Alexander R. Bruccoleri

Plasma etch fabrication of 60:1 aspect ratio silicon nanogratings with 200 nm pitch

The authors present a breakthrough multistage dry-etch process to create 100 nm half-pitch gratings in silicon with depths up to 6 μm. Interference lithography was used to pattern gratings in an optically matched stack of materials to form a 400-nm-thick silicon oxide hard-mask. The oxide was then used to mask the subsequent deep reactive-ion etching of silicon. In this article, the authors describe their grating patterning, pattern transfer, and deep etch processes, and present progress toward combining this technique with coarser scale lithography steps designed to form an integrated mechanical support structure to produce freestanding x-ray diffraction gratings.

Fabrication of nanoscale, high throughput, high aspect ratio freestanding gratings

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 vi...

Stress control of plasma enhanced chemical vapor deposited silicon oxide film from tetraethoxysilane

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.

Potassium hydroxide polishing of nanoscale deep reactive-ion etched ultrahigh aspect ratio gratings

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 ...

The Marshall Grazing Incidence X-Ray Spectrometer (MaGIXS)

The Marshall Grazing Incidence X-ray Spectrograph (MaGIXS) is a proposed sounding rocket experiment designed to observe spatially resolved soft X-ray spectra of the solar corona for the first time. The instrument is a purely grazing-incidence design, consisting of aWolter Type-1 sector telescope and a slit spectrograph. The telescope mirror is a monolithic Zerodur mirror with both the parabolic and hyperbolic surfaces. The spectrograph comprises a pair of paraboloid mirrors acting as a collimator and reimaging mirror, and a planar varied-line-space grating, with reflective surfaces operate at a graze angle of 2 degrees. This produces a flat spectrum on a detector covering a wavelength range of 6-24Å (0.5-1.2 keV). The design achieves 20 mÅ spectral resolution (10 mÅ /pixel) and 5 arcsec spatial resolution (2.5 arcsec / pixel) over an 8-arcminute long slit. The spectrograph is currently being fabricated as a laboratory prototype. A flight candidate telescope mirror is also under development.

Fabrication process for 200 nm-pitch polished freestanding ultrahigh aspect ratio gratings

A fully integrated fabrication process has been developed to fabricate freestanding, ultrahigh aspect ratio silicon gratings with potassium hydroxide (KOH)-polished sidewalls. The gratings are being developed for wavelength-dispersive, soft x-ray spectroscopy on future space telescopes. For this application, the grating needs to have a large open-area fraction and smooth sidewalls (roughness < 1 nm) to maximize efficiency. The prototype gratings fabricated with the process presented here have been tested on a synchrotron beamline and have demonstrated an absolute diffraction efficiency greater than 30% for 2 nm-wavelength x-rays in blazed orders. This efficiency is greater than twice the efficiency of previously fabricated gratings. The fabrication process utilizes silicon-on-insulator wafers where the grating and a cross support are etched in the device layer, and an additional structural support is etched in the handle layer. The device layer and handle layer are both etched via deep reactive-ion etchin...

Critical-angle x-ray transmission grating spectrometer with extended bandpass and resolving power > 10,000

A number of high priority subjects in astrophysics can be addressed by a state-of-the-art soft x-ray grating spectrometer, such as the role of Active Galactic Nuclei in galaxy and star formation, characterization of the Warm-Hot Intergalactic Medium and the missing baryon problem, characterization of halos around the Milky Way and nearby galaxies, as well as stellar coronae and surrounding winds and disks. An Explorer-scale, largearea (> 1,000 cm2), high resolving power (R =λ/Δλ > 3,000) soft x-ray grating spectrometer is highly feasible based on Critical-Angle Transmission (CAT) grating technology, even for telescopes with angular resolution of 5-10 arcsec. Still, significantly higher performance can be provided by a CAT grating spectrometer on an X-ray- Surveyor-type mission. CAT gratings combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (lowmass, relaxed alignment tolerances and temperature requirements, transparent at higher energies) with minimalmission resource requirements. They are high-efficiency blazed transmission gratings that consist of freestanding, ultra-high aspect-ratio grating bars fabricated from silicon-on-insulator (SOI) wafers using advanced anisotropic dry and wet etch techniques. Blazing is achieved through grazing-incidence reflection off the smooth grating bar sidewalls. The reflection properties of silicon are well matched to the soft x-ray band, and existing silicon CAT gratings can exceed 30% absolute diffraction efficiency, with clear paths for further improvement. Nevertheless, CAT gratings with sidewalls made of higher atomic number elements allow extension of the CAT grating principle to higher energies and larger dispersion angles, thus enabling higher resolving power at shorter wavelengths. We show x-ray data from CAT gratings coated with a thin layer of platinum using atomic layer deposition, and demonstrate efficient blazing to higher energies and much larger blaze angles than possible with silicon alone. We also report on measurements of the resolving power of a breadboard CAT grating spectrometer consisting of a Wolter-I slumped-glass focusing mirror pair from Goddard Space Flight Center and CAT gratings, performed at the Marshall Space Flight Center Stray Light Facility. Measurement of the Al Kα doublet in 18th diffraction order shows resolving power > 10,000, based on conservative preliminary analysis. This demonstrates that currently fabricated CAT gratings are compatible with the most advanced grating spectrometer instrument designs for future soft x-ray spectroscopy missions.

High-efficiency blazed transmission gratings for high-resolution soft x-ray spectroscopy

High-resolution spectroscopy of astrophysical sources is the key to gaining a quantitative understanding of the history, dynamics, and current conditions of the cosmos. A large-area (> 1,000 cm2), high resolving power (R = λ/Δλ> 3000) soft x-ray grating spectrometer (XGS) that covers the lines of C, N, O, Ne and Fe ions is the ideal tool to address a number of high-priority science questions from the 2010 Decadal Survey, such as the connection between super-massive black holes and large-scale structure via cosmic feedback, the evolution of large- scale structure, the behavior of matter at high densities, and the conditions close to black holes. While no grating missions or instruments are currently approved, an XGS aboard a potential future X-ray Surveyor could easily surpass the above performance metrics. To improve the chances for future soft x-ray grating spectroscopy missions or instruments, grating technology has to progress and advance to higher Technology Readiness Levels (TRLs). To that end we have developed Critical-Angle Transmission (CAT) gratings that combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (low mass, relaxed alignment tolerances and temperature requirements, high transparency at higher energies). A CAT grating-based spectrometer can provide performance 1-2 orders of magnitude better than current grating instruments on Chandra and Newton-XMM with minimal resource requirements. At present we have fabricated large-area freestanding CAT gratings with narrow integrated support structures from silicon-on- insulator wafers using advanced lithography and a combination of deep reactive-ion and wet etching. Our latest x-ray test results show record high absolute diffraction efficiencies in blazed orders in excess of 30% with room for improvement.

Nanofabrication advances for high efficiency critical-angle transmission gratings

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.

Critical-angle transmission grating technology development for high resolving power soft x-ray spectrometers on Arcus and Lynx

Soft x-ray spectroscopy with high resolving power (R = λ/Δλ) and large effective area (A) addresses numerous unanswered science questions about the physical laws that lead to the structure of our universe. In the soft x-ray band R > 1000 can currently only be achieved with diffraction grating-based spectroscopy. Criticalangle transmission (CAT) gratings combine the advantages of blazed reflection gratings (high efficiency, use of higher diffraction orders) with those of conventional transmission gratings (relaxed alignment tolerances and temperature requirements, transparent at higher energies, low mass), resulting in minimal mission resource requirements, while greatly improving figures of merit. Diffraction efficiency > 33% and R > 10, 000 have been demonstrated for CAT gratings. Last year the technology has been certified at Technology Readiness Level 4 based on a probe class mission concept. The Explorer-scale (A > 450 cm2 , R > 2500) grating spectroscopy Arcus mission can be built with todays CAT grating technology and has been selected in the current Explorer round for a Phase A concept study. Its figure of merit for the detection of weak absorption lines will be an order of magnitude larger than current instruments on Chandra and XMM-Newton. Further CAT grating technology development and improvements in the angular resolution of x-ray optics can provide another order of magnitude improvement in performance, as is envisioned for the X-ray Surveyor/Lynx mission concept currently under development for input into the 2020 Decadal Survey. For Arcus we have tested CAT gratings in a spectrometer setup in combination with silicon pore optics (SPO) and obtained resolving power results that exceed Arcus requirements before and after environmental testing of the gratings. We have recently fabricated the largest (32 mm x 32 mm) CAT gratings to date, and plan to increase grating size further. We mounted two of these large gratings to frames and aligned them in the roll direction using a laser-based technique. Simultaneous x-ray illumination of both gratings with an SPO module demonstrated that we can exceed Arcus grating-to-grating alignment requirements without x rays.