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Specimen holder for X ray diffraction analysis presents the specimen to the incident X rays in a curvature. This permits the use of an X ray beam having a larger divergence angle, the beam intensity is increased, and the statistical accuracy of analysis is improved.
Reduces spectral contamination by spurious X-ray. Specimen holder made of compressed carbon, securely retains standard electron microscope grid (disk) 3 mm in diameter and absorbs backscattered electrons that otherwise generate spurious X-rays. Since holder inexpensive, dedicated to single specimen when numerous samples examined.
Fixture holds sheet specimens for flammability tests. Frame and clamps designed to minimize local overstress on specimen. Heat capacity of fixture low, interfering less with interpretation of results of test by drawing less heat away from specimen. Accepts films, fabrics, foams, and other sheets, rigid or flexible. Specimens thin or thick, or of variable thickness. Bent to accommodate curved rigid specimens. Also used for such other tests as particle-impact tests.
Test specimen and loading frame developed for fatigue and fracture testing of materials under mode-II (sliding-mode) loading. Assembly placed in compression-testing machine. Loads directed oppositely along centerline cause self-similar crack to propagate. Enables consistently accurate alignment of specimens before insertion of specimen/frame assemblies into compression-testing machine. Makes design attractive for testing in hostile environments in which access to machine or furnace limited. Additional feature, with little or no modification, placed horizontally into impact testing machine and subjected to loading at high speeds.
Microscope-stage holder keeps filter pad flat to keep it in focus. Specimen holder is special vacuum chuck that applies suction through flat screen. Suction keeps filter pad flat against specimen holder while microscope stage moving to scan areas denoted by grid. In microscope system equipped with video camera, image-analyzing/particle-counting computer, and automatic focus, use of stage speeds count considerably by eliminating need to stop frequently for manual refocusing. Technician free to perform other tasks while computer controls translation of stage and takes count automatically.
Single-ended notch design facilitates accurate measurements of crack progression. Novel test specimen and novel loading fixture and fracture testing of materials under Mode II, or sliding-mode, loading. Testing required for analysis of failures in structural materials, bearings, and the like.
Small mass-spectrometer specimens are positioned in three dimensions by manipulator that employs two bellows to provide vacuum seal and accommodate movement of specimen holder. Inner bellows and outer bellows accommodate vertical and horizontal motion, respectively. Y-axis movement is in and out of plane of page. Specimen-holder column is hollow so electrical wires can pass through it to specimen.
New instrument allows in situ measurement of flow resistivity on Earth's ground surface. Nonintrusive instrument includes specimen holder inserted into ground. Flow resistivity measured by monitoring compressed air passing through flow-meters; pressure gages record pressure at ground surface. Specimen holder with knife-edged inner and outer cylinders easily driven into ground. Air-stream used in measuring flow resistivity of ground enters through quick-connect fitting and exits through screen and venthole.
Effects of specimen preparation on measured values of an acrylic's electomagnetic properties at X-band microwave frequencies, TE sub 1,0 mode, utilizing an automatic network analyzer have been studied. For 1 percent or less error, a gap between the specimen edge and the 0.901-in. wall of the specimen holder was the most significant parameter. The gap had to be less than 0.002 in. The thickness variation and alignment errors in the direction parallel to the 0.901-in. wall were equally second most significant and had to be less than 1 degree. Errors in the measurement f the thickness were third most significant. They had to be less than 3 percent. The following parameters caused errors of 1 percent or less: ratios of specimen-holder thicknesses of more than 15 percent, gaps between the specimen edge and the 0.401-in. wall less than 0.045 in., position errors less than 15 percent, surface roughness, hickness variation in the direction parallel to the 0.401-in. wall less than 35 percent, and specimen alignment in the direction parallel to the 0.401-in. wall mass than 5 degrees.
A small, lightweight, compact, hand-held photomicroscope provides simultaneous viewing and photographing, with adjustable specimen illumination and exchangeable camera format. The novel photomicroscope comprises a main housing having a top plate, bottom plate, and side walls. The objective lens is mounted on the top plate in an inverted manner relative to the normal type of mounting. The specimen holder has an adjusting mechanism for adjustably moving the specimen vertically along an axis extending through the objective lens as well as transverse of the axis. The lens system serves to split the beam of light into two paths, one to the eyepiece and the other to a camera mounting. A light source is mounted on the top plate and directs light onto the specimen. A rheostat device is mounted on the top plate and coupled to the power supply for the light source so that the intensity of the light may be varied.
X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.
An airflow resistivity instrument features a novel specimen holder, especially designed for in situ measurement on the earth's ground surface. This capability eliminates the disadvantages of prior intrusive instruments, which necessitate the removal of a test specimen from the ground. A prototype instrument can measure airflow resistivities in the range 10-5000 cgs rayl/cm, at specimen depths up to 15.24 cm (6 in.), and at differential pressures up to 2490.8 dyn sq cm (1 in. H2O) across the specimen. Because of the close relationship between flow resistivity and acoustic impedance, this instrument should prove useful in acoustical studies of the earth's ground surface. Results of airflow resistivity measurements on an uncultivated grass field for varying values of moisture content are presented.
Radial distribution profiles of elemental carbon in lunar soils consisting of particles in the size range of 50 to 150 microns were investigated. Initial experiments on specimen preparation and the analysis of prepared specimens by Auger electron spectrometry (AES) and scanning electron microscopy (SEM) are described. Results from splits of samples 61501,84 and 64421,11, which were mounted various ways in several specimen holders, are presented. A low carbon content was observed in AES spectra from soil particles that were subjected to sputter-ion cleaning with 960eV argon ions for periods of time up to a total exposure for one hour. This ion charge was sufficient to remove approximately 70 nm of material from the surface. All of the physically adsorbed carbon (as well as water vapor, etc.) would normally be removed in the first few minutes, leaving only carbon in the specimen, and metal support structure, to be detected thereafter.
An improved promoted-combustion system has been developed for studying the effects of elevated temperatures on the flammability of metals in pure oxygen. In prior promoted-combustion chambers, initial temperatures of metal specimens in experiments have been limited to the temperatures of gas supplies, usually near room temperature. Although limited elevated temperature promoted-combustion chambers have been developed using water-cooled induction coils for preheating specimens, these designs have been limited to low-pressure operation due to the hollow induction coil. In contrast, the improved promoted-combustion chamber can sustain a pressure up to 10 kpsi (69 MPa) and, through utilization of a solid induction coil, is capable of preheating a metal specimen up to its melting point [potentially in excess of 2,000 F (approximately equal to 1,100 C)]. Hence, the improved promoted combustion chamber makes a greater range of physical conditions and material properties accessible for experimentation. The chamber consists of a vertical cylindrical housing with an inner diameter of 8 in. (20.32 cm) and an inner height of 20.4 in. (51.81 cm). A threaded, sealing cover at one end of the housing can be unscrewed to gain access for installing a specimen. Inlet and outlet ports for gases are provided. Six openings arranged in a helical pattern in the chamber wall contain sealed sapphire windows for viewing an experiment in progress. The base of the chamber contains pressure-sealed electrical connectors for supplying power to the induction coil. The connectors feature a unique design that prevents induction heating of the housing and the pressure sealing surfaces; this is important because if such spurious induction heating were allowed to occur, chamber pressure could be lost. The induction coil is 10 in. (25.4 cm) long and is fitted with a specimen holder at its upper end. At its lower end, the induction coil is mounted on a ceramic base, which affords thermal insulation to prevent heating of the base of the chamber during use. A sapphire cylinder protects the coil against slag generated during an experiment. The induction coil is energized by a 6-kW water-cooled power supply operating at a frequency of 400 kHz. The induction coil is part of a parallel-tuned circuit, the tuning of which is used to adjust the coupling of power to the specimen. The chamber is mounted on a test stand along with pumps, valves, and plumbing for transferring pressurized gas into and out of the chamber. In addition to multiple video cameras aimed through the windows encircling the chamber, the chamber is instrumented with gauges for monitoring the progress of an experiment. One of the gauges is a dual-frequency infrared temperature transducer aimed at the specimen through one window. Chamber operation is achieved via a console that contains a computer running apparatus-specific software, a video recorder, and real-time video monitors. For safety, a blast wall separates the console from the test stand.
A prerequisite for conducting valid corrosion experiments by in situ electron microscopy techniques is not only the achievement of UHV background pressure conditions at the site of the specimen but also the ability to clean the surface of the thin metal substrate specimen before initiation of the corrosive interaction. A miniaturized simple ion gun has been constructed for this purpose. The gun is small enough to be incorporated into an UHV electron microscope specimen chamber with hot stage in such a way as to permit bombardment of the substrate specimen while observing it by transmission electron microscopy TEM. It is shown that the ion beam generated is confined well enough to cause a sputtering removal of substrate material at a rate of approximately 5-10 A/min and to prevent the sputter deposition of contaminating material from the specimen holder.
A simple laboratory method for determining ignitability of materials is described. The apparatus consists of a Mellen high-flux heater capable of producing up to 13 W/sq cm heat flux, a Medtherm water-cooled radiometer for measuring heat flux, a mounting frame to hold all components in proper position, and specimen holders of the type used for the NBS smoke test. Time to ignition at different heat flux levels is recorded. Test results are presented for a variety of materials.
The Bond method was employed to measure the lattice parameter in an area of 0.4 mm in diameter of EFG Si-ribbons to an accuracy of + or - 0.00008 A. A Bond goniometer was built which included a goniostat with a special specimen holder to mount ribbons 1 m in length and 75 mm in width which could be rotated about two orthogonal axes, and a Leitz microscope for precision alignment of a particular area into the center of the goniostat and the small primary X-ray beam. The (321) planes were found to be parallel to the surface of the ribbons with an angular spread of about 15 deg. The poles of the (111) planes clustered about an angle of 25 deg away from the surface normal, again with a spread of 10 deg. The lattice parameter of a small piece of ribbon material was found to be a sub o = 5.43075 A. A maximum stress of 115 MPa was observed in a fractured ribbon which corresponded to the fracture stress of single crystals of Si.
Shock-wave data are presented for liquid helium which has been compressed to densities up to five times greater than the normal liquid. The helium was heated to temperatures up to 21,000 K, while the maximum pressure attained was 56 GPa. The properties of helium and hydrogen are important for modeling the giant planets Saturn and Jupiter where these elements are the major constituents. Conditions on Saturn are of particular interest because studies have suggested that this planet has an internal energy source which is associated with unmixing and gravitational separation of the hydrogen-helium fluid at pressures below 1 TPa. The existence of this phase transition depends very sensitively on the hydrogen and helium equation of state. In the experiments, strong shock waves were generated by the impact of planar projectiles into cryogenic specimen holders.