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The experimental apparatus used in the investigation consisted of an ultrahigh-vacuum chamber, a triple-grid, a microwave-excited resonance lamp, and an electron energy analyzer. The chemical nature of the chemisorbed species was studied, taking into account the energy distribution of photoemitted electrons, work function determinations, and low-energy electron diffraction patterns.
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A thermoplastic rubber is made from a mixture of between about 10 percent and about 50 percent of asphalt, between about 5 percent and about 30 percent fluxing oil, and between about 35 percent and about 70 percent of a copolymer of polyethylene and vinyl acetate.
The rate constant for the H+C2H4 reaction has been measured as a function of temperature. Experiments were performed with high pressures of Ar heat bath gas at seven temperatures from 198 to 320 K with the flash photolysis-resonance fluorescence (FP-RF) technique. Pressures were chosen so as to isolate the addition rate constant k1. The results are well represented by an Arrhenius expression. The results are compared with other studies and are theoretically discussed.
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The secondary electron emission coefficient was measured for a charged polymer (FEP-Teflon) with normally and obliquely incident primary electrons. Theories of secondary emission are reviewed and the experimental data is compared to these theories. Results were obtained for angles of incidence up to 60 deg in normal electric fields of 1500 V/mm. Additional measurements in the range from 50 to 70 deg were made in regions where the normal and tangential fields were approximately equal. The initial input angles and measured output point of the electron beam could be analyzed with computer simulations in order to determine the field within the chamber. When the field is known, the trajectories can be calculated for impacting electrons having various energies and angles of incidence. There was close agreement between the experimental results and the commonly assumed theoretical model in the presence of normal electric fields for angles of incidence up to 60 deg. High angle results obtained in the presence of tangential electric fields did not agree with the theoretical models.
The rates of hydrogen abstraction by peroxy radicals were proven to be too slow for significant oxidation of the alkane substrate to be important. The numerical procedure, independent of our particular data base was verified by reproducing concentration time profiles for a model reaction set describing the cesium flare system in the upper atmosphere. Simulation was identical to that given in the literature. Experimental verification of the data base is to be attempted by weatherometry studies in the coming year. Work on the new diagnostic techniques was completed. The adapted automated viscometer was demonstrated to be an efficient and reliable tool for routine measurements of viscosity (molecular weight) changes in solid samples after batch solutions have been made up. The laser photolysis GC method for monitoring extremely low levels of oxidation in polymers proved to be impractical because the yields of carbon monoxide were too low for quantification. Much progress was made with the computer model. The reaction matrix was completely revised, resulting in a new scheme of 31 reactions and time, lifetimes in excess of ten years. The results to date lead us to some tentative observations.
A computer model which simulates, in principle, the chemical changes in the photooxidation of hydrocarbons using as input data a set of elementary reactions, corresponding kinetic rate data and appropriate initial conditions was developed. The Model was refined and exploited to examine more closely the photooxidation and photostabilization of a hydrocarbon polymer. The results lead to the following observations. (1) The time to failure, tau sub f (chosen as the level of 5% C-H bond oxidation which is within the range anticipated for marked change in mechanical properties) varies as the inverse square root of the light intensity. However, tau sub f is almost unaffected by both the photoinitiator type and concentration. (2) The time to failure decreases with the rate of abstraction of C-H by peroxy radicals but increases with the rate of bimolecular radical termination controlled by diffusion. (3) Of the various stabilization mechanisms considered, the trapping of peroxy radicals is distinctly the most effective, although the concommitant decomposition of hydroperoxide is also desirable.
A computer model was developed which can generate realistic concentration versus time profiles of the chemical species formed during photooxidation of hydrocarbon polymers using as input data a set of elementary reactions with corresponding rate constants and initial conditions. The results of computer simulation have been shown to be consistent with the general experimental observations of the photooxidation of polyethylene exposed to sunlight at ambient temperatures. The useful lifetime (5% oxidation) of the unstabilized polyethylene is predicted to vary from a few months in hot weather (100 F) to almost two years in cool weather (45 F) with an apparent net activation energy of 10 kcal/mol. Modelling studies of alternate mechanisms for stabilization of clear, amorphous, linear polyethylene suggest that the optimum stabilizer would be a molecularly dispensed additive in very low concentration which can trap peroxy radicals and also decompose hydroperoxides.
A test method is described for predicting the long-time survivability of elastomers in hydrazine under dynamic stressing conditions. The method selected is based upon the existence and approximate invariance of a 'physical property surface' relating the mechanical response of the elastomer in terms of stress, strain, time, and temperature. The property surface was generated for two selected elastomers (EPT-10 and AF-E-332). A novel carousel testing tank was designed to allow sequential testing of eight tensile specimens immersed in liquid hydrazine within a constant-temperature water bath. The test procedure and data reduction methods used to generate the property surface are described. The utility and validity of these results applied to fatigue and flexure loading to these elastomeric materials over long-time periods are discussed.
New results have been obtained which contribute to the understanding of hydrocarbon reactions on the surface of highly dispersed metal systems. Small particle of Pd were grown by electron beam evaporation on cleavage planes of high purity natural mica under ultrahigh vacuum conditions. Samples were subsequently characterized by transmission electron microscopy. Average particle sizes ranged from about 1 to 10 nm diameter. The chemisoption and decomposition of C2H4 on the Pd particles was studied using Auger electron spectroscopy and flash thermal desorption. It is shown that (a) C2H4 decomposes on Pd particles at room temperature, (b) specific surface sites are causing decomposition, and (c) the proportion of such active sites is significantly greater for the smaller metal particles. This enhanced reactivity may be due to an increase in the density of step, corner, and edge sites with a decrease in particle size.
Five coaxial tubular opposed jet burners (OJBs) with tube diameter D(T) of 1.8-10 mm and 5 mm conical nozzles were used to form dish-shaped counterflow diffusion flames centered by opposing laminar jets of nitrogen and hydrocarbon-diluted H2 versus air in an argon-purged chamber at 1 atm. Area-averaged air jet velocities at blowoff of the central flame, U(air), characterized extinction of the airside flame as functions of input H2 concentration on the fuelside. A master plot of extensive U(air) data at blowoff versus D(T) shows that U(air) varies linearly with D(T). This and other data sets are used to find that nozzle OJB results for U(air)/diameter average 4.24 + or - 0.28 times larger than tubular OJB results for the same fuel compositions. Critical radial velocity gradients consistent with one-dimensional stagnation point boundary theory and with plug flow inputs are estimated. The results compare favorably with published numerical results based only on potential flow.
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The testing and development of existing global and detailed chemical kinetic models for soot formation requires measurements of soot and radical concentrations in flames. A clearer understanding of soot particle inception relies upon the evaluation and refinement of these models in comparison with such measurements. We present measurements of soot formation and hydroxyl (OH) concentration in sequences of flat premixed atmospheric-pressure C2H4/O2/N2 flames and 80-torr C2H4/O2 flames for a unique range of equivalence ratios bracketting the critical equivalence ratio (phi(sub c)) and extending to more heavily sooting conditions. Soot volume fraction and number density profiles are measured using a laser scattering-extinction apparatus capable of resolving a 0.1 percent absorption. Hydroxyl number density profiles are measured using laser-induced fluorescence (LIF) with broadband detection. Temperature profiles are obtained from Rayleigh scattering measurements. The relative volume fraction and number density profiles of the richer sooting flames exhibit the expected trends in soot formation. In near-phi(sub c) visibility sooting flames, particle scattering and extinction are not detected, but an LIF signal due to polycyclic aromatic hydrocarbons (PAH's) can be detected upon excitation with an argon-ion laser. A linear correlation between the argon-ion LIF and the soot volume fraction implies a common mechanistic source for the growth of PAH's and soot particles. The peak OH number density in both the atmospheric and 80-torr flames declines with increasing equivalence ratio, but the profile shape remains unchanged in the transition to sooting, implying that the primary reaction pathways for OH remain unchanged over this transition. Chemical kinetic modeling is demonstrated by comparing predictions using two current reaction mechanisms with the atmospheric flame data. The measured and predicted OH number density profiles show good agreement. The predicted benzene number density profiles correlate with the measured trends in soot formation, although anomalies in the benzene profiles for the richer and cooler sooting flames suggest a need for the inclusion of benzene oxidation reactions.
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