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Infrared Optical Constants from Pressed Pellets of Powders: I. Improved n and k Values of (NH4)(2)SO(4)from Single-Angle Reflectance
In combination with other parameters, the real, n(?), and imaginary, k(?), components of the complex refractive index, = n + ik, can be used to simulate the optical properties of a material in different forms, e.g. its infrared spectra. But obtaining reliable values of the optical constants n/k for solid materials is challenging due to the lack of optical quality specimens, usually crystals, large enough to measure. An alternative to crystals is to press the powder into a uniform disk. We have produced pellets from ammonium sulfate, (NH4)2SO4, powder and derived the pellets’ n and k values via single-angle reflectance using a specular reflectance device in combination with a Fourier transform infrared spectrometer. The single-angle technique measures amplitude of light reflected from the material as a function of wavelength over a wide spectral domain; the optical constants are determined from the reflectance data using the Kramers-Kronig relationship. We investigate several parameters associated with the pellets and pellet formation and their effects upon delivering the most reliable n/k values. Parameters studied include pellet diameter, mass and density (void space), drying, grinding, sieving and particle size in the pellet formation, as well as pressing pressure and duration. Of these parameters, using size-selected mixtures of dried, small (< 100 µm) particles and pressing at = 10 tons for at least 30 minutes were found key to forming highly reflective samples. Comparison to two sets of previous literature n(?) and k(?) values obtained from crystalline (NH4)2SO4 both as crystal reflectance as well as extinction spectra of aerosols measured in a flow tube show reasonable agreement, but suggests the present values, as confirmed from two independent techniques, represent a substantial improvement for n/k values for (NH4)2SO4, also demonstrating promise to measure the optical constants of other materials.
Chemical Vapor Deposition of Zirconium Compounds: A Review
Coatings of zirconium compounds are used in a wide variety of fields, yet an understanding and descriptions of deposition mechanisms are scant in the public literature. The mechanisms of deposition for metallic zirconium, ZrC, ZrN, ZrO 2 , ZrB 2 , and zirconium silicides are discussed based on the direct vapor deposition research of those compounds where possible or compared to complementary titanium systems when direct research is lacking. Both inorganic and organometallic deposition systems are discussed. As a class of compounds, an understanding of the vapor deposition mechanisms can be significantly improved by investigations on metallic zirconium deposition by zirconium halides and hydrogen and by in situ analysis techniques such as Fourier-transform infrared (FTIR) spectroscopy or x-ray photoelectron spectroscopy (XPS).
Vibronic Relaxation Pathways in Molecular Spin Qubit Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O under Pressure
In order to explore how spectral sparsity and vibronic decoherence pathways can be controlled in a model qubit system with atomic clock transitions, we combined diamond anvil cell techniques with synchrotron-based far infrared spectroscopy and first-principles calculations to reveal the vibrational response of Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O under compression. Because the hole in the phonon density of states acts to reduce the overlap between the phonons and f manifold excitations in this system, we postulated that pressure might move the HoO 4 rocking, bending, and asymmetric stretching modes that couple with the M J = ±5, ±2, and ±7 levels out of resonance, reducing their interactions and minimizing decoherence processes, while a potentially beneficial strategy for some molecular qubits, pressure slightly hardens the phonons in Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O and systematically fills in the transparency window in the phonon response. The net result is that the vibrational spectrum becomes less sparse and the overlap with the various M J levels of the Ho 3+ ion actually increases. These findings suggest that negative pressure, achieved using chemical means or elongational strain, could further open the transparency window in this rare earth-containing spin qubit system, thus paving the way for the use of device surfaces and interface elongational/compressive strains to better manage decoherence pathways.
Spectral ratio imaging methods for geological remote sensing from aircraft and satellites
The author has identified the following significant results. The production of ratio images from multispectral scanner data is described and several examples of ratio images from aircraft and ERTS-1 data are given for visible, reflective infrared, and thermal infrared wavelengths. The application of photogrammetric techniques to ratio images, defined for this paper as ratio scannergrammetry, is considerably aided by the lesser dependence of ratio images on atmospheric and solar illumination variations, compared with single channel scanner imagery or aerial photos. Ratio scannergrammetry is further aided by the proportionality between ratios of a target deduced from ratio images and ratios of reflectances calculated from laboratory spectra of samples from the target area. Consequently, ratios calculated from laboratory data can be used to predict which ratios are best for discriminating a given rock or mineral, to predict what other rocks or minerals will be confused with it, and finally, to place ratio scannergrammetry on an absolute basis, within an estimated standard error on the order of 5% to 10%. Examples of relative agreement between laboratory data and ratio images are given from two iron oxides, hematite and magnetite.
The molecular dynamics of atmospheric reaction
Detailed information about the chemistry of the upper atmosphere took the form of quantitative data concerning the rate of reaction into specified states of product vibration, rotation and translation for exothermic reaction, as well as concerning the rate of reaction from specified states of reagent vibration, rotation and translation for endothermic reaction. The techniques used were variants on the infrared chemiluminescence method. Emphasis was placed on reactions that formed, and that removed, vibrationally-excited hydroxyl radicals. Fundamental studies were also performed on exothermic reactions involving hydrogen halides.
Marine Resources
The papers presented in the marine session may be broadly grouped into several classes: microwave region instruments compared to infrared and visible region sensors, satellite techniques compared to aircraft techniques, open ocean applications compared to coastal region applications, and basic research and understanding of ocean phenomena compared to research techniques that offer immediate applications.
Characterization of initial cure reactions in propargyl and nadic end capped model compounds
Imide model compounds containing propargyl and nadic groups were studied to obtain a fundamental understanding of the reaction of these groups attached to imide oligomers. The initial cure reactions were examined by a variety of characterization techniques including high pressure liquid chromatography, infrared spectroscopy, thermal analyses, and mass spectroscopy. The initial step in the cure of propargyl end capped model compounds probably involved the formation of a new terminal acetylenic group. Configurational changes involving endo/exo isomerism was found in the nadimide model compounds. Nadimide compounds heated in air and in nitrogen appeared to cure by different mechanisms.
Impact-induced water loss from serpentine, nontronite and kernite
Preliminary experiments have been conducted to study shock-release of volatiles from minerals. Impact-induced loss of bound water from hydrous minerals has been observed, using infrared absorption and X-ray powder diffractometer techniques. Serpentine (Mg3Si2O5(OH)4) and nontronite (.5Ca(0.7)Fe4/(Si(7.3)Al(0.7))O20/(OH)4.nH2O) were shocked and recovered from pressures of up to 38 GPa, using one-dimensional shock reverberation techniques. Kernite (Na2B4O7.4H2O) was impacted by a spherical pyrex projectile traveling at 4.89 km/sec, which produced a peak pressure of approximately 33 GPa. The infrared absorption spectra indicate that some of the bound water from these three minerals was released as a result of shock compression and subsequent rarefaction. This evidence is supported by the recovery of small amounts of vapor from the serpentine shocked to 23.5 GPa and the nontronite shocked to 18 GPa. The recovered vapor is inferred to be water from the shocked minerals. X-ray diffraction spectra indicate no major changes in the unit cell dimensions of the two silicates, except for a decrease in the lattice constant in the c-direction of the nontronite, consistent with the loss of interlayer water.
A monolithic lead sulfide-silicon MOS integrated-circuit structure
A technique is developed for directly integrating infrared photoconductive PbS detector material with MOS transistors. A layer of chromium, instead of aluminum, is deposited followed by a gold deposition in order to ensure device survival during the chemical deposition of the PbS. Among other devices, a structure was fabricated and evaluated in which the PbS was directly coupled to the gate of a PMOS. The external bias, load, and source resistors were connected and the circuit was operated as a source-follower amplifier. Radiometric evaluations were performed on a variety of different MOSFETs of different geometry. In addition, various detector elements were simultaneously fabricated to demonstrate small element capability, and it was shown that elements of 25 x 25 microns could easily be fabricated. Results of room temperature evaluations using a filtered 700 K black body source yielded a detectivity at peak wavelength of 10 to the 11th cm (root Hz)/W at 100 Hz chopping frequency.
Tunable diode laser heterodyne spectrometer for remote observations near 8 microns
Infrared heterodyne spectroscopy is a passive technique employing coherent optical detection for the study of spectral features in remote sources. It employs optical components such as mirrors and lenses normally associated with incoherent optics, but because of it's coherent nature, it offers the advantages of ultrahigh spectral resolving power, high frequency precision, and diffraction limited field-of-view. Attention is given to the development of an ultrahigh resolution diode laser heterodyne spectrometer for observational and laboratory use. The instrument is designed for operation in the spectral range from 7.5 to 8.5 microns. A PbSe tuneable diode laser (TDL) is employed as local oscillator. A closed-cycle cooler is employed to keep the oscillator at operating temperatures in the range from 12 to 60 K. Attention is given to factors determining the TDL heterodyne sensitivity, the spectrometer design, and a survey of 8 micron observations, SiO could be detected in the sunspot spectrum.
Thermal bifurcation in the upper solar photosphere inferred from heterodyne spectroscopy of OH rotational lines
Low noise high spectral resolution observations of two pure rotation transitions of OH from the solar photosphere were obtained. The observations were obtained using the technique of optically null-balanced infrared heterodyne spectroscopy, and consist of center-to-limb line profiles of a v=1 and a v=0 transition near 12 microns. These lines should be formed in local thermodynamic equilibrium (LTE), and are diagnostics of the thermal structure of the upper photosphere. The v=0 R22 (24.5)e line strengthens at the solar limb, in contradiction to the predictions of current one dimensional photospheric models. Data for this line support a two dimensional model in which horizontal thermal fluctuations of order + or - 800K occur in the region Tau (sub 5000) approximately .001 to .01. This thermal bifurcation may be maintained by the presence of magnetic flux tubes, and may be related to the solar limb extensions observed in the 30 to 200 micron region.
Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications
Fourier transform infrared spectroscopy is currently the best technique for observing hydrolytic changes in DC 1200 silane the primers caused by moisture in the atmosphere. To further prove that FTIR can be used as a criterion test for acceptance of silane primer lots, intensities of the FTIR OH- band are being compared with primer adhesive bond strength using a mechanical test suggested by NASA. Results of tests for shear strength and Oh-absorption are tabulated and compared with FTIR absorption intensities in the OH-region.
Granitic terrains viewed remotely by Shuttle infrared radiometry - Some compositional predictions
Ratios of intensities of near-infrared spectral bands, measured in reflectance, quantitatively predict the iron content of granitic rocks. Such data from the 1.60- and 1.05-micron bands of the Shuttle multispectral infrared radiometer have been used to study granitic rocks along orbits crossing Baja California, Mexico, and the Eastern Desert of Egypt. Both regions are arid and relatively to essentially free of vegetation, and there is no indication in the spectra that surface chemical alteration masks the true composition of the unweathered rock. Predicted values of iron are consistent with known compositional types of most of the rocks along the orbital paths. Results demonstrate that the near-infrared method used is a powerful technique to average the variability of these rocks on the scales of meters to kilometers.
Efficient frequency conversion of laser sources in nonlinear crystals
The use of nonlinear crystals to extend the frequency range of solid-state laser sources is proposed. The harmonic generation of high-average-power laser sources and CW-laser-sources nonlinear crystals is considered. The development of Nd:YAG pumped parametric oscillators and optical parametric amplifiers using LiNbO3 or AgGaS2 is studied. The LiNbO3 oscillator has tunable output over the 1.4-4.0 micron range and is applicable for remote sensing measurements of molecules and of humidity and temperature; AgGaS2 oscillators provide the potential for 3-15 micron infrared generation. Advances in material synthesis techniques related to the design and synthesis of nonlinear media are discussed. Various procedures for the synthesis of nonlinear crystals are described.
Developments in flow visualization methods for flight research
With the introduction of modern airplanes utilizing laminar flow, flow visualization has become an important diagnostic tool in determining aerodynamic characteristics such as surface flow direction and boundary-layer state. A refinement of the sublimating chemical technique has been developed to define both the boundary-layer transition location and the transition mode. In response to the need for flow visualization at subsonic and transonic speeds and altitudes above 20,000 feet, the liquid crystal technique has been developed. A third flow visualization technique that has been used is infrared imaging, which offers non-intrusive testing over a wide range of test conditions. A review of these flow visualization methods and recent flight results is presented for a variety of modern aircraft and flight conditions.
Stability and reactivity of dimethylethoxysilane
The chemistry of the compound dimethylethoxysilane (DMES) is discussed especially as it relates to waterproofing silica surfaces. Some of the desirable properties of this compound are that it readily reacts with silica in the vapor phase, it is a low boiling point liquid (54 C), and the by-product of its reaction with silica is the rather inert substances ethanol. It is currently used by NASA to re-waterproof the HRSI shuttle tiles before relaunching the vehicle. Very little information is available on this particular compound in the literature or even on related silane compounds that have both a hydride group and an alkoxy group. Since the close proximity of two groups often drastically affects the chemical behavior of each group, chemical reactions were carried out in the laboratory with DMES to verify the expected behavior of these two functional groups located on DMES. Some of the reactions tested would be potentially useful for quantitative or qualitative measurements on DMES. To study the reactions of DMES with silica surfaces, cabosil was used as a silica substrate because of its high surface area and the ease of detection by infrared spectroscopy as well as other techniques.
A typical pointed observation in IRAS designed to fit into a 15 minute window
A typical pointed observation in the Infrared Astronomical Satellite (IRAS) was designed to fit into a 15 minute window. Observing constraints, however, did not always permit targets from the scientific program to be observed on exactly 15 minute centers and a few months into the mission it was realized that the automatic scheduling program left times when no observations were being made. In order to use this potentially wasted observing time, a mode of pointed observations, the 'filler' mode, with shorter observation duration was initiated. Locations were picked on an arbitrary grid, spaced relatively uniformly in ecliptic coordinates, and the telescope was pointed to one of these sites whenever a gap potentially occurred. One of us (GXN) was the coordinator of this effort (the FL sub-group). There are a total of 22 FL fields, 13 of which have more than 50 component observations. These 13 fields cover about 30 square degrees. It was proposed to concentrate on one filler field, FL29, a field with 53 coverages which thus had among the deepest coverage of those observed in this mode. This field was also observed extensively at various non-infrared wavelengths by a variety of techniques. Because the IRAS observations of FL29 were made at the limits of the survey sensitivity and at different twist angles it was necessary to make significant technical advances in the methods used in the processing and analyzing the data. In particular, if normal IRAS coaddition procedures were used, the noise resulting from coaddition of the multiple frames did not decrease in the manner expected once significantly different twist angles were included in the coaddition. The technical effort needed to reduce the observations of FL29 was completed and now the noise behavior is understood and well behaved. The reduction of the field FL29 observations is done.