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The scanning electron microscope (SEM) is considered as a tool for both failure analysis as well as device characterization. A survey is made of various operational SEM modes and their applicability to image processing methods on semiconductor devices.
A method of providing cathode redundancy which consists of two fixed cathodes and uses electromagnetic and/or electrostatic fields to direct the electron beam to the electron optical axis is presented, with application to the cathode system of the Scanning Electron Microscope and Particle Analyzer proposed for NASA's Mariner Mark II Comet Rendezvous/Asteroid Flyby projected for the 1990s. The symmetric double deflection system chosen has the optical property that the image of the effective electron source is formed above the magnet assembly near the apparent position of the effective source, and it makes the transverse positions of the electron sources independent of the electron beam energy. Good performance of the system is found, with the sample imaging resolution being the same as for the single-axis cathode.
Beam from either cathode electromagnetically aligned with exit port. Electron beam from either of two cathodes deflected by magnetic and electric fields to central axis. Mechanical alignment of beam easy because cathode axes, anode apertures, and electron trajectories coplanar. Applications where uninterrupted service needed: scanning electron microscopes, transmission electron microscopes, electron-beam lithography equipment, Auger instruments, and microfocused x-ray sources.
The Comet Rendezvous Asteroid Flyby Mission (CRAF) is described. After gravity assists from Venus and Earth, the spacecraft will fly by the asteroid 46 Hestia en route to a rendezvous with P/Tempel 2 in Nov. 1996, when the comet is near aphelion. The scientific experiments for the CRAF mission are: an imaging system; a visual and infrared mapping spectrometer; an infrared radiometer; a penetrator carrying a gamma-ray spectrometer, a scanning differential calorimeter and evolved gas analyzer, accelerometers, and temperature probes; a neutral gas and thermal ion mass spectrometer; a secondary ion mass spectrometer for analyzing dust, gas, and thermal ions; a scanning electron microscope and particle analyzer; an X-ray fluorescence and gas chromatographic analyzer for collected dust and ice samples; a dust counter and velocity analyzer; a retarding potential ion mass spectrometer; a supra-thermal ion mass spectrometer and electron analyzer; a magnetometer; and a coordinated radio, electron, and plasma wave analyzer.
An in situ fatigue loading stage inside a scanning electron microscope (SEM) was used to determine the fatigue crack growth behavior of a PWA 1480 single-crystal nickel-based superalloy. The loading stage permits real-time viewing of the fatigue damage processes at high magnification. The PWA 1480 single-crystal, single-edge notch specimens were tested with the load axis parallel to the (100) orientation. Two distinct fatigue failure mechanisms were identified. The crack growth rate differed substantially when the failure occurred on a single slip system in comparison to multislip system failure. Two processes by which crack branching is produced were identified and are discussed. Also discussed are the observed crack closure mechanisms.
The mechanical properties of two neat resin systems for use in carbon fiber epoxy composites were characterized. This included tensile and shear stiffness and strengths, coefficients of thermal and moisture expansion, and fracture toughness. Tests were conducted on specimens in the dry and moisture-saturated states, at temperatures of 23, 82 and 121 C. The neat resins tested were American Cyanamid 1806 and Union Carbide ERX-4901B(MPDA). Results were compared to previously tested neat resins. Four unidirectional carbon fiber reinforced composites were mechanically characterized. Axial and transverse tension and in-plane shear strengths and stiffness were measured, as well as transverse coefficients of thermal and moisture expansion. Tests were conducted on dry specimens only at 23 and 100 C. The materials tested were AS4/3502, AS6/5245-C, T300/BP907, and C6000/1806 unidirectional composites. Scanning electron microscopic examination of fracture surfaces was performed to permit the correlation of observed failure modes with the environmental test conditions.
The performance of candidate erosion resistant airfoil coatings installed in ground tested experimental JT8D and JT9D engines and subjected to cyclic endurance at idle, takeoff and intermediate power conditions has been evaluated. Engine tests were terminated prior to the scheduled 1000 cycles of endurance test due to high cycle fatigue fracture of the Gator-Gard plasma sprayed 88WC-12Co coating on titanium alloy airfoils. Coated steel (AMS5616) and nickel base alloy (Incoloy 901) performed well in both engine tests. Post test airfoil analyses consisted of binocular, scanning electron microscope and metallographic examinations.
The Lead-Zinc binary equilibrium system is currently being investigated. Ground based studies of this system were performed to examine the possibility of obtaining a couple which, after diffusion, could be examined continuously along the diffusion axis by quantitative metallography to determine the extent of diffusion. The specimens were analyzed by X-ray fluorescence in the scanning electron microscope to provide exact information on the chemical composition gradient. Two diffusion experiments were run simultaneously in the multipurpose furnace, each in its own isothermal cavity. Two flight samples, two flight backup samples, and two flight space samples were generated.
Results are reported of low magnetic field studies of dc magnetic susceptibility and ac magnetic susceptibility of bulk samples and powders. These data are analyzed and compared with the microstructures and compositions of the samples as determined by scanning electron microscopic micrographs, X-ray and chemical analysis. Particular emphasis is given to the interpretation of the ac magnetic susceptibility data which were obtained as function of the magnitude and frequency of the ac measuring field, and low values of an applied dc magnetic field. Two general conclusions are given and briefly discussed.
A continuous powder coating system was developed for coating carbon fiber with LaRC-TPI (Langley Research Center-Thermoplastic Polyimide), a high-temperature thermoplastic polymide invented by NASA-Langley. The coating line developed used a pneumatic fiber spreader to separate the individual fibers. The polymer was applied within a recirculating powder coating chamber then melted using a combination of direct electrical resistance and convective heating to make it adhere to the fiber tow. The tension and speed of the line were controlled with a dancer arm and an electrically driven fiber wind-up and wind-off. The effects of heating during the coating process on the flexibility of the prepreg produced were investigated. The uniformity with which the fiber tow could be coated with polymer also was examined. Composite specimens were fabricated from the prepreg and tested to determine optimum process conditions. The study showed that a very uniform and flexible prepeg with up to 50 percent by volume polymer could be produced with this powder coating system. The coating line minimized powder loss and produced prepeg in lengths of up to 300 m. The fiber spreading was found to have a major effect on the coating uniformity and flexibility. Though test results showed low composite tensile strengths, analysis of fracture surfaces under scanning electron microscope indicated that fiber/matrix adhesion was adequate.
Fatigue crack delay behavior at high stress ratio caused by single peak overloads was investigated in two thicknesses of 7475-T731 aluminum alloy. Closure measurements indicated no closure occurred before or throughout the overload plastic zones following the overload. This was further substantiated by comparing the specimen compliance following the overload with the compliance of a low R ratio test when the crack was fully open. Scanning electron microscope studies revealed that crack tunneling and possibly reinitiation of the crack occurred, most likely a result of crack-tip blunting. The number of delay cycles was greater for the thinner mixed mode stress state specimen than for the thicker plane strain stress state specimen, which is similar to low R ratio test results and may be due to a larger plastic zone for the mixed mode cased.
An in situ fatigue loading stage inside a scanning electron microscope (SEM) was used to determine the fatigue crack growth behavior of a PWA 1480 single-crystal nickel-based superalloy. The loading stage permits real-time viewing of the fatigue damage processes at high magnification. The PWA 1480 single-crystal, single-edge notch specimens were tested with the load axis parallel to the (100) orientation. Two distinct fatigue failure mechanisms were identified. The crack growth rate differed substantially when the failure occurred on a single slip system in comparison to multislip system failure. Two processes by which crack branching is produced were identified and are discussed. Also discussed are the observed crack closure mechanisms.
One of NASA'S agency-wide goals is the commercial development of space. To further this goal NASA is implementing a policy whereby U.S. firms are encouraged to utilize NASA facilities to develop and test concepts having commercial potential. Goddard, in keeping with this policy, will make the facilities and capabilities described in this document available to private entities at a reduced cost and on a noninterference basis with internal NASA programs. Some of these facilities include: (1) the Vibration Test Facility; (2) the Battery Test Facility; (3) the Large Area Pulsed Solar Simulator Facility; (4) the High Voltage Testing Facility; (5) the Magnetic Field Component Test Facility; (6) the Spacecraft Magnetic Test Facility; (7) the High Capacity Centrifuge Facility; (8) the Acoustic Test Facility; (9) the Electromagnetic Interference Test Facility; (10) the Space Simulation Test Facility; (11) the Static/Dynamic Balance Facility; (12) the High Speed Centrifuge Facility; (13) the Optical Thin Film Deposition Facility; (14) the Gold Plating Facility; (15) the Paint Formulation and Application Laboratory; (16) the Propulsion Research Laboratory; (17) the Wallops Range Facility; (18) the Optical Instrument Assembly and Test Facility; (19) the Massively Parallel Processor Facility; (20) the X-Ray Diffraction and Scanning Auger Microscopy/Spectroscopy Laboratory; (21) the Parts Analysis Laboratory; (22) the Radiation Test Facility; (23) the Ainsworth Vacuum Balance Facility; (24) the Metallography Laboratory; (25) the Scanning Electron Microscope Laboratory; (26) the Organic Analysis Laboratory; (27) the Outgassing Test Facility; and (28) the Fatigue, Fracture Mechanics and Mechanical Testing Laboratory.
Electron microscopy will be useful for characterization of inorganic dust grains in returned comet nucleus samples. The choice of instrument(s) will depend primarily on the nature of the samples, but ultimately a variety of electron-beam methods could be employed. Scanning and analytical (transmission) electron microscopy are the logical choise for morphological, mineralogical, and bulk chemical analyses of dust grains removed from ices. It may also be possible to examine unmelted ice/dust mixtures using an environmental scanning electron microscope equipped with a cryo-transfer unit and a cold stage. Electron microscopic observations of comet nuclei might include: (1) porosities of dust grains; (2) morphologies and microstructures of individual mineral grains; (3) relative abundances of olivine, pyroxene, and glass; and (4) the presence of phases that might have resulted from aqueous alteration (layer silicates, carbonates, sulfates).
A method of reacting TiCl4 with water saturated gaseous nitrogen (GN2) at the entrance into a high temperature gas flow is described. The TiO2 particles formed are then entrained in the gas flow and used as seed particles for making laser anemometry (LA) measurements of the flow velocity distribution in the hot gas. Scanning electron microscope photographs of the TiO2 particles are shown. Data rate of the LA processor was measured to determine the amount of TiO2 formed. The TiCl4 and mixing gas flow diagram is shown. This work was performed in an open jet burner.
Long flexible-boom models were required to develop ground-vibration test methods for very-low-frequency space structures with applications to the proposed Space Station. Pultruded quasi-isotropic composite beams were selected as an option over extruded aluminum alloy structures because of the lower cost potential, the higher specific strength, the flexural properties, and the dynamic similarity considerations. The reinforcement material that was used was biaxial (0 deg/90 deg) fiberglass roving held in place with knitted polyester yarn such that equal fiber volume in 0 deg and 90 deg orientations provided nearly equal strength in both longitudinal and transverse directions. An isophthalic polyester resin system was used as the matrix. Continuous lengths up to 270 ft were easily pultruded with biaxial fabric. Tracking problems were encountered with similar unidirectional fabrics. Analyses of processing problems were conducted to determine causes for delamination, scaling, and sloughing. Ultrasonic C-scanning and scanning electron microscope examinations were conducted as well as mechanical testing to failure. Test results indicate that pultrusion processes can be used to produce quasi-isotropic composite structures.
An investigation was conducted to characterize and model the fatigue crack growth (FCG) behavior of a SCS-6/Ti-15-3 metal matrix composite. Part of the study was conducted using a fatigue loading stage mounted inside a scanning electron microscope (SEM). This unique facility allowed high magnification viewing of the composite fatigue processes and measurement of the near crack tip displacements. The unidirectional composite was tested in the (0)8 (i.e., longitudinal) and (90)8 (i.e., transverse) orientations. For comparison purposes unreinforced matrix material produced by the identical process as the reinforced material was also tested. The results of the study reveal that the fatigue crack growth behavior of the composite is a function of specimen geometry, fiber orientation and the interaction of local stress fields with the highly anisotropic composite. In the case of (0)8 oriented single edge notch (SEN) specimens and (90)8 oriented compact tension (CT) specimens, the crack growth was normal to the loading direction. However, for the (0)8 CT specimens the crack grew mostly parallel to the loading and the fiber direction. The unusual fatigue behavior of the (0)8 CT specimens was attributed to the specimen geometry and the associated high tensile bending stresses perpendicular to the fiber direction. These stresses resulted in preferential cracking in the weak interface region perpendicular to the fiber direction. The interface region, and in particular the carbon coating surrounding the fiber proved to be the composites weakest link. In the (0)8 SEN the crack growth was confined to the matrix leaving behind unbroken fibers which bridged the cracked surfaces. As the crack grew longer, more fibers bridged the crack resulting in a progressive decrease in the crack growth rates and eventual crack arrest. The actual near crack tip displacement measurements were used in a proposed formulation for a bridging-corrected effective crack driving force, delta K(sub eff). This parameter was able to account for most of the experienced bridging and correlated the (0)8 SEN fatigue crack growth data reasonably well.
Previous analyses of the composition of mineral and matrix in the bone of young rats following space flight has revealed deficits in calcium, phosphorus, and osteocalcin, a non-collagenous protein, without an associated decrease in collagen. To characterize the location and nature of this mineralization defect in a weight bearing long bone, the femur, researchers attempted to relate the spatial distribution of mineral in situ in the proximal, central and distal thirds of the femoral diaphysis to the biochemical composition of bone from the same area. Biochemical analyses revealed lower concentrations of calcium, phosphorus and osteocalcin but not collagen only in the central third of the diaphysis of the flight animals (F) compared to synchronous controls (S). Collagen concentration was reduced only in the proximal third of the diaphysis, where all 3 crosslinks, expressed as nM/mol collagen were higher in F than S. A new technique, x ray microtomography, with a resolution of 26 microns, was used to obtain semi-quantitative data on mineral distribution in reconstructed sections of wet whole bone. To improve the resolution of the mineral density distribution, images of the surfaces of cut sections were analyzed by backscattered electrons in a scanning electron microscope (BSE). There was good agreement between the results of the two stereochemical techniques which revealed distinct patterns of mineralization in transverse and longitudinal directions of the diaphysis. The novel methodology developed for this flight experiment shows considerable promise in elucidating the biochemical nature of what appear to be regional alterations in the mineralization of long bones of animals exposed to spaceflight.