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Applications of synchrotron radiation to materials science: Diffraction imaging (topography) and microradiography
Synchrotron radiation sources are now available throughout the world. The use of hard X-ray radiation from these sources for materials science is described with emphasis on diffraction imaging for material characterization. With the availability of synchrotron radiation, real-time in situ measurements of dynamic microstructural phenomena have been started. This is a new area where traditional application of X-rays has been superseded. Examples are chosen from limited areas and are by no means exhaustive. The new emerging information will, no doubt, have great impact on materials science and engineering.
Nondestructive evaluation of structural ceramics by photoacoustic microscopy
A photoacoustic microscopy (PAM) digital imaging system was developed and utilized to characterize silicon nitride material at the various stages of the ceramic fabrication process. Correlation studies revealed that photoacoustic microscopy detected failure initiating defects in substantially more specimens than microradiography and ultrasonic techniques. Photoacoustic microscopy detected 10 to 100 micron size surface and subsurface pores and inclusions, respectively, up to 80 microns below the interrogating surface in machined sintered silicon nitride. Microradiography detected 50 micron diameter fracture controlling pores and inclusions. Subsurface holes were detected up to a depth of 570 microns and 1.00 mm in sintered silicon nitride and silicon carbide, respectively. Seeded voids of 20 to 30 micron diameters at the surface and 50 microns below the interrogating surface were detected by photoacoustic microscopy and microradiography with 1 percent X-ray thickness sensitivity. Tight surface cracks of 96 micron length x 48 micron depth were detected by photoacoustic microscopy. PAM volatilized and removed material in the green state which resulted in linear shallow microcracks after sintering. This significantly limits the use of PAM as an in-process NDE technique.
Real-time visualization of particle evolution during reactive flux-assisted processing of aluminum melts
Here, a multi-modal, multi-scale correlative tomography investigation of Al-TiC metal matrix composites processed via flux-assisted reaction synthesis is reported. Synchrotron X-ray microradiography is utilized to visualize the reaction and particle evolution in real-time. Changes in particle diameter and areal number density suggest that the process is nucleation- rather than growth-dominated. At 950 °C, the bulk of the reaction takes place in a relatively short time span of less than 600 s. The microstructure is imaged at higher resolution in 2D (scanning electron microscopy) and 3D (synchrotron X-ray nanotomography), revealing the formation of carbide particles with a hexagonal platelet morphology. We propose that the morphology arises due to the incorporation of Si impurities during the experiment. It is expected that the correlative tomography workflow and analysis may guide future metal matrix composite (MMC) processing strategies.
A compact and flexible induction furnace for in situ X-ray microradiograhy and computed microtomography at Elettra: design, characterization and first tests
A compact and versatile induction furnace for in situ high-resolution synchrotron and laboratory hard X-ray microradiography and computed microtomography is described. The furnace can operate from 773 to 1723 K. Its programmable controller enables the user to specify multiple heating and cooling ramp rates as well as variable dwell times at fixed temperatures allowing precise control of heating and cooling rates to within 5 K. The instrument can work under a controlled atmosphere. Thanks to the circular geometry of the induction coils, the heat is homogeneously distributed in the internal volume of the graphite cell ( ca . 150 mm 3 ) where the sample holder is located. The thermal gradient within the furnace is less than 5 K over a height of ca . 5 mm. This new furnace design is well suited to the study of melting and solidification processes in geomaterials, ceramics and several metallic alloys, allowing fast heating (tested up to 6.5 K s -1 ) and quenching (up to 21 K s -1 ) in order to freeze the sample microstructure and chemistry under high-temperature conditions. The sample can be held at high temperatures for several hours, which is essential to follow phenomena with relatively slow dynamics, such as crystallization processes in geomaterials. The utility of the furnace is demonstrated through a few examples of experimental applications performed at the Elettra synchrotron laboratory (Trieste, Italy).
Tensile fracture of unidirectional B-Al composite.
Fracture studies on unidirectional boron filament/aluminum matrix composite under axial tension were conducted using scanning electron microscopy, microradiography, and an acoustic emission technique. The combination of these analysis techniques has allowed the description and microstructural characterization of a new noncumulative fracture mode which involves filament break propagation. This fracture mode was found to severely limit the tensile strength of the composite, since the initiation of break propagation leads immediately to catastrophic failure at filament stress levels above a critical value. This critical filament stress was found to be 170,000 psi, and it appeared to be independent of filament diameter, number of filament layers, and the type of matrix alloy.
Investigation of solidification in zero-gravity environment; M553 sphere forming experiment. Phase C: Evaluation of Skylab specimens
Results on specimen evaluation and discussion of solidification behavior in each case are reported in the following order: (1) specimen SL-1.6, (2) specimen SL-2.8, (3) specimen SL-2.4, (4) specimen SL-1.10 and (5) specimen SL-1.11. Comparison is made with ground-processed specimens of similar composition, whenever pertinent and meaningful. Among the nondestructive evaluation methods the measurement of sphericity was conducted by micrometric and shadowgraphic techniques. The intricate shape of specimens in some cases appeared difficult to define. In measuring the density, liquid penetration inside cavities that outcrop on the surface was avoided by sealing off these cavities. Among the destructive evaluation methods the use of the Quantimet 720 required particular attention, because of the small difference in contrast between second phases and micropores. With regard to microporosity microvoids in the core of some specimens were so fine that X-ray microradiography had to be used.
Evidence for arrested bone formation during spaceflight
Addressing the question of whether the bone formed in space is unusual, the morphology of bone made at the tibial diaphysis of rats before, during, and after spaceflight is studied. Evidence of arrest lines in the bone formed in space is reported suggesting that bone formation ceases along portions of the periosteum during spaceflight. Visualized by microradiography, the arrest lines are shown to be less mineralized than the surrounding bone matrix. When viewed by scanning electron microscopy, it is seen that bone fractures more readily at the site of an arrest line. These observations are seen as suggesting that arrest lines are a zone of weakness and that their formation may result in decreased bone strength in spite of normalization of bone formation after flight. The occurrence, location, and morphology of arrest lines are seen as suggesting that they are a visible result of the phenomenon of arrested bone formation.
Quantitative 3-D imaging topogrammetry for telemedicine applications
The technology to reliably transmit high-resolution visual imagery over short to medium distances in real time has led to the serious considerations of the use of telemedicine, telepresence, and telerobotics in the delivery of health care. These concepts may involve, and evolve toward: consultation from remote expert teaching centers; diagnosis; triage; real-time remote advice to the surgeon; and real-time remote surgical instrument manipulation (telerobotics with virtual reality). Further extrapolation leads to teledesign and telereplication of spare surgical parts through quantitative teleimaging of 3-D surfaces tied to CAD/CAM devices and an artificially intelligent archival data base of 'normal' shapes. The ability to generate 'topogrames' or 3-D surface numerical tables of coordinate values capable of creating computer-generated virtual holographic-like displays, machine part replication, and statistical diagnostic shape assessment is critical to the progression of telemedicine. Any virtual reality simulation will remain in 'video-game' realm until realistic dimensional and spatial relational inputs from real measurements in vivo during surgeries are added to an ever-growing statistical data archive. The challenges of managing and interpreting this 3-D data base, which would include radiographic and surface quantitative data, are considerable. As technology drives toward dynamic and continuous 3-D surface measurements, presenting millions of X, Y, Z data points per second of flexing, stretching, moving human organs, the knowledge base and interpretive capabilities of 'brilliant robots' to work as a surgeon's tireless assistants becomes imaginable. The brilliant robot would 'see' what the surgeon sees--and more, for the robot could quantify its 3-D sensing and would 'see' in a wider spectral range than humans, and could zoom its 'eyes' from the macro world to long-distance microscopy. Unerring robot hands could rapidly perform machine-aided suturing with precision micro-sewing machines, splice neural connections with laser welds, micro-bore through constricted vessels, and computer combine ultrasound, microradiography, and 3-D mini-borescopes to quickly assess and trace vascular problems in situ. The spatial relationships between organs, robotic arms, and end-effector diagnostic, manipulative, and surgical instruments would be constantly monitored by the robot 'brain' using inputs from its multiple 3-D quantitative 'eyes' remote sensing, as well as by contact and proximity force measuring devices. Methods to create accurate and quantitative 3-D topograms at continuous video data rates are described.
Imaging the inside of thick structures using cosmic rays
The authors present here a new method to image reinforcement elements inside thick structures and the results of a demonstration measurement performed on a mock-up wall built at Los Alamos National Laboratory. The method, referred to as “multiple scattering muon radiography”, relies on the use of cosmic-ray muons as probes. The work described in this article was performed to prove the viability of the technique as a means to image the interior of the dome of Florence Cathedral Santa Maria del Fiore, one of the UNESCO World Heritage sites and among the highest profile buildings in existence. Its result shows the effectiveness of the technique as a tool to radiograph thick structures and image denser object inside them.