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NASA NTRS2005

The Application of Infrared Thermographic Inspection Techniques to the Space Shuttle Thermal Protection System

The Nondestructive Evaluation Sciences Branch at NASA s Langley Research Center has been actively involved in the development of thermographic inspection techniques for more than 15 years. Since the Space Shuttle Columbia accident, NASA has focused on the improvement of advanced NDE techniques for the Reinforced Carbon-Carbon (RCC) panels that comprise the orbiter s wing leading edge. Various nondestructive inspection techniques have been used in the examination of the RCC, but thermography has emerged as an effective inspection alternative to more traditional methods. Thermography is a non-contact inspection method as compared to ultrasonic techniques which typically require the use of a coupling medium between the transducer and material. Like radiographic techniques, thermography can be used to inspect large areas, but has the advantage of minimal safety concerns and the ability for single-sided measurements. Principal Component Analysis (PCA) has been shown effective for reducing thermographic NDE data. A typical implementation of PCA is when the eigenvectors are generated from the data set being analyzed. Although it is a powerful tool for enhancing the visibility of defects in thermal data, PCA can be computationally intense and time consuming when applied to the large data sets typical in thermography. Additionally, PCA can experience problems when very large defects are present (defects that dominate the field-of-view), since the calculation of the eigenvectors is now governed by the presence of the defect, not the "good" material. To increase the processing speed and to minimize the negative effects of large defects, an alternative method of PCA is being pursued where a fixed set of eigenvectors, generated from an analytic model of the thermal response of the material under examination, is used to process the thermal data from the RCC materials. Details of a one-dimensional analytic model and a two-dimensional finite-element model will be presented. An overview of the PCA process as well as a quantitative signal-to-noise comparison of the results of performing both embodiments of PCA on thermographic data from various RCC specimens will be shown. Finally, a number of different applications of this technology to various RCC components will be presented.

Cramer, K. E.↗
NASA NTRS2007

Overview of Supersonic Aerodynamics Measurement Techniques in the NASA Langley Unitary Plan Wind Tunnel

An overview is given of selected measurement techniques used in the NASA Langley Research Center (NASA LaRC) Unitary Plan Wind Tunnel (UPWT) to determine the aerodynamic characteristics of aerospace vehicles operating at supersonic speeds. A broad definition of a measurement technique is adopted in this paper and is any qualitative or quantitative experimental approach that provides information leading to the improved understanding of the supersonic aerodynamic characteristics. On-surface and off-surface measurement techniques used to obtain discrete (point) and global (field) measurements and planar and global flow visualizations are described, and examples of all methods are included. The discussion is limited to recent experiences in the UPWT and is, therefore, not an exhaustive review of existing experimental techniques. The diversity and high quality of the measurement techniques and the resultant data illustrate the capabilities of a ground-based experimental facility and the key role that it plays in the advancement of our understanding, prediction, and control of supersonic aerodynamics.

Erickson, Gary E.↗
NASA NTRS2007

Application of Semi Active Control Techniques to the Damping Suppression Problem of Solar Sail Booms

Solar sails provide a propellant free form for space propulsion. These are large flat surfaces that generate thrust when they are impacted by light. When attached to a space vehicle, the thrust generated can propel the space vehicle to great distances at significant speeds. For optimal performance the sail must be kept from excessive vibration. Active control techniques can provide the best performance. However, they require an external power-source that may create significant parasitic mass to the solar sail. However, solar sails require low mass for optimal performance. Secondly, active control techniques typically require a good system model to ensure stability and performance. However, the accuracy of solar sail models validated on earth for a space environment is questionable. An alternative approach is passive vibration techniques. These do not require an external power supply, and do not destabilize the system. A third alternative is referred to as semi-active control. This approach tries to get the best of both active and passive control, while avoiding their pitfalls. In semi-active control, an active control law is designed for the system, and passive control techniques are used to implement it. As a result, no external power supply is needed so the system is not destabilize-able. Though it typically underperforms active control techniques, it has been shown to out-perform passive control approaches and can be unobtrusively installed on a solar sail boom. Motivated by this, the objective of this research is to study the suitability of a Piezoelectric (PZT) patch actuator/sensor based semi-active control system for the vibration suppression problem of solar sail booms. Accordingly, we develop a suitable mathematical and computer model for such studies and demonstrate the capabilities of the proposed approach with computer simulations.

Adetona, O.↗
NASA NTRS2008

New Techniques in Characterization of Ferroelectric Materials

Two new techniques have been developed to characterize Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT) based ferroelectric single crystals: (i) electro-thermal imaging, and (ii) single crystal x-ray diffraction in the transmission mode. (i) Electro-thermal imaging is a remote sensing technique that can detect the polarization direction and poling state of a whole crystal slice. This imaging technique utilizes an IR camera to determine the field induced temperature change and does not require any special or destructive sample preparation. In the resulting images it is possible to distinguish regions of 180 deg domains. This powerful technique can be used remotely during poling to determine the poling state of the crystal to avoid over-poling that can result in inferior properties and/or cracking of the crystals. Electro-thermal imaging produced the first direct observations of polarization rotation. Under bipolar field, the domains near the corners were the first to switch direction. As the field increased above the coercive field, domains at the center part of the crystals switched direction. (ii) X-ray diffraction in the transmission mode has long been used in structure determination of organic crystals and proteins; however, it is not used much to characterize inorganic systems. 0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 single crystals were examined by this XRD technique for the first time, and a never-before-seen super-lattice was revealed with a doubling of the unit cell in all three directions, giving a cell volume eight times that of a traditional perovskite unit cell. The significance of the super-lattice peaks increased with poling, indicating a structural contribution to ordering. Lack of such observations by electron diffraction in the transmission electron microscope examinations suggests the presence of a bulk effect.

Sehirlioglu, Alp↗
NASA NTRS2009

New Flutter Analysis Technique for CFD-based Unsteady Aeroelasticity

This paper presents a flutter analysis technique for the transonic flight regime. The technique uses an iterative approach to determine the critical dynamic pressure for a given mach number. Unlike other CFD-based flutter analysis methods, each iteration solves for the critical dynamic pressure and uses this value in subsequent iterations until the value converges. This process reduces the iterations required to determine the critical dynamic pressure. To improve the accuracy of the analysis, the technique employs a known structural model, leaving only the aerodynamic model as the unknown. The aerodynamic model is estimated using unsteady aeroelastic CFD analysis combined with a parameter estimation routine. The technique executes as follows. The known structural model is represented as a finite element model. Modal analysis determines the frequencies and mode shapes for the structural model. At a given mach number and dynamic pressure, the unsteady CFD analysis is performed. The output time history of the surface pressure is converted to a nodal aerodynamic force vector. The forces are then normalized by the given dynamic pressure. A multi-input multi-output parameter estimation software, ERA, estimates the aerodynamic model through the use of time histories of nodal aerodynamic forces and structural deformations. The critical dynamic pressure is then calculated using the known structural model and the estimated aerodynamic model. This output is used as the dynamic pressure in subsequent iterations until the critical dynamic pressure is determined. This technique is demonstrated on the Aerostructures Test Wing-2 model at NASA's Dryden Flight Research Center.

Pak, Chan-gi↗
NASA NTRS2009

Low-Complexity Lossless and Near-Lossless Data Compression Technique for Multispectral Imagery

This work extends the lossless data compression technique described in Fast Lossless Compression of Multispectral- Image Data, (NPO-42517) NASA Tech Briefs, Vol. 30, No. 8 (August 2006), page 26. The original technique was extended to include a near-lossless compression option, allowing substantially smaller compressed file sizes when a small amount of distortion can be tolerated. Near-lossless compression is obtained by including a quantization step prior to encoding of prediction residuals. The original technique uses lossless predictive compression and is designed for use on multispectral imagery. A lossless predictive data compression algorithm compresses a digitized signal one sample at a time as follows: First, a sample value is predicted from previously encoded samples. The difference between the actual sample value and the prediction is called the prediction residual. The prediction residual is encoded into the compressed file. The decompressor can form the same predicted sample and can decode the prediction residual from the compressed file, and so can reconstruct the original sample. A lossless predictive compression algorithm can generally be converted to a near-lossless compression algorithm by quantizing the prediction residuals prior to encoding them. In this case, since the reconstructed sample values will not be identical to the original sample values, the encoder must determine the values that will be reconstructed and use these values for predicting later sample values. The technique described here uses this method, starting with the original technique, to allow near-lossless compression. The extension to allow near-lossless compression adds the ability to achieve much more compression when small amounts of distortion are tolerable, while retaining the low complexity and good overall compression effectiveness of the original algorithm.

Xie, Hua↗
NASA NTRS2007

Flash Diffusivity Technique Applied to Individual Fibers

A variant of the flash diffusivity technique has been devised for determining the thermal diffusivities, and thus the thermal conductivities, of individual aligned fibers. The technique is intended especially for application to nanocomposite fibers, made from narrower fibers of polyphenylene benzobisthiazole (PBZT) and carbon nanotubes. These highly aligned nanocomposite fibers could exploit the high thermal conductivities of carbon nanotubes for thermal-management applications. In the flash diffusivity technique as practiced heretofore, one or more heat pulse(s) is (are) applied to the front face of a plate or disk material specimen and the resulting time-varying temperature on the rear face is measured. Usually, the heat pulse is generated by use of a xenon flash lamp, and the variation of temperature on the rear face is measured by use of an infrared detector. The flash energy is made large enough to produce a usefully high temperature rise on the rear face, but not so large as to significantly alter the specimen material. Once the measurement has been completed, the thermal diffusivity of the specimen is computed from the thickness of the specimen and the time dependence of the temperature variation on the rear face. Heretofore, the infrared detector used in the flash diffusivity technique has been a single-point detector, which responds to a spatial average of the thermal radiation from the rear specimen surface. Such a detector cannot distinguish among regions of differing diffusivity within the specimen. Moreover, two basic assumptions of the thermaldiffusivity technique as practiced heretofore are that the specimen is homogeneous and that heat flows one-dimensionally from the front to the rear face. These assumptions are not valid for an inhomogeneous (composite) material.

Mayeaux, Brian↗
NASA NTRS2010

Developing NDE Techniques for Large Cryogenic Tanks - Year 2 Report

The Shuttle Program requires very large cryogenic ground storage tanks in which to store liquid oxygen and hydrogen. The existing Launch Complex-39 Pad tanks, which will be passed onto future launch programs, are over 40 years old and have received minimal refurbishment and only external inspections over the years. The majority of the structure is inaccessible without a full system drain of cryogenic liquid and insulation in the annular region. It was previously thought that there was a limit to the number of temperature cycles that the tanks could handle due to possible insulation compaction before undergoing a costly and time consuming complete overhaul; therefore the tanks were not drained and performance issues with these tanks, specifically the Pad B LH2 tank, were accepted. There is a need and an opportunity, as the Shuttle program ends and work to upgrade the launch pad progresses, to develop innovative non-destructive evaluation (NDE) techniques to analyze the current tanks. Techniques are desired that can aid in determining the extent of refurbishment required to keep the tanks in service for another 20+ years. A non-destructive technique would also be a significant aid in acceptance testing of new and refurbished tanks, saving significant time and money, if corrective actions can be taken before cryogen is introduced to the systems. Year one of this project concentrated on analysis of the current tanks located at LC-39 while cryogen was present. Year two of this project concentrated on analysis of detectable thermal variations on the outer surface of the tanks as the cryogen was drained and the inner vessel warmed to ambient conditions. Two techniques have been deployed in the field to monitor the tank. The first consisted of a displacement sensor to monitor for any expansions at the base of the tank during warm-up that could indicate a compaction issue with the insulation. The second technique was continued thermal monitoring of the tank through and after warm up. The indications noted in the thermal images were compared to bore-scope images of the annular region taken once the tank was inert and warmed to ambient conditions. Similar thermal imaging was performed on a smaller tank where an insulation void was induced to compare the effectiveness of thermal imagining on a different tank geometry.

Arens, Ellen↗
NASA NTRS2011

Technique for Radiometer and Antenna Array Calibration with Two Antenna Noise Diodes

This paper presents a new technique to calibrate a microwave radiometer and phased array antenna system. This calibration technique uses a radiated noise source in addition to an injected noise sources for calibration. The plane of reference for this calibration technique is the face of the antenna and therefore can effectively calibration the gain fluctuations in the active phased array antennas. This paper gives the mathematical formulation for the technique and discusses the improvements brought by the method over the existing calibration techniques.

Srinivasan, Karthik↗
NASA NTRS2006

Techniques for Connecting Superconducting Thin Films

Several improved techniques for connecting superconducting thin films on substrates have been developed. The techniques afford some versatility for tailoring the electronic and mechanical characteristics of junctions between superconductors in experimental electronic devices. The techniques are particularly useful for making superconducting or alternatively normally conductive junctions (e.g., Josephson junctions) between patterned superconducting thin films in order to exploit electron quantum-tunneling effects. The techniques are applicable to both low-Tc and high-Tc superconductors (where Tc represents the superconducting- transition temperature of a given material), offering different advantages for each. Most low-Tc superconductors are metallic, and heretofore, connections among them have been made by spot welding. Most high-Tc superconductors are nonmetallic and cannot be spot welded. These techniques offer alternatives to spot welding of most low-Tc superconductors and additional solutions to problems of connecting most high-Tc superconductors.

Mester, John↗
NASA NTRS2008

New Techniques to Evaluate the Incendiary Behavior of Insulators

New techniques for evaluating the incendiary behavior of insulators is presented. The onset of incendive brush discharges in air is evaluated using standard spark probe techniques for the case simulating approaches of an electrically grounded sphere to a charged insulator in the presence of a flammable atmosphere. However, this standard technique is unsuitable for the case of brush discharges that may occur during the charging-separation process for two insulator materials. We present experimental techniques to evaluate this hazard in the presence of a flammable atmosphere which is ideally suited to measure the incendiary nature of micro-discharges upon separation, a measurement never before performed. Other measurement techniques unique to this study include; surface potential measurements of insulators before, during and after contact and separation, as well as methods to verify fieldmeter calibrations using a charge insulator surface opposed to standard high voltage plates. Key words: Kapton polyimide film, incendiary discharges, brush discharges, contact and frictional electrification, ignition hazards, insulators, contact angle, surface potential measurements.

Buhler, Charles↗
NASA NTRS2013

Investigation of a Cross-Correlation Based Optical Strain Measurement Technique for Detecting radial Growth on a Rotating Disk

The Aeronautical Sciences Project under NASA`s Fundamental Aeronautics Program is extremely interested in the development of novel measurement technologies, such as optical surface measurements in the internal parts of a flow path, for in situ health monitoring of gas turbine engines. In situ health monitoring has the potential to detect flaws, i.e. cracks in key components, such as engine turbine disks, before the flaws lead to catastrophic failure. In the present study, a cross-correlation imaging technique is investigated in a proof-of-concept study as a possible optical technique to measure the radial growth and strain field on an already cracked sub-scale turbine engine disk under loaded conditions in the NASA Glenn Research Center`s High Precision Rotordynamics Laboratory. The optical strain measurement technique under investigation offers potential fault detection using an applied high-contrast random speckle pattern and imaging the pattern under unloaded and loaded conditions with a CCD camera. Spinning the cracked disk at high speeds induces an external load, resulting in a radial growth of the disk of approximately 50.0-im in the flawed region and hence, a localized strain field. When imaging the cracked disk under static conditions, the disk will be undistorted; however, during rotation the cracked region will grow radially, thus causing the applied particle pattern to be .shifted`. The resulting particle displacements between the two images will then be measured using the two-dimensional cross-correlation algorithms implemented in standard Particle Image Velocimetry (PIV) software to track the disk growth, which facilitates calculation of the localized strain field. In order to develop and validate this optical strain measurement technique an initial proof-of-concept experiment is carried out in a controlled environment. Using PIV optimization principles and guidelines, three potential speckle patterns, for future use on the rotating disk, are developed and investigated in the controlled experiment. A range of known shifts are induced on the patterns; reference and data images are acquired before and after the induced shift, respectively, and the images are processed using the cross-correlation algorithms in order to determine the particle displacements. The effectiveness of each pattern at resolving the known shift is evaluated and discussed in order to choose the most suitable pattern to be implemented onto a rotating disk in the Rotordynamics Lab. Although testing on the rotating disk has not yet been performed, the driving principles behind the development of the present optical technique are based upon critical aspects of the future experiment, such as the amount of expected radial growth, disk analysis, and experimental design and are therefore addressed in the paper.

Clem, Michelle M.↗
NASA NTRS2013

Progress of a Cross-correlation Based Optical Strain Measurement Technique for Detecting Radial Growth on a Rotating Disk

The Aeronautical Sciences Project under NASAs Fundamental Aeronautics Program is extremely interested in the development of fault detection technologies, such as optical surface measurements in the internal parts of a flow path, for in situ health monitoring of gas turbine engines. In situ health monitoring has the potential to detect flaws, i.e. cracks in key components, such as engine turbine disks, before the flaws lead to catastrophic failure. In the present study, a cross-correlation imaging technique is investigated in a proof-of-concept study as a possible optical technique to measure the radial growth and strain field on an already cracked sub-scale turbine engine disk under loaded conditions in the NASA Glenn Research Centers High Precision Rotordynamics Laboratory. The optical strain measurement technique under investigation offers potential fault detection using an applied background consisting of a high-contrast random speckle pattern and imaging the background under unloaded and loaded conditions with a CCD camera. Spinning the cracked disk at high speeds induces an external load, resulting in a radial growth of the disk of approximately 50.8-m in the flawed region and hence, a localized strain field. When imaging the cracked disk under static conditions, the disk will appear shifted. The resulting background displacements between the two images will then be measured using the two-dimensional cross-correlation algorithms implemented in standard Particle Image Velocimetry (PIV) software to track the disk growth, which facilitates calculation of the localized strain field. In order to develop and validate this optical strain measurement technique an initial proof-of-concept experiment is carried out in a controlled environment. Using PIV optimization principles and guidelines, three potential backgrounds, for future use on the rotating disk, are developed and investigated in the controlled experiment. A range of known shifts are induced on the backgrounds; reference and data images are acquired before and after the induced shift, respectively, and the images are processed using the cross- correlation algorithms in order to determine the background displacements. The effectiveness of each background at resolving the known shift is evaluated and discussed in order to choose to the most suitable background to be implemented onto a rotating disk in the Rotordynamics Lab. Although testing on the rotating disk has not yet been performed, the driving principles behind the development of the present optical technique are based upon critical aspects of the future experiment, such as the amount of expected radial growth, disk analysis, and experimental design and are therefore addressed in the paper.

Clem, Michelle M.↗
NASA NTRS2014

Simulation/Emulation Techniques: Compressing Schedules With Parallel (HW/SW) Development

NASA has always been in the business of balancing new technologies and techniques to achieve human space travel objectives. NASA's Kedalion engineering analysis lab has been validating and using many contemporary avionics HW/SW development and integration techniques, which represent new paradigms to NASA's heritage culture. Kedalion has validated many of the Orion HW/SW engineering techniques borrowed from the adjacent commercial aircraft avionics solution space, inserting new techniques and skills into the Multi - Purpose Crew Vehicle (MPCV) Orion program. Using contemporary agile techniques, Commercial-off-the-shelf (COTS) products, early rapid prototyping, in-house expertise and tools, and extensive use of simulators and emulators, NASA has achieved cost effective paradigms that are currently serving the Orion program effectively. Elements of long lead custom hardware on the Orion program have necessitated early use of simulators and emulators in advance of deliverable hardware to achieve parallel design and development on a compressed schedule.

Mangieri, Mark L.↗
NASA NTRS2013

Sabots, Obturator and Gas-In-Launch Tube Techniques for Heat Flux Models in Ballistic Ranges

For thermal protection system (heat shield) design for space vehicle entry into earth and other planetary atmospheres, it is essential to know the augmentation of the heat flux due to vehicle surface roughness. At the NASA Ames Hypervelocity Free Flight Aerodynamic Facility (HFFAF) ballistic range, a campaign of heat flux studies on rough models, using infrared camera techniques, has been initiated. Several phenomena can interfere with obtaining good heat flux data when using this measuring technique. These include leakage of the hot drive gas in the gun barrel through joints in the sabot (model carrier) to create spurious thermal imprints on the model forebody, deposition of sabot material on the model forebody, thereby changing the thermal properties of the model surface and unknown in-barrel heating of the model. This report presents developments in launch techniques to greatly reduce or eliminate these problems. The techniques include the use of obturator cups behind the launch package, enclosed versus open front sabot designs and the use of hydrogen gas in the launch tube. Attention also had to be paid to the problem of the obturator drafting behind the model and impacting the model. Of the techniques presented, the obturator cups and hydrogen in the launch tube were successful when properly implemented

obturators↗
NASA NTRS2014

MAG4 Versus Alternative Techniques for Forecasting Active-Region Flare Productivity

MAG4 is a technique of forecasting an active region's rate of production of major flares in the coming few days from a free-magnetic-energy proxy. We present a statistical method of measuring the difference in performance between MAG4 and comparable alternative techniques that forecast an active region's major-flare productivity from alternative observed aspects of the active region. We demonstrate the method by measuring the difference in performance between the "Present MAG4" technique and each of three alternative techniques, called "McIntosh Active-Region Class," "Total Magnetic Flux," and "Next MAG4." We do this by using (1) the MAG4 database of magnetograms and major-flare histories of sunspot active regions, (2) the NOAA table of the major-flare productivity of each of 60 McIntosh active-region classes of sunspot active regions, and (3) five technique-performance metrics (Heidke Skill Score, True Skill Score, Percent Correct, Probability of Detection, and False Alarm Rate) evaluated from 2000 random two-by-two contingency tables obtained from the databases. We find that (1) Present MAG4 far outperforms both McIntosh Active-Region Class and Total Magnetic Flux, (2) Next MAG4 significantly outperforms Present MAG4, (3) the performance of Next MAG4 is insensitive to the forward and backward temporal windows used, in the range of one to a few days, and (4) forecasting from the free-energy proxy in combination with either any broad category of McIntosh active-region classes or any Mount Wilson active-region class gives no significant performance improvement over forecasting from the free-energy proxy alone (Present MAG4).

Falconer, David A.↗
NASA NTRS2014

Progress of a Cross-Correlation Based Optical Strain Measurement Technique for Detecting Radial Growth on a Rotating Disk

The Aeronautical Sciences Project under NASA's Fundamental Aeronautics Program is interested in the development of novel measurement technologies, such as optical surface measurements for the in situ health monitoring of critical constituents of the internal flow path. In situ health monitoring has the potential to detect flaws, i.e. cracks in key components, such as engine turbine disks, before the flaws lead to catastrophic failure. The present study, aims to further validate and develop an optical strain measurement technique to measure the radial growth and strain field of an already cracked disk, mimicking the geometry of a sub-scale turbine engine disk, under loaded conditions in the NASA Glenn Research Center's High Precision Rotordynamics Laboratory. The technique offers potential fault detection by imaging an applied high-contrast random speckle pattern under unloaded and loaded conditions with a CCD camera. Spinning the cracked disk at high speeds (loaded conditions) induces an external load, resulting in a radial growth of the disk of approximately 50.0-μm in the flawed region and hence, a localized strain field. When imaging the cracked disk under static conditions, the disk will be undistorted; however, during rotation the cracked region will grow radially, thus causing the applied particle pattern to be 'shifted'. The resulting particle displacements between the two images is measured using the two-dimensional cross-correlation algorithms implemented in standard Particle Image Velocimetry (PIV) software to track the disk growth, which facilitates calculation of the localized strain field. A random particle distribution is adhered onto the surface of the cracked disk and two bench top experiments are carried out to evaluate the technique's ability to measure the induced particle displacements. The disk is shifted manually using a translation stage equipped with a fine micrometer and a hotplate is used to induce thermal growth of the disk, causing the particles to become shifted. For both experiments, reference and test images are acquired before and after the induced shifts, respectively, and then processed using PIV software. The controlled manual translation of the disk resulted in detection of the particle displacements accurate to ~1.75% of full scale and the thermal expansion experiment resulted in successful detection of the disk's thermal growth as compared to the calculated thermal expansion results. After validation of the technique through the induced shift experiments, the technique is implemented in the Rotordynamics Lab for preliminary assessment in a simulated engine environment. The discussion of the findings and plans for future work to improve upon the results are addressed in the paper.

rotordynamics↗
NASA NTRS2014

A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain

The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically <100micron) from the surface of an asteroid (25143 Itokawa). These precious samples provide important insights into early Solar System processes, but their sizes pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on sample preparation. We developed a hybrid technique combining traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for more thorough in situ investigations of grain surfaces and interiors. Using this method, we increase the number of FIB-prepared sections that can be recovered from a particle with dimensions on the order of tens of microns. These sections can be subsequently analyzed using a variety of analytical techniques. Particle RA-QD02-0211 is a approx. 40×40×20 micron particle from Itokawa containing olivine and Fe sulfides. It was embedded in low viscosity epoxy and partly sectioned to a depth of approx 10 micron; sections are placed on Cu grids with thin amorphous films for transmission electron microscope (TEM) analyses. With the sample surface partly exposed, the epoxy bullet is trimmed to a height of approx. 5mm to accommodate the allowable dimensions for FIB work (FEI Quanta 600 3D dual beam FIB-SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ≳3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.

Berger, Eve L.↗