Mechanism of the atmospheric interaction with the fatigue of metals Summary report, 4 Aug. 1965 - 1 Sep. 1966
Effects of temperature, test interruption, and residual gas pressure on fatigue properties of aluminum
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Effects of temperature, test interruption, and residual gas pressure on fatigue properties of aluminum
Computer program for interpretation of residual gas analyzer mass spectra, considering vacuum environmental testing of spacecraft
Graphite properties in high and ultrahigh vacuum, suggesting use as electrode material in vacuum gages and residual gas analyzers
The V-3 contamination test was designed to measure the degree to which the vacuum facility might be a source of contamination. One test measurement subsystem consisting of a quadrupole residual gas analyzer, a quartz crystal microbalance, and an ion gage is described.
An experimental program was undertaken in which mass accretion rates, as determined by a liquid nitrogen cooled quartz crystal microbalance, were compared with the mass flux rates, as determined by both a cycloidal type and a quadrupole type residual gas analyzer for five simple materials. The data indicate a high degree of correlation between these instruments insofar as the shape of the curves. There are large variations however among the absolute values.
A commercial quadrupole residual gas analyzer system has been upgraded for operation at extended cable lengths. Operation inside a vacuum chamber for the standard quadrupole nude head is limited to approximately 2 m from its externally located rf/dc generator because of the detuning of the rf oscillator circuits by the coaxial cable reactance. The advance of long distance remote operation inside a vacuum chamber for distances of 45 and 60 m was made possible without altering the quadrupole's rf/dc generator circuit by employing an rf link to drive the quadrupole rods. Applications of the system have been accomplished for in situ space simulation thermal/vacuum testing of sophisticated payloads.
A commercial quadrupole mass spectrometer (residual gas analyzer, RGA) system has been modified to operate at large separations of its electronics console and sensing head. The methods implemented have made practical applications, as well as operation, of such a system possible for the first time. This advance was stimulated by a need for placing sensors at remote (45 or 60 m) chamber locations for space simulation testing of orbital flight spacecraft. Emphasis is placed on instrument functional requirements and describing the hardware changes and adjustment techniques necessary to assure operation at the extended cable lengths.
Direct evidence is reported for the simultaneous occurrence of Ostwald ripening and short-distance cluster mobility during annealing of discontinuous metal films on clean amorphous substrates. The annealing characteristics of very thin particulate deposits of silver on amorphized clean surfaces of single crystalline thin graphite substrates were studied by in-situ transmission electron microscopy (TEM) under controlled environmental conditions (residual gas pressure of 10 to the minus 9th power torr) in the temperature range from 25 to 450 C. Sputter cleaning of the substrate surface, metal deposition, and annealing were monitored by TEM observation. Pseudostereographic presentation of micrographs in different annealing stages, the observation of the annealing behavior at cast shadow edges, and measurements with an electronic image analyzing system were employed to aid the visual perception and the analysis of changes in deposit structure recorded during annealing. Slow Ostwald ripening was found to occur in the entire temperature range, but the overriding surface transport mechanism was short-distance cluster mobility.
The dark and photoconductivities of four high voltage spacecraft insulators, Kapton-H, FEP Teflon, Parylene, and fused quartz, were studied under a variety of conditions intended to simulate a space environment. All measurements were made in a vacuum of less than .00001 torr while the temperature was varied from 22 C to 100 C. Some of the samples used employed conventional deposited metal electrodes--others employed electrodes composed either of an electron beam or a plasma formed by ionization of the residual gas in the test chamber. Test results show: (1) Kapton had unusual conduction properties; it conductivity decreased by more than an order of magnitude when heated at 100 C in a vacuum, but ultimately attained a stable and reproducible value. (2) Both Teflon and fused quartz had high dark resistivities but low photoresistivities when exposed to UV. Optical-density measurements revealed that both materials transmitted UV with little attenuation. (3) Parylene was found to have a low but relatively stable resistivity--comparatively minor changes occurred upon heating or illuminating the sample. Optical-density measurements showed that Parylene was absorbent in the UV and would prevent photoemission from the metal electrode on the back surface.
Residual gas analysis techniques were employed to measure the moisture in sealed hybrid packages as a function of substrate attach material, vacuum bake time and sequence, and sealing procedure. It is shown that when room atmospheric exposure is eliminated following the vacuum bakeout moisture levels of less than 1000 ppm may be achieved for modest bake times and solder substrate attach techniques. Suitable moisture levels were achieved for epoxy attached substrates only when seam sealing procedures were employed.
An ion tracking system utilizing a single detector was designed to resolve two dimensional potential distributions in a vacuum. The ion detector consisted of a continuous dynode electron multiplier tube mounted behind a series of aperture plates. The detector was located on a track below a wedge shaped structure used to produce the desired potential distribution. A 150 volt electron beam aimed at selected regions, ionized the residual gas in the chamber. The ions were ejected from their source points by electrostatic forces causing them to drift downward toward the detector. Measurements of particle energy, detector position, and entry angle of the incoming particle flux were used to initialize a computer trajectory-tracing program. The program assumes a known theoretically calculated potential distribution near the wedge for computation of particle trajectories, providing a basis for evaluating the data. Special attention was given to characterization of the ion detector.
These 10 surface-analysis tests can be run without breaking vacuum: secondary-ion mass spectroscopy, ion-scattering spectroscopy, electron-stimulated desorption, residual-gas analysis, auger electron spectroscopy, x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, characteristic-electron energy-loss spectroscopy, scanning electron microscope, scanning low-energy electron probe. Quadruple mass spectrometer, used in first 4 tests, serves as electron transfer lens in last 6 tests.
Metal outgassing currently limits the pressures attained in vacuum chambers. The dominant residual gas in a carefully degassed metal system is usually hydrogen. The atomic hydrogen within bulk metals could be removed by diffusion processes if surface effects did not interfere. It is proposed that removing the surface hydrogen during vacuum bakeout by continuous electron bombardment (or similar irradiation) would allow the diffusion to proceed and lead to lower outgassing rates and operating pressures.
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.
An extensive laboratory test program was performed to characterize outgassing of five satellite materials. The materials were Chemglaze Z-306 over 9922 primer, M-773 adhesive, multilayer insulation, polyurethane foam, and silverized Teflon. The souces were prepared to the specifications of a typical satellite program. Dynamic thermogravimetric mass loss characteristics of these five materials were obtained in vacuum with a beam microbalance. The temperature of the material was linearly raised from 25 C to over 650 C while monitoring the mass loss, rate of mass loss, temperature, and the composition of the outgassed material by residual gas analysis. Isothermal source emission/capture coefficients/reemission parameters were obtained with an array of quartz crystal microbalances (QCM). A detailed test matrix in which the temperatures of the QCMs (-160 C, - 100 C, -40 C, and +10 C) and the source material (125 C, and 90 C, and 50 C) were varied was performed. The array of QCMs was also used to measure the spatial distribution of the source emission. The effects of vacuum ultraviolet radiation on the deposition and reemission parameters was determined.
Liquid hydrazine dissociated and residual gas removed to produce almost pure nitrogen. Nitrogen-generation module catalytically dissociates liquid hydrazine then dissociates and separates product gases to yield almost pure nitrogen.
Outgassing reduced in some but not all nonmetallic materials. Eleven polymeric materials tested by determining outgassing species as temperature of conditioned and unconditioned materials raised to 300 degrees C. Conditioning process consisted of vacuum bake for 24 hours at 80 degrees C in addition to usual cure. Baking did not change residual gas percentage of water molecules.
The Earth radiation budget components and dynamics and the interactions of this energy cycle, which influences our climate were investigated. The satellite package was subjected to space simulation testing. The size of the spacecraft dictated that the testing be conducted in the new BRUTUS Thermal Vacuum Facility. Computer aided control (CAC), quartz crystal microbalance (QCM), and residual gas analysis (RGA) monitoring are combined with rigid contamination control procedures to protect the flight hardware from anomalous and potentially destructive out of scope test environments.