Electron-beam fabrication of gray-scale occulting spots in high-energy beam sensitive (HEBS) glass
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Introduction: Presolar grains preserve isotopic, chemical and microstructural records of physical and chemical processing, and formation mechanisms within a vast range of evolved stellar systems, the interstellar medium, solar nebula and their parent bodies. These evolutionary records are preserved at the micrometric to atomic scale, requiring coordinated studies to expand our understanding of evolutionary processes occurringthroughout ours and external stellar systems [1]. NanoSIMS enabled rapid in situ identification and isotopic characterisation of presolar grains and their stellar origins using 17O/16O and 18O/16O, and 13C/12C isotopic ratios [1]. Coordination with transmission electron microscopy (TEM) revealed crystallographic and localised contextual relationships and quantitively constrained their major and minor compositions [1]. However, trace elements cannot be quantified, the most sensitive geochemical tracers of environmental conditions, essential to unravelling the chemical record of their evolutionary pathway and parent stellar systems [2-3] . Furthermore, owing to the combination of technical limitations (only 5 – 7 isotopes can be measured per NanoSIMS run) and their small grain sizes of 100 nm < 3 μm (with rare exceptions in nanodiamonds (2 nm ≤) and SiC (< 40 μm)), the number of measurable isotopes per grain volume is limited [1,3] . Through more comprehensive isotopic studies of presolar grains, NanoSIMS studies have shown the importance of the latter, identifying Fe and Mg as important indicators of nuclear synthetic processing and their stellar origins, respectively [4- 5]. Coordination of NanoSIMS and Atom Probe Tomography (APT) revealed morphological signatures, and isotopic and chemical signatures at major to trace levels without requirements for preselection of elements [6]. However, crystallographic signatures in localized contextual relationships cannot be measured. Consequently, coordination of NanoSIMS, TEM and APT is essential to gain access to almost all contextual, structural and geochemical signatures within each presolar grain.Transmission electron microscopy requires a 100 nm thin lamella which is unstable in APT and would not produce any viable data. Atom probe tomography requires a needle-shaped specimen which when measured in TEM removes the local context, impacts the quality of the TEM diffraction images due to the shank angle of the needle, and can alter the chemistry of beam sensitive materials from the higher degree of surface exposure at the tip. To address these issues, we developed METIS-Fa (Multi-technical measurements of Electron Transparent materials using an Indium Sandwich - a FIB approach). A novel method which enables coordination of NanoSIMS, TEM and APT for generalized and targeted studies of individual grains, including beam sensitive materials, without compromising sample preparation requirements for TEM and APT. This method requires only indium and a Focus Ion Beam (FIB), minimizing the movement of fragile materials while still enabling preparation of TEM lamella into APT needles. Samples: Initial experimental development and testing of the method occurred at Astromaterials Research and Exploration Science (ARES), Johnson Space Centre (JSC), NASA and APT measurements and needle preparation occurred at JdLC, Curtin University. Synthetic silicate samples were used as analogs for presolar silicates when performing a trial run of the method. Samples were extracted from a polished thin section created at JSC, NASA, comprised of 38 wt.% Si, 17 wt.% FeO, 13 wt.% MgO, 12 wt.% Al, 11 wt.% Ca based on electron microprobe analysis (EMPA) [8] . Experimental details, pressure and temperature conditions were presented in [8] and references therein. Testing of the capability to target individual grains in mineral matrices using this method for acquisition in APT, measured matrix regions in meteoritic thin sections of primitive meteorites. These meteorites and their identified presolar grains for future targeted studies are detailed in [9]. Techniques: The TEM-FIB lamella were prepared using a FIB. An e-beam assisted pt deposition was used as a protective coating for the synthetic and meteoritic samples. When targeting individual grains, a secondary e-beam assisted pt deposition button is placed over the desired grain before the protective coating to denote its location. A JEOL 2500SE field-emission TEM was used for high-resolution imaging, energy-dispersive X-ray (EDX) and electron diffraction data.TheMETIS-Fa method was experimentally designed, tested and executed using a FIB at ARES, JSCNASA. Needles for APT were prepared using the Tescan Lyra3 GM Dual Beam Focus Ion Beam (FIB) Field Emission SEM (FE-SEM) at the JdLC, Curtin University. Atom probe tomography measurements were conducted using a CAMECA Local Electrode Atom Probe, LEAP 4000X HR. Two pure indium needles were analyzed initially to constraining acquisition parameters and stability under the beam. Manual acquisition was required to maintain evaporation of specimen’s at the apex and monitor interactions with measurement parameters. Experimental Design: Indium foil is pressed onto an Al stub with a pneumatic press and mounted into the FIB adjacent to the TEM-FIB lamella of interest. Using a FIB, two indium slices (5 μm x ~300 nm x 3 μm) are extracted from indium foil and aligned with the TEM-FIB lamella before touching the TEM-FIB lamella. Each slice is then attached through cold welding to the FIB-TEM lamella. This approach eliminates the need for chemical treatments and proved effective for aligning the Indium within the region of interest for APT, holding it in place for up to 4 days during testing.Once both indium slices are attached within their pre-determined region per grain targeting requirements, they are gradually melted onto the FIB-TEM lamella.When targeting a specific grain, measurements should be taken of the pt button and its distance from edge to edge of the lamella before and after sandwiching. A secondary button should be placed over the same region after the Indium slices have been attached to improve precision when preparing APT needles. Results: Figure 1 shows two indium slices melted onto a FIB-TEM lamella, adding additional bulk for preparation into APT needles as shown in Figure 2 [7] . The latter was essential so samples could be measured in TEM and APT without compromising sample preparation requirements and consequently data quality and acquisition stability. METIS-Fa proved effective forimproving geometry. Figure 3 shows a successful APTrun of the synthetic silicate. EMPA, TEM and APTshowed no chemical alterations. During targetingtesting, a solar silicate grain was successfully identifiedand measured in TEM, and prepared into an APTneedle. However, the indium was melted too long during sample preparation, causing expansion andformation of internal porosity leading to sample loss.Conclusion: METIS-Fa greatly expands the number of isotopic and chemical signatures measured per grain volume, and enables measurements of contextual, structural, crystallographic, isotopic and geochemical signatures within individual grains. Gaining access to such a vast range of evolutionary signatures required for expanding our understanding of external stellar and planetary systems and the evolution of our solar system. This method was designed for application to a vast range of phases including being sensitive materials and thus provides a way for coordination of NanoSIMS, TEM and APT not just for the study of presolar grains and by extension primitive astromaterials, but studies in a vast range of other fields including the geosciences and material sciences.Acknowledgments: Thankyou to ARES, JSC, NASA; JdLC Curtin University and Space Science Technology Centre for the use of laboratory facilities and funding [confirm].
New designs, and materials appropriate for such designs, are under investigation in an effort to develop coronagraph occulting masks having broad-band spectral characteristics superior to those currently employed. These designs and materials are applicable to all coronagraphs, both ground-based and spaceborne. This effort also offers potential benefits for the development of other optical masks and filters that are required (1) for precisely tailored spatial transmission profiles, (2) to be characterized by optical-density neutrality and phase neutrality (that is, to be characterized by constant optical density and constant phase over broad wavelength ranges), and/or (3) not to exhibit optical- density-dependent phase shifts. The need for this effort arises for the following reasons: Coronagraph occulting masks are required to impose, on beams of light transmitted through them, extremely precise control of amplitude and phase according to carefully designed transmission profiles. In the original application that gave rise to this effort, the concern has been to develop broad-band occulting masks for NASA s Terrestrial Planet Finder coronagraph. Until now, experimental samples of these masks have been made from high-energy-beam-sensitive (HEBS) glass, which becomes locally dark where irradiated with a high-energy electron beam, the amount of darkening depending on the electron-beam energy and dose. Precise mask profiles have been written on HEBS glass blanks by use of electron beams, and the masks have performed satisfactorily in monochromatic light. However, the optical-density and phase profiles of the HEBS masks vary significantly with wavelength; consequently, the HEBS masks perform unsatisfactorily in broad-band light. The key properties of materials to be used in coronagraph occulting masks are their extinction coefficients, their indices of refraction, and the variations of these parameters with wavelength. The effort thus far has included theoretical predictions of performances of masks that would be made from alternative materials chosen because the wavelength dependences of their extinction coefficients and their indices of refraction are such that that the optical-density and phase profiles of masks made from these materials can be expected to vary much less with wavelength than do those of masks made from HEBS glass. The alternative materials considered thus far include some elemental metals such as Pt and Ni, metal alloys such as Inconel, metal nitrides such as TiN, and dielectrics such as SiO2. A mask as now envisioned would include thin metal and dielectric films having stepped or smoothly varying thicknesses (see figure). The thicknesses would be chosen, taking account of the indices of refraction and extinction coefficients, to obtain an acceptably close approximation of the desired spatial transmittance profile with a flat phase profile
The design and performance of an f/35 submillimeter photometer are discussed. It is noted that the instrument provides for both broad- and medium-width passbands between 350 microns and 2 mm and for beam sizes between 28 arcsec and 100 arcsec FWHM. Under good atmospheric conditions, a broad-band 400 micron sensitivity of approximately 1.5 Jy is found to be obtainable in one hour. A description is given of the photometer's support housing, submillimeter radiometer, and electronics and data-handling system. In evaluating the performance, attention is given to sensitivity, beam profiles, and the effect of changes in the aperture on the signal.
Presolar grains are remnants of evolved stellar systems preserved within primitive extraterrestrial materials. They are important for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium, Solar Nebula and their parent stellar environments [1]. Our recent work has shown coordinated nano-scale Secondary Ion Mass Spectrometry (NanoSIMS) and Atom Probe Tomography (APT) can show isotopic and chemical signatures at major to trace levels, morphological signatures, and regional contextual relationships [2,3]. Previous studies have shown Transmission Electron Microscopy (TEM) of Focus Ion Beam (FIB) TEM lamella, can provide localized contextual relationships, crystallographic information and chemical information [1]. Coordinating NanoSIMS, TEM, and APT could gain access to almost all contextual, structural and geochemical signatures within each presolar grain. However, this has proved challenging owing to the preparation requirements for TEM and APT. For example, studying specimen prepared as APT needles in TEM removes the local context, the higher degree of surface exposure can alter the chemistry of beam sensitive materials, and the shank angle of the needle can impact the quality of TEM diffraction images. We designed a new FIB method which takes a 100 nm thick FIB-TEM lamella and sandwiches it between two indium slices (5 μm x ~300 nm x 3 μm). The indium is melted onto the lamella surface using the electron beam (Fig 1). This process adds bulk to the lamella, making it more amenable to APT needle formation (Fig 2). Consequently, samples can be prepared per the optimal requirements for each technique improving data quality, acquisition stability, and access to the signatures and relationships summarised earlier. This technique can be used for measuring multiple phases across a TEM lamella and targeting an individual phase. For example, a presolar grain identified in NanoSIMS could be targeted, studied in TEM and then indium sandwiched with its precise location in the TEM lamella marked using a Pt button for preparation of an APT needle and atomic scale acquisition. [1] A. M. Davis (2014) Meteorites and cosmochemical processes, 1. [2] Nevill N. et al. (2023) LPSC, 54, #1707. [3] Nevill N. et al. (2023) LPSC, 54, #1714.
Analyses with a scanning transmission x-ray microscope (STXM) using x-ray absorption near edge structure (XANES) spectroscopy were applied for the molecular characterization of two kinds of carbonaceous particles of unknown origin, termed category 3, which were collected from the Hayabusa spacecraft sample catcher. Carbon-XANES spectra of the category 3 particles displayed typical spectral patterns of heterogeneous organic macromolecules; peaks corresponding to aromatic/olefinic carbon, heterocyclic nitrogen and/or nitrile, and carboxyl carbon were all detected. Nitrogen-XANES spectra of the particles showed the presence of N-functional groups such as imine, nitrile, aromatic nitrogen, amide, pyrrole, and amine. An oxygen-XANES spectrum of one of the particles showed a ketone group. Differences in carbon- and nitrogen-XANES spectra of the category 3 particles before and after transmission electron microscopic (TEM) observations were observed, which demonstrates that the carbonaceous materials are electron beam sensitive. Calcium-XANES spectroscopy and elemental contrast mapping identified a calcium carbonate grain from one of the category 3 particles. No fluorine-containing molecular species were detected in fluorine-XANES spectra of the particles. The organic macromolecular features of the category 3 particles were distinct from commercial and/or biological ‘fresh (non-degraded)’ polymers, but the category 3 molecular features could possibly reflect degradation of contaminant polymer materials or polymer materials used on the Hayabusa spacecraft. However, an extraterrestrial origin for these materials cannot currently be ruled out.
Sensitivity to velocity changes along beam axis reduced. Weighted-end cantilever beams of accelerometer deflected equally by acceleration in y direction. When acceleration to right as well as up or down, right beam deflected more, while left beam deflected less. Bridge circuit averages outputs of strain gauges measuring deflections, so cross-axis sensitivity of accelerometer reduced. New device simple and inexpensive.
When observed in a cesium beam frequency standard, the hyperfine transition frequency of the atoms differs slightly from the invariant transition frequency of the unperturbed atoms at rest. The various physical and technical origins of the frequency offsets are stated. They relate to fundamental physical effects, to the method of probing the atomic resonance and to the frequency control of the slaved oscillator. The variation of the frequency offsets under a change of the value of the internal operating characteristics is considered. The sensitivity to a change of the magnetic induction, the microwave power, and the temperature is given. A comparison is made of the sensitivity of cesium beam frequency standards of the commercially available type, making use of magnetic state selection, and of devices under study, in which the state preparation and detection is accomplished optically. The pathways between the external stimuli and the physical origin of the frequency offsets are specified.
A multi-beam, multi-color, polarized laser transmitter has been developed for mapping applications. It uses commercial off-the-shelf components for a lowcost approach for a ruggedized laser suitable for field deployment. The laser transmitter design is capable of delivering dual wavelengths, multiple beams on each wavelength with equal (or variable) intensities per beam, and a welldefined state of polarization. This laser transmitter has been flown on several airborne campaigns for the Slope Imaging Multi-Polarization Photon Counting Lidar (SIMPL) instrument, and at the time of this reporting is at a technology readiness level of between 5 and 6. The laser is a 1,064-nm microchip high-repetition-rate laser emitting energy of about 8 microjoules per pulse. The beam was frequency-doubled to 532 nm using a KTP (KTiOPO4) nonlinear crystal [other nonlinear crystals such as LBO (LiB3O5) or periodically poled lithium niobiate can be used as well, depending on the conversion efficiency requirements], and the conversion efficiency was approximately 30 percent. The KTP was under temperature control using a thermoelectric cooler and a feedback monitoring thermistor. The dual-wavelength beams were then spectrally separated and each color went through its own optical path, which consisted of a beam-shaping lens, quarterwave plate (QWP), and a birefringent crystal (in this case, a calcite crystal, but others such as vanadate can be used). The QWP and calcite crystal set was used to convert the laser beams from a linearly polarized state to circularly polarized light, which when injected into a calcite crystal, will spatially separate the circularly polarized light into the two linear polarized components. The spatial separation of the two linearly polarized components is determined by the length of the crystal. A second set of QWP and calcite then further separated the two beams into four. Additional sets of QWP and calcite can be used to further split the beams into multiple orders of two. The spatially separated beams had alternating linearly polarization states; a half-wave plate (HWP) array was then made to rotate the alternating states of A multi-beam, multi-color, polarized laser transmitter has been developed for mapping applications. It uses commercial off-the-shelf components for a lowcost approach for a ruggedized laser suitable for field deployment. The laser transmitter design is capable of delivering dual wavelengths, multiple beams on each wavelength with equal (or variable) intensities per beam, and a welldefined state of polarization. This laser transmitter has been flown on several airborne campaigns for the Slope Imaging Multi-Polarization Photon Counting Lidar (SIMPL) instrument, and at the time of this reporting is at a technology readiness level of between 5 and 6. The laser is a 1,064-nm microchip high-repetition-rate laser emitting energy of about 8 microjoules per pulse. The beam was frequency-doubled to 532 nm using a KTP (KTiOPO4) nonlinear crystal [other nonlinear crystals such as LBO (LiB3O5) or periodically poled lithium niobiate can be used as well, depending on the conversion efficiency requirements], and the conversion efficiency was approximately 30 percent. The KTP was under temperature control using a thermoelectric cooler and a feedback monitoring thermistor. The dual-wavelength beams were then spectrally separated and each color went through its own optical path, which consisted of a beam-shaping lens, quarterwave plate (QWP), and a birefringent crystal (in this case, a calcite crystal, but others such as vanadate can be used). The QWP and calcite crystal set was used to convert the laser beams from a linearly polarized state to circularly polarized light, which when injected into a calcite crystal, will spatially separate the circularly polarized light into the two linear polarized components. The spatial separation of the two linearly polarized components is determined by the length of the crystal. A cond set of QWP and calcite then further separated the two beams into four. Additional sets of QWP and calcite can be used to further split the beams into multiple orders of two. The spatially separated beams had alternating linearly polarization states; a half-wave plate (HWP) array was then made to rotate the alternating states of
Sensitive method, identifying effective damping mechanisms, involves comparing experimentally determined ratio of first to second mode magnification factors related to common point on beam. Cluster size has little effect on frequencies of elements, magnification factor decreases with cluster size, and viscous and stress damping are dominant damping mechanisms.
Robotic welding controlled by reliable, relatively-noise-free optoelectronic unit. Bounding off meniscus of pool of molten metal, laser beam impinges on position-sensitive photodetector. Beam diameter adjusted for width of weld. Optical filters screen out light from arc. Made from small, low-cost components and utilizing optical fibers to conduct signals, system immune to electromagnetic interference common in industrial environments. Aimed for automatic welders, robot welders in particular and also adaptable to other types of welding, including tungsten/inert-gas, laser, and electron-beam techniques.
At NASA Lewis Research Center, the feasibility of beaming power from orbiting satellites to the surface of the moon was studied. Reference microwave and laser beam power concepts were found to be 1/3 to 1/6 the mass of surface solar systems. Further analysis was performed to determine the sensitivity of the reference concepts to technology performance levels and mission architecture scenarios, such as beaming to multiple surface sites and lunar rovers. Previous studies concluded that frequencies above 35 GHz for the microwave systems were not critical for reducing the main base mass; however, when multiple sites and rovers are considered, this may become necessary. In addition, for the laser system, the pointing accuracy of the satellites becomes a critical factor for rover applications. These issues and other important results of the parametric studies, are discussed.
Particle beam power density detection and measurement apparatus
An experimentally-based method for determining the stiffness and damping of truss joints is described. The analytical models use springs and both viscous and friction dampers to simulate joint load-deflection behavior. A least-squares algorithm is developed to identify the stiffness and damping coefficients of the analytical joint models from test data. The effects of nonlinear joint stiffness such as joint dead band are also studied. Equations for predicting the sensitivity of beam deformations to changes in joint stiffness are derived and used to show the level of joint stiffness required for nearly rigid joint behavior. Finally, the global frequency sensitivity of a truss structure to random perturbations in joint stiffness is discussed.
Strain and temperature response of Multiwalled Carbon Nanotube (MWCNT/CNT) yarns on a stainless steel test beam has been studied. The carbon nanotube yarns are spun from a multiwalled carbon nanotube forest grown on a silicon substrate to a 4-ply yarn with a diameter of about 15-20 microns. Four of the 4-ply CNT yarns are arranged in a Wheatstone bridge configuration on the stainless steel test beam using a thin layer of polyurethane resin that insulates and protects the yarns from the test beam. Strain sensitivities of the CNT yarn sensors range from 1.39 to 1.75 mV/V/1000 microstrain at room temperature, and temperature sensitivity of the CNT yarn bridge is 91 microA/degC. Resistance of the yarns range from 215 to 270 ohms for CNT yarn length of approximately 5 mm. Processes used in attaching the CNT yarns on the test beam and experimental procedures used for the measurements are described. Conventional metallic foil strain gages are attached to the test beam to compare with the CNT sensors. The study demonstrates multifunctional capability of the sensor for strain and temperature measurements and shows its applicability where engineering strain is less than 3%.
An analysis was performed in order to find the best placement for proof-mass actuators and to determine the importance of placement, i.e., what is the sensitivity of beam flexure to actuator placement. The analysis was performed by using the NASTRAN finite element model for a flexible beam with 21 grid points on beam, by using the nonlinear DISCOS simulation of 20 deg slew and the use of a closed-loop linear quadratic regulator (lqr). Some conclusions reached are: (1) proof-mass actuators can reduce flexure amplitude and damp oscillations; (2) amplitude of deformations during slew is relatively insensitive to placement of actuators; (3) damping factor of oscillations is sensitive to actuator placement; and (4) the degree of controllability method indicates most effective placement for actuators.
A key step in the application of formal automated design techniques to structures under transient loading is the calculation of sensitivities of response quantities to the design parameters. This paper considers structures with general forms of damping acted on by general transient loading and addresses issues of computational errors and computational efficiency. The equations of motion are reduced using the traditional basis of vibration modes and then integrated using a highly accurate, explicit integration technique. A critical point constraint formulation is used to place constraints on the magnitude of each response quantity as a function of time. Three different techniques for calculating sensitivities of the critical point constraints are presented. The first two are based on the straightforward application of the forward and central difference operators, respectively. The third is based on explicit differentiation of the equations of motion. Condition errors, finite difference truncation errors, and modal convergence errors for the three techniques are compared by applying them to a simple five-span-beam problem. Sensitivity results are presented for two different transient loading conditions and for both damped and undamped cases.
A key step in the application of formal automated design techniques to structures under transient loading is the calculation of sensitivities of response quantities to the design parameters. This paper considers response quantities to the design parameters. This paper considers structures with general forms of damping acted on by general transient loading and addresses issues of computational errors and computational efficiency. The equations of motion are reduced using the traditional basis of vibration modes and then integrated using a highly accurate, explicit integration technique. A critical point constraint formulation is used to place constraints on the magnitude of each response quantity as a function of time. Three different techniques for calculating sensitivities of the critical point constraints are presented. The first two are based on the straightforward application of the forward and central difference operators, respectively. The third is based on explicit differentiation of the equations of motion. Condition errors, finite difference truncation errors, and modal convergence errors for the three techniques are compared by applying them to a simple five-span-beam problem. Sensitivity results are presented for two different transient loading conditions and for both damped and undamped cases.