted to different diffraction chambers for soft x-ray resonant magnetic scattering. Without breaking the vacuum due to He-ion bombardment, structural and magnetic modifications of the samples can be studied in situ and element specifically.     

High-sensitivity Q-band electron spin resonance imaging system with submicron resolution

A pulsed electron spin resonance (ESR) microimaging system operating at the Q-band frequency range is presented. The system includes a pulsed ESR spectrometer, gradient drivers, and a unique high-sensitivity imaging probe. The pulsed gradient drivers are capable of producing peak currents ranging from ～9 A for short 150 ns pulses up to more than 94 A for long 1400 ns gradient pulses. Under optimal conditions, the imaging probe provides spin sensitivity of ～1.6 × 10(8) spins∕√Hz or ～2.7 × 10(6) spins for 1 h of acquisition. This combination of high gradients and high spin sensitivity enables the acquisition of ESR images with a resolution down to ～440 nm for a high spin concentration solid sample (～10(8) spins∕μm(3)) and ～6.7 μm for a low spin concentration liquid sample (～6 × 10(5) spins/μm(3)). Potential applications of this system range from the imaging of point defects in crystals and semiconductors to measurements of oxygen concentration in biological samples.     

Two-chord interferometry using 3.39 μm He-Ne laser on a flux-coil-generated FRC

A two-chord λ(IR)～3.39?μm He-Ne laser interferometer system was developed for a flux-coil-generated field-reversed configuration to estimate the electron density and the total temperature of the field-reversed configuration (FRC) plasma. This two-chord heterodyne interferometer system consists of a single ～2?mW infrared He-Ne laser, a visible (λ(vis)～632.8?nm) He-Ne laser for the alignment, a 40 MHz acousto-optic modulator, photodetectors, and quadrature phase detectors. Initial measurement was performed and the measured average electron densities were 2-10×10(19)?m(-3) at two different radial positions in the midplane. A time shift in density was observed as the FRC expands radially. The time evolution of the line-averaged density agrees with the density estimated from the in situ internal magnetic probes, based on a rigid-rotor profile model.     

Measurement of volume resistivity∕conductivity of metallic alloy in inhibited seawater by optical interferometry techniques

Optical interferometry techniques were used for the first time to measure the volume resistivity∕conductivity of carbon steel samples in seawater with different concentrations of a corrosion inhibitor. In this investigation, the real-time holographic interferometry was carried out to measure the thickness of anodic dissolved layer or the total thickness, U(total), of formed oxide layer of carbon steel samples during the alternating current (ac) impedance of the samples in blank seawater and in 5-20 ppm TROS C-70 inhibited seawater, respectively. In addition, a mathematical model was derived in order to correlate between the ac impedance (resistance) and the surface (orthogonal) displacement of the surface of the samples in solutions. In other words, a proportionality constant [resistivity (ρ) or conductivity (σ) = 1∕ρ] between the determined ac impedance [by electrochemical impedance spectroscopy (EIS) technique] and the orthogonal displacement (by the optical interferometry techniques) was obtained. The value of the resistivity of the carbon steel sample in the blank seawater was found similar to the value of the resistivity of the carbon steel sample air, around 1 × 10(-5) Ω cm. On the contrary, the measured values of the resistivity of the carbon steel samples were 1.85 × 10(7), 3.35 × 10(7), and 1.7 × 10(7) Ω cm in 5, 10, and 20 ppm TROS C-70 inhibited seawater solutions, respectively. Furthermore, the determined value range of ρ of the formed oxide layers, from 1.7 × 10(7) to 3.35 × 10(7) Ω cm, is found in a reasonable agreement with the one found in literature for the Fe oxide-hydroxides, i.e., goethite (α-FeOOH) and for the lepidocrocite (γ-FeOOH), 1 × 10(9) Ω cm. The ρ value of the Fe oxide-hydroxides, 1 × 10(9) Ω cm, was found slightly higher than the ρ value range of the formed oxide layer of the present study. This is because the former value was determined by a dc method rather than by an electromagnetic method, i.e., holographic interferometry with applications of EIS, i.e., ac method. As a result, erroneous measurements were recorded due to the introduction of heat to Fe oxide-hydroxides.     

Combined low-temperature scanning tunneling/atomic force microscope for atomic resolution imaging and site-specific force spectroscopy

We present the design and first results of a low-temperature, ultrahigh vacuum scanning probe microscope enabling atomic resolution imaging in both scanning tunneling microscopy (STM) and noncontact atomic force microscopy (NC-AFM) modes. A tuning-fork-based sensor provides flexibility in selecting probe tip materials, which can be either metallic or nonmetallic. When choosing a conducting tip and sample, simultaneous STM/NC-AFM data acquisition is possible. Noticeable characteristics that distinguish this setup from similar systems providing simultaneous STM/NC-AFM capabilities are its combination of relative compactness (on-top bath cryostat needs no pit), in situ exchange of tip and sample at low temperatures, short turnaround times, modest helium consumption, and unrestricted access from dedicated flanges. The latter permits not only the optical surveillance of the tip during approach but also the direct deposition of molecules or atoms on either tip or sample while they remain cold. Atomic corrugations as low as 1 pm could successfully be resolved. In addition, lateral drifts rates of below 15 pm/h allow long-term data acquisition series and the recording of site-specific spectroscopy maps. Results obtained on Cu(111) and graphite illustrate the microscope's performance.     

A high-vacuum deposition system for in situ and real-time electrical characterization of organic thin-film transistors

We present a home-built high-vacuum system for performing organic semiconductor thin-film growth and its electrical characterization during deposition (real-time) or after deposition (in situ). Since the environment conditions remain unchanged during the deposition and electrical characterization process, a direct correlation between growth mode and electrical properties of thin film can be obtained. Deposition rate and substrate temperature can be systematically set in the range 0.1-10 ML∕min and RT-150 °C, respectively. The sample-holder configuration allows the simultaneous electrical monitoring of up to five organic thin-film transistors (OTFTs). The OTFTs parameters such as charge carrier mobility μ, threshold voltage V(TH), and the on-off ratio I(on)∕I(off) are studied as a function of the semiconductor thickness, with a submonolayer accuracy. Design, operation, and performance of the setup are detailed. As an example, the in situ and real-time electrical characterization of pentacene TFTs is reported.     

An apparatus based on a plasma emitter for electron-beam transportation to air

An apparatus for electron-beam transportation to air has been developed on the basis of an electron gun with a plasma emitter. A pressure drop from values of (1–3) × 10^?4 Torr in an accelerating gap to an air pressure of 760 Torr is produced by the differential pumping system. Usually, no less than three pumping stages are used in apparatuses based on hot-cathode guns for electron-beam transportation to air because of the need to maintain the pressure in the hot-cathode area at a level of 10^?5 Torr. It is possible to simplify the differential pumping system by reducing the number of stages to two via to the use of a gun with a plasma emitter. The construction of an apparatus for electron-beam transportation to air is described and its key characteristics are presented.