Showing papers in "Review of Scientific Instruments in 2001"

Application of acoustic resonators in photoacoustic trace gas analysis and metrology

Abstract: The application of different types of acoustic resonators such as pipes, cylinders, and spheres in photoacoustics is considered. This includes a discussion of the fundamental properties of these resonant cavities. Modulated and pulsed laser excitation of acoustic modes is discussed. The theoretical and practical aspects of high-Q and low-Q resonators and their integration into complete photoacoustic detection systems for trace gas monitoring and metrology are covered in detail. The characteristics of the available laser sources and the performance of the photoacoustic resonators, such as signal amplification, are discussed. Setup properties and noise features are considered in detail. This review is intended to give newcomers the information needed to design and construct state-of-the-art photoacoustic detectors for specific purposes such as trace gas analysis, spectroscopy, and metrology.

Computer-generated holographic optical tweezer arrays

Abstract: Holographic techniques significantly extend the capabilities of laser tweezing, making possible extended trapping patterns for manipulating large numbers of particles and volumes of soft matter. We describe practical methods for creating arbitrary configurations of optical tweezers using computer-generated diffractive optical elements. While the discussion focuses on ways to create planar arrays of identical tweezers, the approach can be generalized to three-dimensional arrangements of heterogeneous tweezers and extended trapping patterns.

Data reduction in 3ω method for thin-film thermal conductivity determination

Abstract: The 3ω method has been proven to be very useful for determining the thermal conductivity of thin films and their substrates. Several simplifications are often used in determining the thermal conductivity of the films based on the experimentally measured 3ω signal. These simplifications, however, have limited range of applicability. In this work, we present a detailed analysis and mathematical modeling of the 3ω method applied for different experimental conditions. Effects considered include the finite substrate thickness, anisotropic nature of the film and substrate thermal conductivity, the film-substrate thermal property contrasts, the effect of heat capacitance of the heater, and the effect of thermal boundary resistance. Several experimental results are analyzed using the models presented. This work shows that the 3ω method can be extended to a wide range of sample conditions, with anisotropic conductivities in both the substrate and the film, and with small film-substrate conductivity contrast.

3ω method for specific heat and thermal conductivity measurements

Abstract: We present a 3ω method for simultaneously measuring the specific heat and thermal conductivity of a rod- or filament-like specimen using a way similar to a four-probe resistance measurement. The specimen in this method needs to be electrically conductive and with a temperature-dependent resistance, for acting both as a heater to create a temperature fluctuation and as a sensor to measure its thermal response. With this method, we have successfully measured the specific heat and thermal conductivity of platinum wire specimens at cryogenic temperatures, and measured those thermal quantities of tiny carbon nanotube bundles some of which are only ∼10−9 g in mass.

High performance feedback for fast scanning atomic force microscopes

Abstract: We identify the dynamics of an atomic force microscope (AFM) in order to design a feedback controller that enables faster image acquisition at reduced imaging error compared to the now generally employed proportional integral differential (PID) controllers. First, a force model for the tip–sample interaction in an AFM is used to show that the dynamic behavior of the cantilever working in contact mode can be neglected for control purposes due to the relatively small oscillation amplitude of the cantilever in response to a defined topography step. Consequently, the dynamic behavior of the AFM system can be reduced to the behavior of the piezoelectric scanner making the design of a model based controller for the AFM possible. Second, a black box identification of the scanner of a commercial AFM (Nanoscope IIIa, Digital Instruments) is performed using subspace methods. Identification yields a mathematical model of the scanner which allows us to design a new controller utilizing H∞ theory. Finally, this contro...

Slice imaging: A new approach to ion imaging and velocity mapping

Abstract: In this article we present a new approach to the already popular methods of ion imaging and velocity mapping. The novelty of this approach is that the speed and angular distributions are measured directly from the images without the need of inverse Abel transformation as in the conventional approaches. This is achieved by using delayed pulsed extraction of the ions following photodissociation and positioning of the nascent products. Delayed pulsed extraction causes a sufficient velocity spread in the ion cloud such that the time width of the ion packet at the detector is on the order of 500 ns. By using a narrow detector time gate (<40 ns) we are able to image only the center slice of the ion packet. The result is equivalent to that obtained by conventional methods using the inverse Abel transform, however, the artificial noise introduced by this transform is eliminated. The energy resolution of the new approach is at least comparable to that achieved with the velocity mapping technique.

Optical Frequency Synthesis Based on Mode- Locked Lasers

Abstract: The synthesis of optical frequencies from the primary cesium microwave standard has traditionally been a difficult problem due to the large disparity in frequency. Recently this field has been dramatically advanced by the introduction and use of mode-locked lasers. This application of mode-locked lasers has been particularly aided by the ability to generate mode-locked spectra that span an octave. This review article describes how mode-locked lasers are used for optical frequency synthesis and gives recent results obtained using them.

An iterative procedure for the inversion of two-dimensional ion/photoelectron imaging experiments

Abstract: We present an iterative method for the extraction of velocity and angular distributions from two-dimensional (2D) ion/photoelectron imaging experiments. This method is based on the close relationship which exists between the initial 3D angular and velocity distribution and the measured 2D angular and radial distributions, and gives significantly better results than other inversion procedures which are commonly used today. Particularly, the procedure gets rid of the center-line noise which is one of the main artifacts in many current ion/photoelectron imaging experiments.

Laser heated diamond cell system at the Advanced Photon Source for in situ x-ray measurements at high pressure and temperature

Abstract: We describe a laser heated diamond anvil cell system at the GeoSoilEnviroCARS sector at the Advanced Photon Source. The system can be used for in situ x-ray measurements at simultaneously ultrahigh pressures (to >150 GPa) and ultrahigh temperatures (to >4000 K). Design goals of the laser heating system include generation of a large heating volume compared to the x-ray beam size, minimization of the sample temperature gradients both radially and axially in the diamond anvil cell, and maximization of heating stability. The system is based on double-sided laser heating technique and consists of two Nd:YLF lasers with one operating in TEM00 mode and the other in TEM01* mode, optics to heat the sample from both sides, and two spectroradiometric systems for temperature measurements on both sides. When combined with an x-ray microbeam (3–10 μm) technique, a temperature variation of less than 50 K can be achieved within an x-ray sampled region for longer than 10 min. The system has been used to obtain in situ str...

Littrow configuration tunable external cavity diode laser with fixed direction output beam

Abstract: We have developed an enhanced Littrow configuration extended cavity diode laser (ECDL) that can be tuned without changing the direction of the output beam. The output of a conventional Littrow ECDL is reflected from a plane mirror fixed parallel to the tuning diffraction grating. Using a free-space Michelson wavemeter to measure the laser wavelength, we can tune the laser over a range greater than 10 nm without any alteration of alignment.

High resolution nonlinear microscopy: A review of sources and methods for achieving optimal imaging

Abstract: This article reviews the latest instrumentation used in high resolution nonlinear microscopy and techniques for the temporal and spatial calibration of this instrumentation. This includes an overview of currently available ultrashort laser sources, the dispersion characteristics of microscopes, methods for pulse measurement at high numerical aperture, dispersion compensation techniques, and finally a brief overview of a number of nonlinear imaging methods presently used in these systems.

The role of dispersion in ultrafast optics

Abstract: In this article, we review the phenomenon of dispersion, paying particular attention to its impact in the optics of ultrashort pulses, as well as its measurement and management. At present, lasers generating coherent bandwidths of several hundred nanometers have been demonstrated and correspondingly short pulses of 10 fs or so are quite usual. The limits to the breadth of optical spectra and brevity of pulse durations that may be achieved are often set by the dispersive properties of the linear optical elements of which the source is constructed. Progress in ultrafast optics to date has therefore relied extensively on the development of ways to characterize and manipulate dispersion. The means by which this can be accomplished are significantly different for laser oscillators and laser amplifiers, as well as for nonlinear interactions that are used to extend the range of frequencies at which short optical pulses are available, but in all cases it is this phenomenon that determines the output of current optical sources.

Resolution limits for infrared microspectroscopy explored with synchrotron radiation

Abstract: The spatial resolution for infrared microspectroscopy is investigated to determine the practical limits imposed by diffraction or optical aberrations. Quantitative results are obtained using high brightness synchrotron radiation, which serves as a diffraction-limited infrared “point source” for the microscope. The measured resolving power is in good agreement with diffraction theory, including a ∼ 30% improvement for a confocal optical arrangement. The diffraction calculation also shows how the confocal setup leads to better image contrast. The full width at half maximum of the instrument’s resolution pattern is approximately λ/2 for this arrangement. One achieves this diffraction limit when the instrument’s apertures define a region having dimensions equal to the wavelength of interest. While commercial microspectrometers are well corrected for optical aberrations (allowing diffraction-limited results), the standard substrates used for supporting specimens introduce chromatic aberrations. An analysis of ...

A solid-state dedicated circular dichroism spectrophotometer: Development and application

Abstract: A solid-state dedicated circular dichroism (CD) spectrophotometer (J-800KCM) was designed and constructed. As a CD spectrophotometer is a polarization–modulation instrument, CD spectra are necessarily accompanied by artifacts due to macroscopic anisotropies such as linear birefringence (LB) and linear dichroism (LD) which are unique to the solid state. A photomultiplier with the least polarization characteristics and a photoelastic modulator (PEM) with the least residual static birefringence were selected for the new instrument, which was based on the electrical and optical systems of a commercially available spectrophotometer. A phased-locked loop circuit was introduced to a PEM driver, and a sample rotation holder, a stage controller, and an analyzer were installed. We have designed and built a special solid-state sample holder to enable the cancellation of artifact CD, and a lens unit for smaller samples. A set of procedures for obtaining true CD has been devised based on the Mueller matrix method, and...

Collisions of ions with surfaces at chemically relevant energies: Instrumentation and phenomena

Abstract: An overview of gaseous ion/surface collisions is presented, with special emphasis on the behavior of polyatomic projectile ions at hyperthermal collision energies (1–100 eV) and the instrumentation needed for such studies. The inelastic and reactive processes occurring during ion/surface collisions are described in terms of several archetypes, viz., elastic and quasielastic scattering, chemical sputtering leading to release of surface material, inelastic scattering leading to surface-induced dissociation (SID) of the projectile, ion/surface reactions, and soft landing. Parameters that are important in ion/surface interactions are discussed, including the interaction time, the conversion of translational to internal energy, the translational energies of the scattered ions, the effects of scattering angle, and the influence of the nature of the surface. Different types of tandem mass spectrometers, built specifically to study ion/surface collision phenomena, are discussed and the advantages and disadvantages of the individual designs are compared. The role of SID as a technique in bioanalytical mass spectrometry is illustrated and this inelastic collision experiment is compared and contrasted with gas-phase collision-induced dissociation, the standard method of tandem mass spectrometry. Special emphasis is placed on reactive scattering including the use of ion/surface reactions for surface chemical analysis and for surface chemical modification.

A parallel-detection frequency-domain near-infrared tomography system for hemoglobin imaging of the breast in vivo

Abstract: A novel near-infrared frequency-domain system designed for tomographic breast imaging is described. The setup utilizes five optical wavelengths, from 660 to 826 nm, and parallel detection with 16 photomultiplier tubes. Direct fiberoptic coupling with the tissue is achieved with a high precision positioning device using 16 motorized actuators (0.5 μm precision) arranged radially in a circular geometry. Images of breast tissue optical absorption and reduced scattering coefficients are obtained using a Newton-type reconstruction algorithm to solve for the optimal fit between the measurement data and predicted data from a finite element solution to the frequency-domain diffusion equation. The design, calibration, and performance of the tomographic imaging system are detailed. Data acquisition from the system requires under 30 s for a single tomographic slice at one optical wavelength with a measurement repeatability for a single phantom on average of 0.5% in ac intensity and 0.4° in phase. Absorbing and scatt...

Quantitative modulated excitation Fourier transform infrared spectroscopy

Abstract: The detection of weak absorption changes induced by an external excitation is often hindered by intense background absorptions as well as by noise. Modulation spectroscopy is an adequate tool to be applied in such a case, provided the system may be periodically stimulated, leading to a periodic reversible or pseudoreversible response. In modulated excitation (ME) Fourier transform infrared spectroscopy the phase sensitive detection (PSD) used for the demodulation of the periodic system response is generally performed during data acquisition, i.e., applied to the intensity of the interferogram. This leads to a number of problems in quantitative analysis and the requirement of optional equipment. In this article, a method is presented to perform an off-line vector PSD of conventional time-resolved spectra after data acquisition. A detailed mathematical analysis of PSD applied to the spectral intensity, the interferogram intensity, and to time-resolved spectra is presented. It is shown, that vector PSD applied to a set of time-resolved spectra is straightforward and avoids any additional mathematical corrections. Furthermore, it will be shown how ME spectroscopy can be used for experimental separation of overlapping bands and a detailed description for the determination of absolute modulation amplitudes and phase lags is given.

A high-pressure scanning tunneling microscope

Abstract: We present the design and performance of a high-pressure scanning tunneling microscope (HP–STM), which allows atom-resolved imaging of metal surfaces at pressures ranging from ultrahigh vacuum (UHV) to atmospheric pressures (1×10−10–1000 mbar) on a routine basis. The HP–STM is integrated in a gold-plated high-pressure cell with a volume of only ∼0.5 l, which is attached directly to an UHV preparation/analysis chamber. The latter facilitates quick sample transfer between the UHV chamber and the high-pressure cell, and allows for in situ chemical and structural analysis by a number of analytical UHV techniques incorporated in the UHV chamber. Reactant gases are admitted to the high-pressure cell via a dedicated gas handling system, which includes several stages of gas purification. The use of ultrapure gasses is essential when working at high pressures in order to achieve well-defined experimental conditions. The latter is demonstrated in the case of H/Cu(110) at atmospheric H2 pressures where impurity-rela...

Quantitative sensing of nanoscale colloids using a microchip Coulter counter

Abstract: We have fabricated a microchip Coulter counter on a quartz substrate, and have used it to detect individual nanoscale colloidal particles with a sensitivity proportional to each particle's size. We demonstrate the ability of this device to sense colloids as small as 87 nm diameter, and to distinguish between colloids whose diameters differ by less than 10%. Further reductions in the pore size, easily done with current nanofabrication techniques, make our device applicable to measuring biological macromolecules, such as DNA and proteins.

Design and performance of the Thomson scattering diagnostic on LHD

Abstract: This article describes the design and performance of a multi-point (200) high repetition rate (4×50 Hz) Thomson scattering diagnostic installed on the Large Helical Device. A unique feature of this system is its oblique back scattering configuration, which enables us to observe the entire plasma region along a major radius on the midplane under a severely restricted port constraint. High throughput collection optics using a mosaic mirror of 1.5 m×1.8 m area yield high quality data even with 0.5 J pulse energy delivered from 50 Hz repetition rate Nd: yttrium–aluminum–garnet lasers. High repetition and high spatial resolution (2–4 cm) of the system enable us to study island evolution in the plasma.

Experimental configuration for isentropic compression of solids using pulsed magnetic loading

Abstract: A capability to produce quasi-isentropic compression of solids using pulsed magnetic loading on the Z accelerator has recently been developed and demonstrated [C. A. Hall, Phys. Plasmas 7, 2069 (2000)]. This technique allows planar, continuous compression of materials to stresses approaching 1.5 Mbar. In initial stages of development, the experimental configuration used a magnetically loaded material cup or disk as the sample of interest pressed into a conductor. This installation caused distortions that limited the ability to attach interferometer windows or other materials to the rear of the sample. In addition, magnetic pressure was not completely uniform over sample dimensions of interest. A new modular configuration is described that improves the uniformity of loading over the sample surface, allows materials to be easily attached to the magnetically loaded sample, and improves the quality of data obtained. Electromagnetic simulations of the magnetic field uniformity for this new configuration will also be presented. Comparisons between data on copper to ∼300 kbar using the old and new experimental configurations will also be made. Results indicate that to within experimental error, the configurations produce similar results in the pressure-volume plane.

Development of a fast fiber-optic two-color pyrometer for the temperature measurement of surfaces with varying emissivities

Abstract: A two-color pyrometer has been developed to measure the temperature of surfaces with unknown emissivities during high speed turning processes. Quartz fibers enable measurements at locations with limited optical access. The sensitivity of the pyrometer has to be high enough to measure temperatures down to 300 °C of an aluminum alloy with an emissivity as low as 0.2. The accuracy of the two-color pyrometer has been compared with the accuracy of monochromatic pyrometers for different metallic surfaces. The different arguments for the choice of the two pyrometer wavelengths 1.7 and 2.0 μm are explained. The influences of the surface emissivities, the digitization, and the noise on the absolute and relative measurement error have been determined. Fast amplifiers and data acquisition allow a maximum time resolution of a few microseconds and a local resolution of ∼0.5 mm2. Some test measurements of an aluminum alloy surface are presented.

A high-throughput x-ray microtomography system at the Advanced Photon Source

Abstract: A third-generation synchrotron radiation source provides enough brilliance to acquire complete tomographic data sets at 100 nm or better resolution in a few minutes. To take advantage of such high-brilliance sources at the Advanced Photon Source, we have constructed a pipelined data acquisition and reconstruction system that combines a fast detector system, high-speed data networks, and massively parallel computers to rapidly acquire the projection data and perform the reconstruction and rendering calculations. With the current setup, a data set can be obtained and reconstructed in tens of minutes. A specialized visualization computer makes rendered three-dimensional (3D) images available to the beamline users minutes after the data acquisition is completed. This system is capable of examining a large number of samples at sub-μm 3D resolution or studying the full 3D structure of a dynamically evolving sample on a 10 min temporal scale. In the near future, we expect to increase the spatial resolution to be...

Microspectroscopy and imaging using a delay line detector in time-of-flight photoemission microscopy

Abstract: A method for microspectroscopy and energy-selective imaging using a special photoemission electron microscope (PEEM) is presented. A modified commercial PEEM was combined with a delay line device as x, y, t detector serving as the basic arrangement for spectromicroscopy. One can measure the time of flight of the electrons passing a drift section in order to analyze the energy distribution of photoelectrons in PEEM. The time of flight is referenced to the time structure of the synchrotron radiation from an electron storage ring. At electron kinetic energies of less than 20 eV within the drift region a spatial resolution of about 100 nm has been obtained. Fast counting electronics (instead of a camera) delivers an image for real-time monitoring on an oscilloscope screen or for image acquisition by a computer. A time resolution of about 500 ps has been obtained with the potential of further improvement. The spatial resolution of the delay line detector is about 50 μm in the image plane corresponding to 1000 ...

High density gas jet nozzle design for laser target production

Abstract: The optimization of a cylindrical nozzle design to generate a uniform density profile for laser plasmas studies has been investigated using numerical simulations. In addition gas jet flows have been characterized using a Mach–Zehnder interferometer. The experimental results are in very good agreement with the simulation.

Frequency domain instrument for measuring phosphorescence lifetime distributions in heterogeneous samples

Abstract: The luminescence lifetime distribution can be used to determine the distribution of quencher concentrations in a heterogeneous sample We describe a frequency domain instrument for real-time measurements of phosphorescence lifetime distributions in microheterogeneous objects In this system (1) an array of harmonics (typically 100–200 frequencies) is used to modulate the excitation source, a light emitting diode Due to the relatively long triplet state lifetimes, the frequencies required for the modulation are typically below 40 000 kHz, which allows direct digitization of both excitation and emission signals (2) The dependence of the phase/amplitude factor on the modulation frequency is determined by linear least-squares analysis of the emission signal, which is sampled and summed over the multiple excitation cycles (3) The phase/amplitude relationship obtained is analyzed in real time using a “light” version of the maximum entropy algorithm, which provides a complete phosphorescence lifetime distribution (4) The lifetime distribution is converted into the distribution of quencher concentrations using an appropriate model of quenching The instrument is also capable of measuring phosphorescence in “single-frequency” mode, which is useful for rapid evaluation of apparent luminescence lifetimes In this mode, a correction for an in-phase signal, which is due to backscattering and fluorescence, is applied to improve the accuracy of lifetime measurements The instruments were tested in Stern–Volmer calibrations of Pd-porphyrin based phosphors for oxygen measurements and used for preliminary evaluation of oxygen distributions in rat tumor tissues The instruments were found to be capable of accurate determination of lifetimes in the range of 10–3000 μs The average duration of a single lifetime distribution measurement was about 15 s, depending on the sample and on the density of the lifetime grid in the maximum entropy method analysis In the single-frequency mode, the measurement time was reduced to about 02–05 s The instruments provide complete correction for the in-phase signal of up to 40% of the total emission intensity

Effects of temperature and other experimental variables on single molecule vibrational spectroscopy with the scanning tunneling microscope

Abstract: Inelastic electron tunneling spectroscopy (IETS) was performed on single molecules with a variable temperature scanning tunneling microscope. The peak intensity, width, position, and line shape of single molecule vibrational spectra were studied as a function of temperature, modulation bias, bias polarity, and tip position for the (C–H,C–D) stretching vibration of acetylene (C2H2,C2D2) on Cu(001). The temperature broadening of vibrational peaks was found to be a consequence of Fermi smearing as in macroscopic IETS. The modulation broadening of vibrational peaks assumed the expected form for IETS. Extrapolation of the peak width to zero temperature and modulation suggested an intrinsic width of ∼4 meV due primarily to instrumental broadening. The inelastic tunneling cross section at negative bias was reduced by a factor of 1.7 for the C–H stretch mode. Low energy modes of other molecules did not show such a reduction. There was no evidence of a tip-induced Stark shift in the peak positions. The spatial var...

Analog frequency modulation detector for dynamic force microscopy

Abstract: A new analog frequency modulation (FM) detector (demodulator) for dynamic force microscopy (DFM) is presented. The detector is designed for DFM by utilizing the FM detection method where the resonance frequency shift of the force sensor is kept constant to regulate the distance between a tip and a sample surface. The FM detector employs a phase-locked loop (PLL) circuit using a voltage-controlled crystal oscillator (VCXO) so that the thermal drift of the output signal is negligibly reduced. The PLL is used together with a frequency conversion (heterodyne) circuit allowing the FM detector to be used for a wide variety of force sensors with the resonance frequency ranging from 10 kHz to 10 MHz. The minimum detectable frequency shift was as small as 0.1 Hz at the detection bandwidth of 1 kHz. The detector can track a resonance frequency shift as large as 1 kHz. We also present some experimental results including the observations of the Si(111)-7×7 reconstructed surface and fullerene molecules deposited on the surface by DFM using this FM detector.

X-ray backlighting for the National Ignition Facility (invited)

Abstract: X-ray backlighting is a powerful tool for diagnosing a large variety of high-density phenomena. Traditional area backlighting techniques used at Nova and Omega cannot be extended efficiently to National Ignition Facility scale. New, more efficient backlighting sources and techniques are required and have begun to show promising results. These include a backlit-pinhole point-projection technique, pinhole and slit arrays, distributed polychromatic sources, and picket-fence backlighters. In parallel, there have been developments in improving the data signal-to-noise and, hence, quality by switching from film to charge-coupled-device-based recording media and by removing the fixed-pattern noise of microchannel-plate-based cameras.

Edge turbulence measurements in NSTX by gas puff imaging

Abstract: Turbulent filaments in visible light emission corresponding mainly to density fluctuations at the edge have been observed in large aspect ratio tokamaks: TFTR, ASDEX, Alcator C-Mod, and DIII-D. This article reports on similar turbulent structures observed in the National Spherical Torus Experiment (NSTX) using a fast-framing, intensified, digital visible camera. These filaments were previously detected mainly in high recycling regions, such as at limiters or antennas, where the line emission from neutral atoms was modulated by the fluctuations in local plasma density. However, by introducing controlled edge gas puffs, i.e., gas puff imaging, we have increased the brightness and contrast in the fluctuation images and allowed the turbulent structure to be measured independently of the recycling. A set discrete fiber-optically coupled sight-lines also measured the frequency spectra of these light fluctuations with a 200 kHz bandwidth. Initial results in NSTX show that the turbulent filaments are well aligned with the magnetic field which can be up to 45° from the horizontal at the outer midplane of NSTX. The dominant wavelength perpendicular to the magnetic field is ∼7–11 cm, corresponding to a k⊥ ρs of ∼0.3 at an assumed Te=25 eV, and the frequency spectra has a typical broad shape characteristic of edge turbulence extending to about 100 kHz. By imaging a He gas puff along a magnetic field line the characteristic radial scalelength appears to be in the 3–5 cm range.