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At least 37 records · Page 2

Cleaning without chlorinated solvents

Because of health and environmental concerns, many regulations have been passed in recent years regarding the use of chlorinated solvents. The Oak Ridge Y-12 Plant has had an active program to find alternatives for these solvents used in cleaning applications for the past 7 years. During this time frame, the quantity of solvents purchased has been reduced by 92 percent. The program has been a twofold effort. Vapor degreasers used in batch cleaning operations have been replaced by ultrasonic cleaning with aqueous detergent, and other organic solvents have been identified for use in hand-wiping or specialty operations. In order to qualify these alternatives for use, experimentation was conducted on cleaning ability as well as effects on subsequent operations such as welding, painting, and bonding. Cleaning ability was determined using techniques such as x-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) which are capable of examining monolayer levels of contamination on a surface. Solvents have been identified for removal of rust preventative oils, lapping oils, machining coolants, lubricants, greases, and mold releases. Solvents have also been evaluated for cleaning urethane foam spray guns, swelling of urethanes, and swelling of epoxies.

Thompson, L. M.↗

Surface Chemistry, Microstructure, and Tribological Properties of Cubic Boron Nitride Films

This report deals with the surface chemistry, microstructure, bonding state, morphology, and friction and wear properties of cubic boron nitride (c-BN) films that were synthesized by magnetically enhanced plasma ion plating. Several analytical techniques - x-ray photoelectron spectroscopy, transmission electron microscopy and electron diffraction, Fourier transform infrared spectroscopy, atomic force microscopy, and surface profilometry - were used to characterize the films. Sliding friction experiments using a ball-on-disk configuration were conducted for the c-BN films in sliding contact with 440C stainless-steel balls at room temperature in ultrahigh vacuum (pressure, 10(exp -6), in ambient air, and under water lubrication. Results indicate that the boron-to-nitrogen ratio on the surface of the as-deposited c-BN film is greater than 1 and that not all the boron is present as boron nitride but a small percentage is present as an oxide. Both in air and under water lubrication, the c-BN film in sliding contact with steel showed a low wear rate, whereas a high wear rate was observed in vacuum. In air and under water lubrication, c-BN exhibited wear resistance superior to that of amorphous boron nitride, titanium nitride, and titanium carbide.

Watanabe, Shuichi↗

Contamination and Surface Preparation Effects on Composite Bonding

Results presented here demonstrate the effect of several prebond surface contaminants (hydrocarbon, machining fluid, latex, silicone, peel ply residue, release film) on bond quality, as measured by fracture toughness and failure modes of carbon fiber reinforced epoxy substrates bonded in secondary and co-bond configurations with paste and film adhesives. Additionally, the capability of various prebond surface property measurement tools to detect contaminants and potentially predict subsequent bond performance of three different adhesives is also shown. Surface measurement methods included water contact angle, Dyne solution wettability, optically stimulated electron emission spectroscopy, surface free energy, inverse gas chromatography, and Fourier transform infrared spectroscopy with chemometrics analysis. Information will also be provided on the effectiveness of mechanical and energetic surface treatments to recover a bondable surface after contamination. The benefits and drawbacks of the various surface analysis tools to detect contaminants and evaluate prebond surfaces after surface treatment were assessed as well as their ability to correlate to bond performance. Surface analysis tools were also evaluated for their potential use as in-line quality control of adhesive bonding parameters in the manufacturing environment.

Kutscha, Eileen O.↗

Characterizing Nanophase Materials on Mars: Spectroscopic Studies of Allophane and Imogolite

Allophane is an amorphous or poorly crystalline hydrous aluminosilicate material. Allophane's chemical structure represents a hollow nanosphere, 5-6 nm in diameter with 4-7 large pores in the structure. Identification of allophane and other amorphous and nanophase minerals on Mars has provided clues about the aqueous geochemical environment there. These materials likely represent partially altered or leached basaltic ash and therefore, could represent a geologic marker for where water was present on the Martian surface; as well as indicate regions of climate change, where surface water was not present long enough or sufficiently warm to form clays. Characterization of these materials is important for increasing spectral recognition capabilities using visible/near-infrared (VNIR) and thermal infrared (TIR) spectra of Mars. A suite of synthetic allophane samples was created using a method that has been modified to produce allophane with Fe isomorphically substituted for Al in octahedral coordination. Compositions of the materials range from high-Si allophane (molar Al:Si = 1:2) to protoimogolite (Al:Si = 2:1), with Fe(3+) and Fe(2+) isomorphically substituted for Al from 0-10 mol% of total Al. These compositions span the range observed in natural terrestrial allophanes. Fe K-edge X-ray absorption spectroscopy provided information on the speciation and electrochemical and structural position of Fe in the framework. Fourier transform infrared spectroscopy confirmed syntheses and demonstrated changes in infrared spectroscopic signature with Fe substitution. VNIR reflectance spectra and TIR Thermal infrared emissivity spectra were also collected for direct comparison to Martian data. By increasing spectral recognition capacities of nanophase materials, more accurate estimates can be made on the aqueous geochemical environment of Mars.

Jeute, Thomas↗

High-resolution spectroscopy of H2SO4, HDSO4, and D2SO4 vapor in the region 1200-10,000 cm(-1)

The high-resolution (0.05 cm(-1)) spectra of gas-phase H2SO4, HDSO4, and D2SO4 were measured over the frequency region 1200-10,000 cm(-1) using Fourier-transform infrared spectroscopy. The increased resolution of this work compared with previous studies has lead to an improved vibrational analysis of H2SO4. This study has answered unresolved questions about combination bands and overlapping features from previous gas-phase spectroscopic studies of H2SO4 and marks the first experimental measurement of the nu8 and nu15 torsional vibrations in this molecule. This work leads to a brief discussion on vibrational mode mixing in sulfuric acid.

Deuterium/chemistry↗

Heavy Ozone Enrichment from ATMOS Infrared Solar Spectra

Vertical enrichment profiles of stratospheric ozone with oxygen 18 in the second or third position have been derived from space- based solar occultation spectra recorded at 0.01/cm resolution with the ATMOS (Atmospheric Trace Molecule Spectroscopy) Fourier- transform infrared (FTIR) spectrometer.

ozone↗

Heavy Ozone Enrichments from ATMOS Infrared Solar Spectra

Vertical enrichment profiles of stratospheric O-16O-16O-18 and O-16O-18O-16 (hereafter referred to as (668)O3 and (686)O3 respectively) have been derived from space-based solar occultation spectra recorded at 0.01 cm(exp-1) resolution by the ATMOS (Atmospheric Trace MOlecule Spectroscopy) Fourier transform infrared (FTIR) spectrometer. The observations, made during the Spacelab 3 and ATLAS-1, -2, and -3 shuttle missions, cover polar, mid-latitude and tropical regions between 26 to 2.6 mb inclusive (approximately 25 to 41 km). Average enrichments, weighted by molecular (48)O3 density, of (15 +/- 6)% were found for (668)O3 and (10 +/- 7)% for (686)O3. Defining the mixing ratio of (50)O3 as the sum of those for (668)O3 and (686)O3, an enrichment of (13 plus or minus 5)% was found for (50)O3 (1 sigma standard deviation). No latitudinal or vertical gradients were found outside this standard deviation. From a series of ground-based measurements by the ATMOS instrument at Table Mountain, California (34.4 deg N), an average total column (668)O3 enrichment of (17 +/- 4)% (1 sigma standard deviation) was determined, with no significant seasonal variation discernable. Possible biases in the spectral intensities that affect the determination of absolute enrichments are discussed.

Irion, F. W.↗

Synthesis of Submillimeter Radiation for Spectroscopy

The frequency-multiplier submillimeter spectrometer (FMSS) is a laboratory apparatus for far-infrared molecular spectroscopy, embodying several advances over prior such apparatuses. The most innovative part of the FMSS is a source of monochromatic submillimeter- wavelength radiation that can be tuned over a wide frequency range, as needed for trace gas analyses and molecular- structure studies for which such apparatuses are typically used. The radiation source features a modular design and is built mostly from commercially available components. It includes a computer-controlled radio-frequency synthesizer, amplifiers, and frequency multipliers of a type heretofore used in local oscillators for heterodyne far-infrared receivers. In conjunction with the rest of the apparatus, this source makes it possible to perform measurements over large portions of the submillimeter-wavelength spectrum with resolution, accuracy, and sensitivity greater than those achievable in Fourier-transform infrared spectroscopy. In comparison with prior laboratory submillimeter- wavelength radiation sources, this source is much lighter in weight, less cumbersome, less power-hungry, and capable of sustained operation with less intervention by laboratory personnel. Also, unlike some prior submillimeter-wavelength sources, this source does not require a high-voltage power source. As shown in more detail in the figure, the radiation source includes a sweep frequency synthesizer connected to an external waveform generator, the output of which is used as a reference signal. The synthesizer is computer-controlled through a standard general-purpose interface bus (GPIB) and is operated in phase-locked continuous- wave mode for all measurements. The synthesizer output ranges in frequency from 11 to 18 GHz. For suppression of frequency spurs and harmonics, the output of the frequency synthesizer is fed through a tunable yttrium iron garnet (YIG) filter, which is swept in frequency simultaneously with the frequency synthesizer.

Maiwald, Frank↗

Instrumental sensing of stationary source emissions

A variety of programs have been conducted within EPA to evaluate the capability of various ground-based remote-sensing techniques for measuring the SO2 concentration, velocity, and opacity of effluents from coal-burning power plants. The results of the remote measurements were compared with the results of instack measurements made using EPA reference methods. Attention is given to infrared gas-filter correlation radiometry for SO2 concentration, Fourier-transform infrared spectroscopy for SO2 concentration, ultraviolet matched-filter correlation spectroscopy for SO2 concentration, infrared and ultraviolet television for velocity and SO2 concentration, infrared laser-Doppler velocimetry for plume velocity, and visible laser radar for plume opacity.

Herget, W. F.↗

Vapor phase diamond growth technology

Ion beam deposition chambers used for carbon film generation were designed and constructed. Features of the developed equipment include: (1) carbon ion energies down to approx. 50 eV; (2) in suit surface monitoring with HEED; (3) provision for flooding the surface with ultraviolet radiation; (4) infrared laser heating of substrate; (5) residual gas monitoring; (6) provision for several source gases, including diborane for doping studies; and (7) growth from either hydrocarbon source gases or from carbon/argon arc sources. Various analytical techniques for characterization of from carbon/argon arc sources. Various analytical techniques for characterization of the ion deposited carbon films used to establish the nature of the chemical bonding and crystallographic structure of the films are discussed. These include: H2204/HN03 etch; resistance measurements; hardness tests; Fourier transform infrared spectroscopy; scanning auger microscopy; electron spectroscopy for chemical analysis; electron diffraction and energy dispersive X-ray analysis; electron energy loss spectroscopy; density measurements; secondary ion mass spectroscopy; high energy electron diffraction; and electron spin resonance. Results of the tests are summarized.

Angus, J. C.↗

Kinetics of the ClO + NO2 + M reaction

The ClO + NO2 + M reaction has been studied with two techniques: Fourier transform infrared spectroscopy of the products, and flash photolysis-ultraviolet absorption to monitor the decay of ClO in excess NO2. The measured third-order rate constant is 1.5 x 10 to the -31st cm to the 6th/molecule-squared per sec at 298 K with M = N2, in good agreement with previous literature values, but the rate constant appears to decrease by up to a factor of three in the presence of increasing amounts of OClO. For the infrared studies a stoichiometric mixture of ClO and NO2 was prepared in a flow system by mixing NO with OClO; at least as much NO2 as ClONO2 was produced under a variety of experimental conditions. These two sets of results are incompatible with the assumption made in previous kinetic studies that ClONO2 is the only recombination product; other isomers such as OClONO or ClOONO are likely to be formed three to four times faster. These results imply that potential stratospheric ozone depletion due to chlorofluoromethanes may be even larger than previously thought.

Molina, M. J.↗

Dynamic mechanical characterization of cure of a polyimide-graphite fiber composite (PMR 15/Celion 6000)

Dynamic mechanical studies of thermosetting PMR 15 polyimide/Celion 6000 composites were used to characterize cure behavior. Variation in composite shear modulus with cure time for laminates partially cured under 3.45 MPa pressure was compared with that of laminates fully cured under pressure to select a partially cured system whose behavior corresponded with that of the pressure-cured composites. An empirical kinetic model was developed that relates relative composite shear moduli to cure time and temperature. This model, coupled with standard statistical techniques, was used in the determination of an overall activation energy, E = 145 kj/mole (35 kcal/mole) and order of reaction, n, for the cure reaction(s). The empirical relationship defining dynamic modulus as a function of time and temperature remained linear well into the glassy region. Changes in dynamic glass-transition temperature and in the breadth of the transition peaks with cure time are discussed. Shear modulus and damping were found to be more sensitive measures of relative extent of cure than Fourier transform infrared spectroscopy.

Hurwitz, F. I.↗

Processing study of a polyimidesulfone adhesive

An adhesive bonding process cycle study was performed for a polyimidesulfone (PISO2) recently developed as a promising structural adhesive. The high molecular weight, linear aromatic system possesses properties which make it attractive as a processable, low-cost material for elevated temperature applications. The results of a study to better understand the parameters that affect the adhesive properties of the polymer for titanium alloy adherends are detailed. These include the tape preparation, the use of a primer, and press and simulated autoclave processing conditions. The polymer was characterized using Fourier Transform Infrared Spectroscopy, glass transition temperature determination, flow measurements, and weight loss measurements. The adhesive's strength determined by lap shear strength tests was used to evaluate the effects of the bonding process variations. Higher lap shear strengths were obtained at room temperature when a primer (PISO2) was used; however, the results were the same at 232 C (450 F) with or without a primer. The use of a vacuum (simulated autoclave cycle) during titanium bonding produced similar lap shear strengths to those specimens bonded without a vacuum.

Progar, D. J.↗

Resin characterization in cured graphite fiber reinforced composites using diffuse reflectance-FTIR

The feasibility of using diffuse reflectance in combination with Fourier transform infrared spectroscopy to obtain information on cured graphite fiber reinforced polymeric matrix resin composites was investigated. Several graphite/epoxy, polysulfone, and polyimide composites exposed to thermal or radiation environments were examined. An experimental polyimide-sulfone adhesive tape was also studied during processing. In each case, significant changes in resin molecular structure was observed due to environmental exposure. These changes in molecular structure were correlated with previously observed changes in material properties providing new insights into material behavior.

Young, P. R.↗

Processing study of a high temperature adhesive

An adhesive-bonding process cycle study was performed for a polyimidesulphone. The high molecular weight, linear aromatic system possesses properties which make it attractive as a processable, low-cost material for elevated temperature applications. The results of a study to better understand the parameters that affect the adhesive properties of the polymer for titanium alloy adherends are presented. These include the tape preparation, the use of a primer and press and simulated autoclave processing conditions. The polymer was characterized using Fourier transform infrared spectroscopy, glass transition temperature determination, flow measurements, and weight loss measurements. The lap shear strength of the adhesive was used to evaluate the effects of the bonding process variations.

Progar, D. J.↗

Matrix Resin Characterization in Cured Graphite Composites Using Diffuse Reflectance-Ftir

The chemical characterization of cured graphite fiber reinforced polymer matrix composites is complicated by the fact that the resins are insoluble and the composites are apaque. Standard analyses which depend either on the ability to dissolve the sample or to detect transmitted radiation are impossible. As a result, data reported on environmentally exposed composites primarily concern macroscopic information such as weight loss or changes in selected mechanical properties. Diffuse reflectance in combination with fourier transform infrared spectroscopy was developed to gain a basic chemical understanding of composite and adhesive behavior. Several composite and adhesive materials were characterized before and after environmental exposure. In each case significant changes in resin molecular structure were observed and correlated with changes in mechanical properties, providing new insights into material performance.

Young, P. R.↗

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

Silane primers for use as thermal protection on external tanks were subjected to various analytic techniques to determine the most effective testing method for silane lot evaluation. The analytic methods included high performance liquid chromatography, gas chromatography, thermogravimetry (TGA), and fourier transform infrared spectroscopy (FTIR). It is suggested that FTIR be used as the method for silane lot evaluation. Chromatograms, TGA profiles, bar graphs showing IR absorbances, and FTIR spectra are presented.

Mikes, F.↗