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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

The Infrared Spectroscopy of Equilibrium Mixtures of Vapor-Phase Water and Hydrogen Fluoride

Hydrogen fluoride readily associates with water vapor in the air to form the H 2 O-HF complex, which has optical absorption properties that are different from those of unassociated hydrogen fluoride. Consequently, to accurately quantify the total amount of hydrogen fluoride coming from an industrial stack or vent, for example, requires that the complexed amount of hydrogen fluoride be accounted for. To do this, the equilibrium constant for the association reaction is needed. Using statistical mechanical methods, Adebayo and coworkers [Adebayo SLA, AC Legon and DJ Millen. 1991. J. Chem. Soc. Faraday Trans. 87:443-447.] made an estimate of this equilibrium constant based on measured and estimated spectroscopic values for the complex. This value is K eq = 84(18) but has never been confirmed experimentally. In the research described herein, we have measured the equilibrium constant for the formation of H 2 O-HF by monitoring the decrease in the infrared absorption features of water vapor and hydrogen fluoride in mixtures of these two vapors in a temperature-regulated cell. Our experimental values for K eq at 25 °C, based on the diminution of the water vapor and HF transitions, are 77(46) and 51(24), respectively. The decay of the spectral features continues long after (hours) the two vapors are mixed in the gas cell. This suggests that other reactions (the growth of a film of hydrofluoric acid, perhaps) are taking place. While the experimental results agree reasonably well with the calculated equilibrium value of Adebayo et al., further improvements in experimental and analysis techniques are needed to reduce the uncertainties in the experimental results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2012

Rugged, Portable, Real-Time Optical Gaseous Analyzer for Hydrogen Fluoride

Hydrogen fluoride (HF) is a primary evolved combustion product of fluorinated and perfluorinated hydrocarbons. HF is produced during combustion by the presence of impurities and hydrogen- containing polymers including polyimides. This effect is especially dangerous in closed occupied volumes like spacecraft and submarines. In these systems, combinations of perfluorinated hydrocarbons and polyimides are used for insulating wiring. HF is both highly toxic and short-lived in closed environments due to its reactivity. The high reactivity also makes HF sampling problematic. An infrared optical sensor can detect promptly evolving HF with minimal sampling requirements, while providing both high sensitivity and high specificity. A rugged optical path length enhancement architecture enables both high HF sensitivity and rapid environmental sampling with minimal gaseous contact with the low-reactivity sensor surfaces. The inert optical sample cell, combined with infrared semiconductor lasers, is joined with an analog and digital electronic control architecture that allows for ruggedness and compactness. The combination provides both portability and battery operation on a simple camcorder battery for up to eight hours. Optical detection of gaseous HF is confounded by the need for rapid sampling with minimal contact between the sensor and the environmental sample. A sensor is required that must simultaneously provide the required sub-parts-permillion detection limits, but with the high specificity and selectivity expected of optical absorption techniques. It should also be rugged and compact for compatibility with operation onboard spacecraft and submarines. A new optical cell has been developed for which environmental sampling is accomplished by simply traversing the few mm-thick cell walls into an open volume where the measurement is made. A small, low-power fan or vacuum pump may be used to push or pull the gaseous sample into the sample volume for a response time of a few seconds. The optical cell simultaneously provides for an enhanced optical interaction path length between the environmental sample and the infrared laser. Further, the optical cell itself is comprised of inert materials that render it immune to attack by HF. In some cases, the sensor may be configured so that the optoelectronic devices themselves are protected and isolated from HF by the optical cell. The optical sample cell is combined with custom-developed analog and digital control electronics that provide rugged, compact operation on a platform that can run on a camcorder battery. The sensor is inert with respect to acidic gases like HF, while providing the required sensitivity, selectivity, and response time. Certain types of combustion events evolve copious amounts of HF, very little of other gases typically associated with combustion (e.g., carbon monoxide), and very low levels of aerosols and particulates (which confound traditional smoke detectors). The new sensor platform could warn occupants early enough to take the necessary countermeasures.

Pilgrim, Jeffrey↗
DOE OSTI2015

Hydrogen desorption kinetics for aqueous hydrogen fluoride and remote hydrogen plasma processed silicon (001) surfaces

The desorption kinetics of molecular hydrogen (H{sub 2}) from silicon (001) surfaces exposed to aqueous hydrogen fluoride and remote hydrogen plasmas were examined using temperature programmed desorption. Multiple H{sub 2} desorption states were observed and attributed to surface monohydride (SiH), di/trihydride (SiH{sub 2/3}), and hydroxide (SiOH) species, subsurface hydrogen trapped at defects, and hydrogen evolved during the desorption of surface oxides. The observed surface hydride species were dependent on the surface temperature during hydrogen plasma exposure with mono, di, and trihydride species being observed after low temperature exposure (150 °C), while predominantly monohydride species were observed after higher temperature exposure (450 °C). The ratio of surface versus subsurface H{sub 2} desorption was also found to be dependent on the substrate temperature with 150 °C remote hydrogen plasma exposure generally leading to more H{sub 2} evolved from subsurface states and 450 °C exposure leading to more H{sub 2} desorption from surface SiH{sub x} species. Additional surface desorption states were observed, which were attributed to H{sub 2} desorption from Si (111) facets formed as a result of surface etching by the remote hydrogen plasma or aqueous hydrogen fluoride treatment. The kinetics of surface H{sub 2} desorption were found to be in excellent agreement with prior investigations of silicon surfaces exposed to thermally generated atomic hydrogen.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Hydrogen desorption from hydrogen fluoride and remote hydrogen plasma cleaned silicon carbide (0001) surfaces

Due to the extreme chemical inertness of silicon carbide (SiC), in-situ thermal desorption is commonly utilized as a means to remove surface contamination prior to initiating critical semiconductor processing steps such as epitaxy, gate dielectric formation, and contact metallization. In-situ thermal desorption and silicon sublimation has also recently become a popular method for epitaxial growth of mono and few layer graphene. Accordingly, numerous thermal desorption experiments of various processed silicon carbide surfaces have been performed, but have ignored the presence of hydrogen, which is ubiquitous throughout semiconductor processing. In this regard, the authors have performed a combined temperature programmed desorption (TPD) and x-ray photoelectron spectroscopy (XPS) investigation of the desorption of molecular hydrogen (H{sub 2}) and various other oxygen, carbon, and fluorine related species from ex-situ aqueous hydrogen fluoride (HF) and in-situ remote hydrogen plasma cleaned 6H-SiC (0001) surfaces. Using XPS, the authors observed that temperatures on the order of 700–1000 °C are needed to fully desorb C-H, C-O and Si-O species from these surfaces. However, using TPD, the authors observed H{sub 2} desorption at both lower temperatures (200–550 °C) as well as higher temperatures (>700 °C). The low temperature H{sub 2} desorption was deconvoluted into multiple desorption states that, based on similarities to H{sub 2} desorption from Si (111), were attributed to silicon mono, di, and trihydride surface species as well as hydrogen trapped by subsurface defects, steps, or dopants. The higher temperature H{sub 2} desorption was similarly attributed to H{sub 2} evolved from surface O-H groups at ∼750 °C as well as the liberation of H{sub 2} during Si-O desorption at temperatures >800 °C. These results indicate that while ex-situ aqueous HF processed 6H-SiC (0001) surfaces annealed at <700 °C remain terminated by some surface C–O and Si–O bonding, they may still exhibit significant chemical reactivity due to the creation of surface dangling bonds resulting from H{sub 2} desorption from previously undetected silicon hydride and surface hydroxide species.

36 MATERIALS SCIENCE↗
NASA NTRS1994

Southern hemisphere ground based measurements of Carbonyl Fluoride (COF2) and Hydrogen Fluoride (HF): Partitioning between Fluoride reservoir species

We report infrared ground based total column measurements of the stratospheric fluorine reservoir gases COF2 and HF above Lauder, New Zealand (45 deg S, 167.8 deg E) obtained between April 1993 and January 1994. The average retrieved COF2 and HF total columns are 2.81(+/- 0.56) x 10(exp 14) and 9.91(+/- 1.09) x 10(exp 14) molecules/sq cm respectively. The daily average COF2 and HF columns are correlated; this correlation is likely the result of dynamics. The average HF/COF2 column ratio on days with measurements of both HF and COF2 is 3.63 (+/- 0.55). Comparison of this ratio with model calculations implies that the quantum yield for COF2 photolysis is near unity. Our measured COF2 columns are higher than all previously reported values, but inconsistencies among the earlier measurements and uncertainty in the latitudinal gradient of the COF2 column preclude an accurate determination of the long-term COF2 trend.

Reisinger, Andreas R.↗
NASA NTRS2001

Ab Initio Calculations of Anharmonic Vibrational Spectroscopy for Hydrogen Fluoride (HF)n (n=3,4) and Mixed Hydrogen Fluoride/Water (HF)n(H20)n (n=1,2,4) Clusters

Anharmonic vibrational frequencies and intensities are computed for hydrogen fluoride clusters (HF)n with n=3,4 and mixed clusters of hydrogen fluoride with water (HF)n(H2O)n where n=1,2. For the (HF)4(H2O)4 complex, the vibrational spectra are calculated at the harmonic level, and anharmonic effects are estimated. Potential energy surfaces for these systems are obtained at the MP2/TZP level of electronic structure theory. Vibrational states are calculated from the potential surface points using the correlation-corrected vibrational self-consistent field (CC-VSCF) method. The method accounts for the anharmonicities and couplings between all vibrational modes and provides fairly accurate anharmonic vibrational spectra that can be directly compared with experimental results without a need for empirical scaling. For (HF)n, good agreement is found with experimental data. This agreement shows that the MP2 potential surfaces for these systems are reasonably reliable. The accuracy is best for the stiff intramolecular modes, which indicates the validity of MP2 in describing coupling between intramolecular and intermolecular degrees of freedom. For (HF)n(H2O)n experimental results are unavailable. The computed intramolecular frequencies show a strong dependence on cluster size. Intensity features are predicted for future experiments.

Chaban, Galina M.↗
NASA NTRS2002

Ab initio calculations of anharmonic vibrational spectroscopy for hydrogen fluoride (HF)n (n = 3, 4) and mixed hydrogen fluoride/water (HF)n(H2O)n (n = 1, 2, 4) clusters

Anharmonic vibrational frequencies and intensities are computed for hydrogen fluoride clusters (HF)n, with n = 3, 4 and mixed clusters of hydrogen fluoride with water (HF)n(H2O)n where n = 1, 2. For the (HF)4(H2O)4 complex, the vibrational spectra are calculated at the harmonic level, and anharmonic effects are estimated. Potential energy surfaces for these systems are obtained at the MP2/TZP level of electronic structure theory. Vibrational states are calculated from the potential surface points using the correlation-corrected vibrational self-consistent field method. The method accounts for the anharmonicities and couplings between all vibrational modes and provides fairly accurate anharmonic vibrational spectra that can be directly compared with experimental results without a need for empirical scaling. For (HF)n, good agreement is found with experimental data. This agreement shows that the Moller-Plesset (MP2) potential surfaces for these systems are reasonably reliable. The accuracy is best for the stiff intramolecular modes, which indicates the validity of MP2 in describing coupling between intramolecular and intermolecular degrees of freedom. For (HF)n(H2O)n experimental results are unavailable. The computed intramolecular frequencies show a strong dependence on cluster size. Intensity features are predicted for future experiments.

Water/chemistry↗
DOE OSTI2015

Atomic layer deposition of magnesium fluoride via bis(ethylcyclopentadienyl)magnesium and anhydrous hydrogen fluoride

A new process has been developed to deposit magnesium fluoride (MgF{sub 2}) thin films via atomic layer deposition (ALD) for use as optical coatings in the ultraviolet. MgF{sub 2} was deposited in a showerhead style ALD reactor using bis(ethylcyclopentadienyl)magnesium and anhydrous hydrogen fluoride (HF) as precursors at substrate temperatures from 100 to 250 °C. The use of HF was observed to result in improved morphology and reduced impurity content compared to other reported MgF{sub 2} ALD approaches that use metal fluoride precursors as the fluorine-containing chemistry. Characterization of these films has been performed using spectroscopic ellipsometry, atomic force microscopy, and x-ray photoelectron spectroscopy for material deposited on silicon substrates. Films at all substrate temperatures were transparent at wavelengths down to 190 nm and the low deposition temperature combined with low surface roughness makes these coatings good candidates for a variety of optical applications in the far ultraviolet.

36 MATERIALS SCIENCE↗
NASA NTRS1997

Discovery of Interstellar Hydrogen Fluoride

We report the first detection of interstellar hydrogen fluoride. Using the Long Wavelength Spectrometer of the Infrared Space Observatory (ISO), we have detected the 121.6973 micron J = 2-1 line of HF in absorption toward the far-infrared continuum source Sagittarius B2. The detection is statistically significant at the 13 sigma level. On the basis of our model for the excitation of HF in Sgr B2, the observed line equivalent width of 1.0 nm implies a hydrogen fluoride abundance of about 3 x 10 (exp -10) relative to H, If the elemental abundance of fluorine in Sgr B2 is the same as that in the solar system, then HF accounts for about 2% of the total number of fluorine nuclei. We expect hydrogen fluoride to be the dominant reservoir of gas-phase fluorine in Sgr B2, because it is formed rapidly in exothermic reactions of atomic fluorine with either water or molecular hydrogen; thus, the measured HF abundance suggests a substantial depletion of fluorine onto dust grains. Similar conclusions regarding depletion have previously been reached for the case of chlorine in dense interstellar clouds. We also find evidence at a lower level of statistical significance (about 5 sigma) for an emission feature at the expected position of the 4(sub 32)-4(sub 23) 121.7219 micron line of water. The emission-line equivalent width of 0.5 mm for the water feature is consistent with the water abundance of 5 x 10(exp -6) relative to H, that has been inferred previously from observations of the hot core of Sgr B2.

Neufeld, David A.↗
NASA NTRS1997

Discovery of Interstellar Hydrogen Fluoride

We report the first detection of interstellar hydrogen fluoride. Using the Long Wavelength Spectrometer of the Infrared Space Observatory (ISO), we have detected the 121.6973 micron J = 2-1 line of HF in absorption toward the far-infrared continuum source Sagittarius B2. The detection is statistically significant at the 13 sigma level. On the basis of our model for the excitation of HF in Sgr B2, the observed line equivalent width of 1.0 nm implies a hydrogen fluoride abundance of approximately 3 x 10(exp -10) relative to H2. If the elemental abundance of fluorine in Sgr B2 is the same as that in the solar system, then HF accounts for approximately 2% of the total number of fluorine nuclei. We expect hydrogen fluoride to be the dominant reservoir of gas-phase fluorine in Sgr B2, because it is formed rapidly in exothermic reactions of atomic fluorine with either water or molecular hydrogen; thus, the measured HF abundance suggests a substantial depletion of fluorine onto dust grains. Similar conclusions regarding depletion have previously been reached for the case of chlorine in dense interstellar clouds. We also find evidence at a lower level of statistical significance (approximately 5 sigma) for an emission feature at the expected position of the 4(sub 32)-4(sub 23) 121.7219 micron line of water. The emission-line equivalent width of 0.5 nm for the water feature is consistent with the water abundance of 5 x 10(exp -6) relative to H2 that has been inferred previously from observations of the hot core of Sgr B2.

Neufeld, David A.↗
DOE OSTI2018

Chemical Conversion of Anhydrous Hydrogen Fluoride for Safe Disposal

A procedure for the safe conversion of a small (~ 1 gram) quantity of anhydrous hydrogen fluoride to calcium fluoride is described. The purpose of the conversion is to put the toxic, corrosive, gaseous compound into a chemical form that is a less toxic solid (calcium fluoride) and easier to dispose of. The hydrogen fluoride, which was contained in a 50 cc metal sample cylinder, was drawn by a small mechanical vacuum pump through an all-metal gas manifold and into a metal trap containing alternating layers of calcium oxide powder and Teflon turnings. The anhydrous hydrogen fluoride reacts with the calcium oxide to produce calcium fluoride and water vapor. Because some of the calcium oxide powder was drawn out of the trap and into the vacuum tubing, it was not possible to quantify the amount of anhydrous hydrogen fluoride converted to calcium fluoride. However, it was noted that there was a temperature rise in the trap when the gas was flowing through it, and no HF gas was detected at the vacuum pump exhaust at this time using a colorimetric Dräger tube. The trap was sealed and disposed of as solid chemical waste.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2014

Quantum theory of atoms in molecules/charge-charge flux-dipole flux models for fundamental vibrational intensity changes on H-bond formation of water and hydrogen fluoride

The Quantum Theory of Atoms In Molecules/Charge-Charge Flux-Dipole Flux (QTAIM/CCFDF) model has been used to investigate the electronic structure variations associated with intensity changes on dimerization for the vibrations of the water and hydrogen fluoride dimers as well as in the water-hydrogen fluoride complex. QCISD/cc-pVTZ wave functions applied in the QTAIM/CCFDF model accurately provide the fundamental band intensities of water and its dimer predicting symmetric and antisymmetric stretching intensity increases for the donor unit of 159 and 47 km mol{sup −1} on H-bond formation compared with the experimental values of 141 and 53 km mol{sup −1}. The symmetric stretching of the proton donor water in the dimer has intensity contributions parallel and perpendicular to its C{sub 2v} axis. The largest calculated increase of 107 km mol{sup −1} is perpendicular to this axis and owes to equilibrium atomic charge displacements on vibration. Charge flux decreases occurring parallel and perpendicular to this axis result in 42 and 40 km mol{sup −1} total intensity increases for the symmetric and antisymmetric stretches, respectively. These decreases in charge flux result in intensity enhancements because of the interaction contributions to the intensities between charge flux and the other quantities. Even though dipole flux contributions are much smaller than the charge and charge flux ones in both monomer and dimer water they are important for calculating the total intensity values for their stretching vibrations since the charge-charge flux interaction term cancels the charge and charge flux contributions. The QTAIM/CCFDF hydrogen-bonded stretching intensity strengthening of 321 km mol{sup −1} on HF dimerization and 592 km mol{sup −1} on HF:H{sub 2}O complexation can essentially be explained by charge, charge flux and their interaction cross term. Atomic contributions to the intensities are also calculated. The bridge hydrogen atomic contributions alone explain 145, 237, and 574 km mol{sup −1} of the H-bond stretching intensity enhancements for the water and HF dimers and their heterodimer compared with total increments of 149, 321, and 592 km mol{sup −1}, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1990

Intercomparison of measurements of stratospheric hydrogen fluoride

Observations of the vertical profile of hydrogen fluoride (HF) vapor in the stratosphere and of the vertical column amounts of HF above certain altitudes were made using a variety of spectroscopic instruments in the 1982 and 1983 Balloon Intercomparison Campaigns. Both emission instruments working in the far-infrared spectral region and absorption instruments using solar occultation in the 2.5-micron region were employed. No systematic differences were seen in results from the two spectral regions. A mean profile from 20 - 45 km is presented, with uncertainties ranging from 20 to 50 percent. Total columns measured from ground and from 12 km are consistent with the profile if the mixing ratio for HF is small in the troposphere and low stratosphere.

Mankin, William G.↗
DOE OSTI2012

HYDROGEN FLUORIDE IN HIGH-MASS STAR-FORMING REGIONS

Hydrogen fluoride (HF) has been established to be an excellent tracer of molecular hydrogen in diffuse clouds. In denser environments, however, the HF abundance has been shown to be approximately two orders of magnitude lower. We present Herschel/HIFI observations of HF J = 1-0 toward two high-mass star formation sites, NGC 6334 I and AFGL 2591. In NGC 6334 I the HF line is seen in absorption in foreground clouds and the source itself, while in AFGL 2591 HF is partially in emission. We find an HF abundance with respect to H{sub 2} of 1.5 Multiplication-Sign 10{sup -8} in the diffuse foreground clouds, whereas in the denser parts of NGC 6334 I we derive a lower limit on the HF abundance of 5 Multiplication-Sign 10{sup -10}. Lower HF abundances in dense clouds are most likely caused by freezeout of HF molecules onto dust grains in high-density gas. In AFGL 2591, the view of the hot core is obstructed by absorption in the massive outflow, in which HF is also very abundant (3.6 Multiplication-Sign 10{sup -8}) due to the desorption by sputtering. These observations provide further evidence that the chemistry of interstellar fluorine is controlled by freezeout onto gas grains.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2014

Hydrogen fluoride toward luminous nearby galaxies: NGC 253 and NGC 4945

We present the detection of hydrogen fluoride (HF) in two luminous nearby galaxies, NGC 253 and NGC 4945 using the Heterodyne Instrument for the Far-Infrared on board the Herschel Space Observatory. The HF line toward NGC 253 has a P-Cygni profile, while an asymmetric absorption profile is seen toward NGC 4945. The P-Cygni profile in NGC 253 suggests an outflow of molecular gas with a mass of M(H{sub 2}){sub out} ∼ 1 × 10{sup 7} M {sub ☉} and an outflow rate as large as M-dot ∼6.4 M {sub ☉} yr{sup –1}. In the case of NGC 4945, the axisymmetric velocity components in the HF line profile are compatible with the interpretation of a fast-rotating nuclear ring surrounding the nucleus and the presence of inflowing gas. The gas falls into the nucleus with an inflow rate of ≤1.2 M {sub ☉} yr{sup –1}, inside an inner radius of ≤200 pc. The gas accretion rate to the central active galactic nucleus is much smaller, suggesting that the inflow may be triggering a nuclear starburst. From these results, the HF J = 1-0 line is seen to provide an important probe of the kinematics of absorbing material along the sight-line to nearby galaxies with bright dust continuum and a promising new tracer of molecular gas in high-redshift galaxies.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1994

Observations of stratospheric hydrogen fluoride by halogen occultation experiment (HALOE)

The Halogen Occultation Experiment (HALOE) Hydrogen Fluoride (HF) channel on the Upper Atmospheric Research Satellite (UARS) is providing the first global measurements of stratospheric HF, the dominant flourine reservoir in the atmosphere. This paper describes the latitudinal and seasonal variations of HALOE-observed HF in terms of vertical profiles, altitude/latitude cross sections, and column abundances. The HF global distribution shows a 'tracerlike' structure and its column amount increases with latitude, in agreement with previous aircraft measurements of the HF column amount. A comparison between the HALOE HF column above 20 km and the ATMOS 1985 measurements is used to estimate the annual rate of increase of stratospheric HF. Exponential rates of 4.9-6.6%/yr and linear growth rates of 6-8.6%/yr in 1985 and 4.3-5.5%/yr in 1992-1993 are found. HALOE HF measurements during the 1993 Antarctic spring are briefly described. This species behaves like a conserved tracer and its distribution shows an area of enhanced mixing ratios correlated with the polar vortex that has a clear latitude boundary. Finally, simulated HF distributions by the National Center for Atmospheric Research (NCAR) two-dimensional model are used to compare with HALOE observations of HF. Reasonable agreements in the global structure and the absolute amount of HF are found. The differences between the model and the observed results indicate the need for improving treatment of atmospheric dynamics and fluorine-related chemical parameters in the model simulations.

Luo, M.↗
DOE OSTI2011

DISCOVERY OF HYDROGEN FLUORIDE IN THE CLOVERLEAF QUASAR AT z = 2.56

We report the first detection of hydrogen fluoride (HF) toward a high-redshift quasar. Using the Caltech Submillimeter Observatory, we detect the HF J = 1-0 transition in absorption toward the Cloverleaf, a broad absorption line quasi-stellar object at z = 2.56. The detection is statistically significant at the {approx}6{sigma} level. We estimate a lower limit of 4 Multiplication-Sign 10{sup 14} cm{sup -2} for the HF column density and using a previous estimate of the hydrogen column density, we obtain a lower limit of 1.7 Multiplication-Sign 10{sup -9} for the HF abundance. This value suggests that, assuming a Galactic N(HF)/N{sub H} ratio, HF accounts for at least {approx}10% of the fluorine in the gas phase along the line of sight to the Cloverleaf quasar. This observation corroborates the prediction that HF should be a good probe of the molecular gas at high redshift. Measurements of the HF abundance as a function of redshift are urgently needed to better constrain the fluorine nucleosynthesis mechanism(s).

79 ASTRONOMY AND ASTROPHYSICS↗