Ralf K. Heilmann

Massachusetts Institute of Technology, Cambridge, Massachusetts, United States

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Publications (97)52.84 Total impact

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    ABSTRACT: Thin silicon dioxide films have been studied as a function of deposition parameters and annealing temperatures. Films were deposited by tetraethoxysilane (TEOS) dual-frequency plasma enhanced chemical vapor deposition with different time interval fractions of high-frequency and low-frequency plasma depositions. The samples were subsequently annealed up to 930 °C to investigate their stress behavior. Films that were deposited in high-frequency dominated plasma were found to have tensile residual stress after annealing at temperatures higher than 800 °C. The residual stress can be controlled to slightly tensile by changing the annealing temperature. High tensile stress was observed during the annealing of high-frequency plasma-deposited films, leading to film cracks that limit the film thickness, as predicted by the strain energy release rate equation. Thick films without cracks were obtained by iterating deposition and annealing to stack multiple layers. A series of wet cleaning experiments were conducted, and we discovered that water absorption in high-frequency plasma-deposited films causes the residual stress to decrease. A ∼40 nm thick low-frequency deposited oxide cap is sufficient to prevent water from diffusing through the film. Large-area free-standing tensile stressed oxide membranes without risk of buckling were successfully fabricated.
    Journal of Micromechanics and Microengineering 01/2014; 24(2). · 1.79 Impact Factor
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    ABSTRACT: We report several break-through nanofabrication developments enabling high efficiency and high resolving power spectrometers in the soft x-ray band. The device is the critical-angle transmission (CAT) grating, which combines the low mass and relaxed alignment tolerances of a transmission grating with the high broad-band efficiency and high diffraction orders of a blazed reflection grating. Past work successfully demonstrated the CAT grating concept; however, the open-area fraction was often less than 20% whilst more than 50% is desired. This presents numerous nanofabrication challenges including a requirement for a freestanding silicon membrane of ultra high-aspect ratio bars at a period of 200 nanometers with minimal cross support blockage. Furthermore, the sidewalls must be smooth to a few nanometers to efficiently reflect soft x-rays. We have developed a complete nanofabrication process for creating freestanding CAT gratings via plasma-etching silicon wafers with a buried layer of SiO2. This removable buried layer enables combining a record-performance plasma etch for the CAT grating with a millimeter-scale honeycomb structural support to create a large-area freestanding membrane. We have also developed a process for polishing sidewalls of plasma-etched ultra-high aspect ratio nanoscale silicon structures via potassium hydroxide (KOH). This process utilizes the anisotropic etch nature of single crystal silicon in KOH. We developed a novel alignment technique to align the CAT grating bars to the {111} planes of silicon within 0.2 degrees, which enables KOH to etch away sidewall roughness without destroying the structure, since the {111} planes etch approximately 100 times slower than the non-{111} planes. Preliminary results of a combined freestanding grating with polishing are presented to enable efficient diffraction of soft x-rays.
    Proc SPIE 09/2013;
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    ABSTRACT: Achieving both high resolution and large collection area in the next generation of x-ray telescopes requires highly accurate shaping of thin mirrors, which is not achievable with current technology. Ion implantation offers a promising method of modifying the shape of mirrors by imparting internal stresses in a substrate, which are a function of the ion species and dose. This technique has the potential for highly deterministic substrate shape correction using a rapid, low cost process. Wafers of silicon and glass (D-263 and BK-7) have been implanted with Si+ ions at 150 keV, and the changes in shape have been measured using a Shack-Hartmann metrology system. We show that a uniform dose over the surface repeatably changes the spherical curvature of the substrates, and we show correction of spherical curvature in wafers. Modeling based on experiments with spherical curvature correction shows that ion implantation could be used to eliminate higher-order shape errors, such as astigmatism and coma, by using a spatially-varying implant dose. We will report on progress in modelling and experimental tests to eliminate higher-order shape errors. In addition, the results of experiments to determine the thermal and temporal stability of implanted substrates will be reported.
    Proc SPIE 09/2013;
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    ABSTRACT: Molding glass by using air bearings is a promising procedure for inexpensive and high precision glass shaping. Thin glass sheets are sandwiched between air bearings and pushed flat while being thermally cycled. In this study, a novel device for shaping glass is created and tested using 0.5 mm thick, 100 mm round, Schott D263 wafers. Numerous samples were shaped with varying values for bearing-to-glass gap and maximum temperature, and were measured with a Shack Hartmann metrology tool. Glass was shaped with bearing-to-glass gaps of >50 μm, 36+/-2.5 μm, and 30.5+/-2.5 μm. The best peak-to-valley (P-V) flatness achieved is 6.7/3.6+/-0.5 μm for front/back of the glass sheet, using a gap of 36+/-2.5 μm. The average steady-state P-V achieved is 12 μm. Using the same device parameters, the best repeatability achieved over the whole 100 mm wafer is 2.7+/-0.5 μm P-V and 9.5 arcseconds RMS slope error. When looking at 60 mm sections, the repeatability improves to <1 μm P-V and 5+/-0.5 arcsec.
    Proc SPIE 09/2013;
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    ABSTRACT: Large area, high resolving power spectroscopy in the soft x-ray band can only be achieved with a state-of-the-art diffraction grating spectrometer, comprised of large collecting-area focusing optics with a narrow point spread function, large-area high-resolving power diffraction gratings, and small pixel, order sorting x-ray detectors. Recently developed critical-angle transmission (CAT) gratings combine the advantages of transmission gratings (low mass, relaxed figure and alignment tolerances) and blazed reflection gratings (high broad band diffraction efficiency, utilization of higher diffraction orders). Several new mission concepts containing CAT grating based spectrometers (AEGIS, AXSIO, SMART-X) promise to deliver unprecedented order-of-magnitude improvements in soft x-ray spectroscopy figures of merit related to the detection and characterization of emission and absorption lines, thereby addressing high-priority questions identified in the Astro2010 Decadal Survey "New Worlds New Horizons". We review the current status of CAT grating fabrication, present recent fabrication results, and describe our plans and technology development roadmap for the coming year and beyond.
    Proc SPIE 09/2013;
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    ABSTRACT: Large area, high resolving power spectroscopy in the soft x-ray band can only be achieved with a state-of-the-art diffraction grating spectrometer. Recently developed critical-angle transmission (CAT) gratings combine the advantages of transmission gratings (low mass, relaxed figure and alignment tolerances) and blazed reflection gratings (high broad band diffraction efficiency, utilization of higher diffraction orders). Since the demise of IXO there are no soft x-ray spectroscopy missions in the pipeline, but several new mission concepts containing CAT grating based spectrometers such as AXSIO promise to deliver unprecedented order-of-magnitude improvements in soft x-ray spectroscopy figures of merit. The CAT grating principle has previously been demonstrated with x rays using small wet-etched samples. We report the latest progress in the fabrication and testing of large (32x32 mm^2) CAT grating prototypes with an integrated hierarchy of low-obstruction support structures. The gratings are fabricated from silicon-on-insulator wafers using advanced lithography and highly anisotropic dry and wet etching techniques. We present our latest grating fabrication results.
    01/2013;
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    ABSTRACT: A fabrication process has been developed to chemically polish the sidewalls of 200 nm-pitch gratings via potassium hydroxide (KOH) etching following the Bosch deep reactive-ion etching (DRIE) process. Previous KOH polishing experiments focused on micron scale features. This work is the first reported combined DRIE-KOH etching process on the nanoscale for ultrahigh aspect ratio structures with feature sizes 30 times smaller than previously published work. The primary application of the gratings is x-ray spectroscopy and requires polished sidewalls for efficient x-ray reflection. Polishing is also critical for increasing the open area by narrowing the grating bars, which increases the throughput of x-rays. The increased open area is also valuable for other applications such as ultraviolet filtration, neutron spectroscopy and biofiltration. Advanced Bosch processes leave approximately 4 nm, root mean square (RMS), of roughness on the sidewalls. This roughness needs to be reduced to below 1 nm to efficiently reflect soft x-rays with wavelengths between 1 and 5 nm. Furthermore, high aspect ratio DRIE can result in bar width variations of approximately a factor of two from the top to the middle of the channel, commonly referred to as bowing. The polishing procedure presented here removes the roughness to below the resolution of the scanning electron microscope, and was measured via an atomic force microscope to be less than 1 nm RMS. The bowing has also been reduced by at least a factor of 3. The polishing process takes advantage of the anisotropy of KOH silicon etching. Specifically, the {111} silicon planes etch approximately 100 times slower than other crystal planes. This anisotropy allows the grating bars to be etched in 50% by weight KOH at room temperature for up to 60 min. Long etches have several key requirements, including 0.2 degree alignment of the grating with respect to the {111} planes, mask roughness below 40Ȁ- ;nm and minimal defects in the silicon. If these requirements are not met, the grating will quickly be destroyed by the etch, which etches the non-{111} planes in excess of 1 μm per hour. The fabrication steps of this work are described in detail including a novel technique to align the 200 nm-pitch interference lithography image grating to the {111} planes of a 〈110〉 silicon wafer.
    Journal of vacuum science & technology. B, Microelectronics and nanometer structures: processing, measurement, and phenomena: an official journal of the American Vacuum Society 01/2013; 31(6):06FF02-06FF02-9. · 1.36 Impact Factor
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    ABSTRACT: We discuss concepts for high-throughput (effective area 250-1400 cm2), high-resolution (spectral resolving power R > 3500) soft X-ray grating spectroscopy in missions of moderate (probe-class or smaller) scale. Such missions can achieve high-priority scientific objectives identified by the Astro2010 Decadal Survey attainable in no other way, and would provide an essential complement to any future large-area X-ray observatory equipped with non-dispersive spectrometers. We enumerate key science drivers and discuss consequences of various alternative design choices for scientific capability and overall mission size.
    Proc SPIE 09/2012;
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    ABSTRACT: SMART-X is a mission concept for a 2.3 m2 effective area, 0.5" angular resolution X-ray telescope, with 5' FOV, 1" pixel size microcalorimeter, 22' FOV imager, and high-throughput gratings.
    Proc SPIE 09/2012;
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    ABSTRACT: MARX is a portable ray-trace program that was originally developed to simulate event data from the trans- mission grating spectrometers on-board the Chandra X-ray Observatory (CXO). MARX has since evolved to include detailed models of all CXO science instruments and has been further modified to serve as an event simulator for future X-ray observatory design concepts. We first review a number of CXO applications of MARX to demonstrate the roles such a program could play throughout the life of a mission, including its design and calibration, the production of input data products for the development of the various software pipelines, and for observer proposal planning. We describe how MARX was utilized in the design of a proposed future X-ray spectroscopy mission called ÆGIS (Astrophysics Experiment for Grating and Imaging Spectroscopy), a mission concept optimized for the 0.2 to 1 keV soft X-ray band. ÆGIS consists of six independent Critical Angle Transmission Grating Spectrometers (CATGS) arranged to provide a resolving power of 3000 and an effective area exceeding 1000 cm2 across its passband. Such high spectral resolution and effective area will permit ÆGIS to address many astrophysics questions including those that pertain to the evolution of Large Scale Structure of the universe, and the behavior of matter at very high densities. The MARX ray-trace of the ÆGIS spectrometer yields quantitative estimates of how the spectrometer’s performance is affected by misalignments between the various system elements, and by deviations of those elements from their idealized geometry. From this information, we are able to make the appropriate design tradeoffs to maximize the performance of the system.
    Proc SPIE 09/2012;
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    ABSTRACT: Recently developed Critical-Angle Transmission (CAT) grating technology - in combination with x-ray CCD cameras and large collecting-area focusing optics - will enable a new generation of soft x-ray spectrometers with unprecedented resolving power and effective area and with at least an order of magnitude improvement in figures-of-merit for emission and absorption line detection. This technology will be essential to address a number of high-priority questions identified in the Astro2010 Decadal Survey “New Worlds New Horizons” and open the door to a new discovery space. CAT gratings combine the advantages of soft x-ray transmission gratings (low mass, relaxed figure and alignment tolerances, transparent at high energies) and blazed reflection gratings (high broad band diffraction efficiency, utilization of higher diffraction orders to increase resolving power). We report on progress in the fabrication of large-area (31× 31 mm2) free-standing gratings with two levels of low-blockage support structures using highly anisotropic deep reactive-ion etching.
    Proc SPIE 09/2012;
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    ABSTRACT: We developed an instrument design capable of measuring linear X-ray polarization over a broad-band using conventional spectroscopic optics. A set of multilayer-coated flats reflects the dispersed X-rays to the instrument detectors. The intensity variation with position angle is measured to determine three Stokes parameters: I, Q, and U -- all as a function of energy. By laterally grading the multilayer optics and matching the dispersion of the gratings, one may take advantage of high multilayer reflectivities and achieve modulation factors >50% over the entire 0.2 to 0.8 keV band. This instrument could be used in a small orbiting mission or the approach could be used on a large dispersive spectrometric facility. We present progress on laboratory work to demonstrate the capabilities of key components. We thank the MIT Kavli Institute and the NASA Astrophysics Research and Analysis program for funding.
    05/2012;
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    ABSTRACT: A nanofabrication process has been developed for a novel critical-angle transmission grating for astronomical x-ray spectroscopy. The pitch of the gratings is 200 nm and the depth is 4 μm, which exceeds the state-of-the-art in aspect ratio by over a factor of 2 for ultrahigh aspect ratio freestanding nanoscale gratings with open areas on the order of 50% and spanning several square centimeters. They have a broad array of other applications, including neutral mass spectroscopy, ultraviolet filtration, and phase contrast imaging x-ray spectroscopy. The gratings are fabricated as a monolithic structure in silicon via two lithographic and pattern transfer processes, integrated together on a silicon-on-insulator wafer. The grating is patterned via interference lithography and transferred into the 4 μm device layer via a Bosch deep reactive-ion etch (DRIE). The grating channels are then filled without voids by spinning photoresist on them, which wicks into the channels. The sample is then bonded under vacuum via Crystal Bond™ to a carrier wafer, and a honeycomb pattern is etched via DRIE through the handle layer until it stops cleanly on the buried SiO2. The buried SiO2 is etched away, and the sample is separated from the carrier. The resist filling is cleaned from the channels and the grating is critical-point dried to create a freestanding structure. The freestanding gratings can now be mounted to external frames and structurally analyzed and tested for launch and deployment in space.
    Journal of Vacuum Science & Technology B Microelectronics and Nanometer Structures 01/2012; 30(6). · 1.36 Impact Factor
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    ABSTRACT: Future X-ray astronomical missions will need to address a number of important goals such as studying the dynamics of clusters of galaxies, determining how elements are created in the explosions of massive stars, and revealing most of the "normal" matter in the universe which is currently thought to be hidden in hot filaments of gas stretching between galaxies. In order to achieve these goals, spectrometers capable of high resolution and high throughput are necessary for the lowest X-ray energies, 0.3-1.0 keV. We present recent progress in the development of off-plane reflection grating technology for use on upcoming missions. Off-plane grating spectrometers consist of an array of gratings capable of reaching resolutions above 3000 (lambda/Deltalambda). Concept designs have been made for the International X-ray Observatory X-ray Grating Spectrometer. More recently however, we have designed an Optics Module Assembly for WHIMex, an Explorer mission concept that incorporates a Wolter telescope, steering flats, and an array of gratings. This paper will discuss these designs and the application of off-plane arrays for the future.
    Proc SPIE 09/2011;
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    ABSTRACT: A method of thermally shaping individual sheets of glass for the International X-Ray Observatory using porous mandrels as air bearings has been developed, which eliminates the problems of sticking and dust particleinduced distortion which plague traditional slumping methods. A detailed mathematical model of the process has been developed, allowing prediction of final glass shape based on process parameters that include air supply pressure, imperfections on the mandrel surface, glass total thickness variations and gravity vector orientation. Experiments to verify model findings are conducted under closed-loop control of pressure and apparatus tilt. Little improvement in repeatability is seen, suggesting that the error is due to unmodeled forces such as contact forces from the glass holding technique. Finally, the design process and fabrication of a third generation slumping tool is presented. In addition to scaling the design to accomodate larger flats, slumps are done horizontally to float the glass and minimize contact during the process. New capabilities of the tool include active gap measurement and control, as well as plenum air temperature monitoring.
    Proc SPIE 09/2011;
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    ABSTRACT: Diffraction grating-based, wavelength dispersive high-resolution soft x-ray spectroscopy of celestial sources promises to reveal crucial data for the study of the Warm-Hot Intergalactic Medium, the Interstellar Medium, warm absorption and outflows in Active Galactic Nuclei, coronal emission from stars, and other areas of interest to the astrophysics community. Our recently developed critical-angle transmission (CAT) gratings combine the advantages of the Chandra high and medium energy transmission gratings (low mass, high tolerance of misalignments and figure errors, polarization insensitivity) with those of blazed reflection gratings (high broad band diffraction efficiency, high resolution through use of higher diffraction orders) such as the ones on XMM-Newton. Extensive instrument and system configuration studies have shown that a CAT grating-based spectrometer is an outstanding instrument capable of delivering resolving power on the order of 5,000 and high effective area, even with a telescope point-spread function on the order of many arc-seconds. We have fabricated freestanding, ultra-high aspect-ratio CAT grating bars from silicon-on-insulator wafers using both wet and dry etch processes. The 200 nm-period grating bars are supported by an integrated Level 1 support mesh, and a coarser external Level 2 support mesh. The resulting grating membrane is mounted to a frame, resulting in a grating facet. Many such facets comprise a grating array that provides light-weight coverage of large-area telescope apertures. Here we present fabrication results on the integration of CAT gratings and the different high-throughput support mesh levels and on membrane-frame bonding. We also summarize recent x-ray data analysis of 3 and 6 micron deep wet-etched CAT grating prototypes.
    Proc SPIE 09/2011;
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    ABSTRACT: We report on measurements of the diffraction efficiency of 200-nm-period freestanding blazed transmission gratings for wavelengths in the 0.96 to 19.4 nm range. These critical-angle transmission (CAT) gratings achieve highly efficient blazing over a broad band via total external reflection off the sidewalls of smooth, tens of nanometer thin ultrahigh aspect-ratio silicon grating bars and thus combine the advantages of blazed x-ray reflection gratings with those of more conventional x-ray transmission gratings. Prototype gratings with maximum depths of 3.2 and 6 μm were investigated at two different blaze angles. In these initial CAT gratings the grating bars are monolithically connected to a cross support mesh that only leaves less than half of the grating area unobstructed. Because of our initial fabrication approach, the support mesh bars feature a strongly trapezoidal cross section that leads to varying CAT grating depths and partial absorption of diffracted orders. While theory predicts broadband absolute diffraction efficiencies as high as 60% for ideal CAT gratings without a support mesh, experimental results show efficiencies in the range of ∼50-100% of theoretical predictions when taking the effects of the support mesh into account. Future minimization of the support mesh therefore promises broadband CAT grating absolute diffraction efficiencies of 50% or higher.
    Applied Optics 04/2011; 50(10):1364-73. · 1.69 Impact Factor
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    ABSTRACT: We developed an instrument design capable of measuring linear X-ray polarization over a broad-band using conventional spectroscopic optics, using a method previously described by Marshall (2008) involving laterally graded, multilayer-coated flat mirrors. We present possible science investigations with such an instrument and two possible configurations. This instrument could be used in a small orbiting mission or scaled up for the International X-ray Observatory. We will present progress on laboratory work to demonstrate the capabilities of key components. This work has been supported in part under a MIT Kavli Institute instrumentation development grant.
    01/2011;
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    ABSTRACT: Volume x-ray gratings consisting of a multilayer coating deposited on a blazed substrate can diffract with very high efficiency, even in high orders if diffraction conditions in-plane (grating) and out-of-plane (Bragg multilayer) are met simultaneously. This remarkable property, however, depends critically on the ability to create a structure with near atomic perfection. In this Letter we report on a method to produce these structures. We report measurements that show, for a 5000l/mm grating diffracting in the third order, a diffraction efficiency of 37.6% at a wavelength of 13.6nm. This work now shows a direct route to achieving high diffraction efficiency in high order at wavelengths throughout the soft x-ray energy range.
    Optics Letters 08/2010; 35(15):2615-7. · 3.39 Impact Factor
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    ABSTRACT: Multilayer coated blazed gratings with high groove density are the best candidates for use in high resolution EUV and soft x-ray spectroscopy. Theoretical analysis shows that such a grating can be potentially optimized for high dispersion and spectral resolution in a desired high diffraction order without significant loss of diffraction efficiency. In order to realize this potential, the grating fabrication process should provide a perfect triangular groove profile and an extremely smooth surface of the blazed facets. Here we report on recent progress achieved at the Advanced Light Source (ALS) in fabrication of high quality multilayer coated blazed gratings. The blazed gratings were fabricated using scanning beam interference lithography followed by wet anisotropic etching of silicon. A 200 nm period grating coated with a Mo/Si multilayer composed with 30 bi-layers demonstrated an absolute efficiency of 37.6percent in the 3rd diffraction order at 13.6 nm wavelength. The groove profile of the grating was thoroughly characterized with atomic force microscopy before and after the multilayer deposition. The obtained metrology data were used for simulation of the grating efficiency with the vector electromagnetic PCGrate-6.1 code. The simulations showed that smoothing of the grating profile during the multilayer deposition is the main reason for efficiency losses compared to the theoretical maximum. Investigation of the grating with cross-sectional transmission electron microscopy revealed a complex evolution of the groove profile in the course of the multilayer deposition. Impact of the shadowing and smoothing processes on growth of the multilayer on the surface of the sawtooth substrate is discussed.
    Proc SPIE 08/2010;