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Preparation for and Performance of a Pseudomonas aeruginosa Biofilm Experiment On Board the International Space Station

Biofilms are a problem on Earth given their ability to degrade the materials upon which they grow and due to their relevance to infections. Remarkably, 65% and 80% of infections and chronic diseases on Earth are associated with biofilms, respectively. In space, these problems' impact is higher because the crew's lives and mission success depend on nominal operation of mechanical systems. Furthermore, the isolated confined environment nature of spaceflight may increase the rates of disease transmission. In the case of the International Space Station (ISS), biofilms are an identified problem on the Environmental Control and Life Support System (ECLSS), namely on the water processor assembly (WPA). In late 2019, the Space Biofilms experiment launched towards ISS to (i) characterize the mass, thickness, morphology, and gene expression of biofilms formed in space with respect to matched Earth controls, (ii) interrogate the expression of antimicrobial resistance genes, and (iii) test novel materials as potential biofilm control strategies for future ECLSS components. For this, 288 bacterial samples were prepared prior to the launch of the Northrop Grumman CRS-12 mission from NASA's Wallops Flight Facility. The samples were integrated into the spaceflight hardware, BioServe's Fluid Processing Apparatus (FPA) packed in sets of eight in Group Activation Packs (GAP). Half of these samples were activated and terminated on orbit by NASA astronauts Jessica Meir and Christina Koch, while the remaining half were processed equivalently on Earth. The spaceflight bacterial samples of Space Biofilms returned on board SpaceX' CRS-19 Dragon spacecraft, in early 2020. We here describe the test campaign implemented to verify the experiment design and confirm it would enable us to achieve the project's scientific goals. This campaign ended with the Experiment Verification Test (EVT), from which we here present example morphology and transcriptomic results. We describe in detail the sample preparation prior to flight, including cleaning and sterilization of the coupons of six materials (SS316, passivated-SS316, lubricant impregnated surface, catheter-grade silicone with and without a nanotopography, and cellulose membrane), loading and integration of growth media, bacterial inoculum, fixative and preservative to enable experiment termination on orbit. Additionally, we describe the performance of the experiment on board the ISS, including crew activities, use of assets, temperature profile, and experiment timeline; all leading to a successful spaceflight experiment.

Pamela Flores↗
NASA NTRS2003

Wafer-Level Membrane-Transfer Process for Fabricating MEMS

A process for transferring an entire wafer-level micromachined silicon structure for mating with and bonding to another such structure has been devised. This process is intended especially for use in wafer-level integration of microelectromechanical systems (MEMS) that have been fabricated on dissimilar substrates. Unlike in some older membrane-transfer processes, there is no use of wax or epoxy during transfer. In this process, the substrate of a wafer-level structure to be transferred serves as a carrier, and is etched away once the transfer has been completed. Another important feature of this process is that two electrodes constitutes an electrostatic actuator array. An SOI wafer and a silicon wafer (see Figure 1) are used as the carrier and electrode wafers, respectively. After oxidation, both wafers are patterned and etched to define a corrugation profile and electrode array, respectively. The polysilicon layer is deposited on the SOI wafer. The carrier wafer is bonded to the electrode wafer by using evaporated indium bumps. The piston pressure of 4 kPa is applied at 156 C in a vacuum chamber to provide hermetic sealing. The substrate of the SOI wafer is etched in a 25 weight percent TMAH bath at 80 C. The exposed buried oxide is then removed by using 49 percent HF droplets after an oxygen plasma ashing. The SOI top silicon layer is etched away by using an SF6 plasma to define the corrugation profile, followed by the HF droplet etching of the remaining oxide. The SF6 plasma with a shadow mask selectively etches the polysilicon membrane, if the transferred membrane structure needs to be patterned. Electrostatic actuators with various electrode gaps have been fabricated by this transfer technique. The gap between the transferred membrane and electrode substrate is very uniform ( 0.1 m across a wafer diameter of 100 mm, provided by optimizing the bonding control). Figure 2 depicts the finished product.

Yang, Eui-Hyeok↗
NASA NTRS1995

Silicon Micromachining in RF and Photonic Applications

Texas Instruments (TI) has developed membrane and micromirror devices since the late 1970s. An eggcrate space membrane was used as the spatial light modulator in the early years. Discrete micromirrors supported by cantilever beams created a new era for micromirror devices. Torsional micromirror and flexure-beam micromirror devices were promising for mass production because of their stable supports. TI's digital torsional micromirror device is an amplitude modulator (known as the digital micromirror device (DMD) and is in production development, discussed elsewhere. We also use a torsional device for a 4 x 4 fiber-optic crossbar switch in a 2 cm x 2 cm package. The flexure-beam micromirror device is an analog phase modulator and is considered more efficient than amplitude modulators for use in optical processing systems. TI also developed millimeter-sized membranes for integrated optical switches for telecommunication and network applications. Using a member in radio frequency (RF) switch applications is a rapidly growing area because of the micromechanical device performance in microsecond-switching characteristics. Our preliminary membrane RF switch test structure results indicate promising speed and RF switching performance. TI collaborated with MIT for modeling of metal-based micromachining.

Lin, Tsen-Hwang↗
NASA NTRS2003

CO2 Acquisition Membrane (CAM)

The objective of CAM is to develop, test, and analyze thin film membrane materials for separation and purification of carbon dioxide (CO2) from mixtures of gases, such as those found in the Martian atmosphere. The membranes are targeted toward In Situ Resource Utilization (ISRU) applications that will operate in extraterrestrial environments and support future unmanned and human space missions. A primary application is the Sabatier Electrolysis process that uses Mars atmosphere CO2 as raw material for producing water, oxygen, and methane for rocket fuel and habitat support. Other applications include use as an inlet filter to collect and concentrate Mars atmospheric argon and nitrogen gases for habitat pressurization, and to remove CO2 from breathing gases in Closed Environment Life Support Systems (CELSS). CAM membrane materials include crystalline faujasite (FAU) zeolite and rubbery polymers such as silicone rubber (PDMS) that have been shown in the literature and via molecular simulation to favor adsorption and permeation of CO2 over nitrogen and argon. Pure gas permeation tests using commercial PDMS membranes have shown that both CO2 permeance and the separation factor relative to other gases increase as the temperature decreases, and low (Delta)P(Sub CO2) favors higher separation factors. The ideal CO2/N2 separation factor increases from 7.5 to 17.5 as temperature decreases from 22 C to -30 C. For gas mixtures containing CO2, N2, and Ar, plasticization decreased the separation factors from 4.5 to 6 over the same temperature range. We currently synthesize and test our own Na(+) FAU zeolite membranes using standard formulations and secondary growth methods on porous alumina. Preliminary tests with a Na(+) FAU membrane at 22 C show a He/SF6 ideal separation factor of 62, exceeding the Knudsen diffusion selectivity by an order of magnitude. This shows that the membrane is relatively free from large defects and associated non-selective (viscous flow) transport mechanisms. The Membrane Test Facility (MTF) has been developed to measure membrane permeance over a wide range of temperature and pressure. The facility uses two volume compartments separated by the membrane that are instrumented to measure temperature, delta pressure across the membrane, and gas composition. A thermal shroud supports and encloses the membrane, and provides temperature control. Methods were developed to determine membrane permeance using the first order decay of the pressure difference between the sealed compartments, using the total pressure for pure gases, and partial pressure of each species in gas mixtures. The technique provides an end-to-end measurement of gas permeance that includes concentration polarization effects. Experiments have shown that in addition to membrane permeance properties, the geometry and design of associated structures play an important role in how membrane systems will function on Mars.

Mason, Larry W.↗
NASA NTRS2013

Fabrication Methods for Adaptive Deformable Mirrors

Previously, it was difficult to fabricate deformable mirrors made by piezoelectric actuators. This is because numerous actuators need to be precisely assembled to control the surface shape of the mirror. Two approaches have been developed. Both approaches begin by depositing a stack of piezoelectric films and electrodes over a silicon wafer substrate. In the first approach, the silicon wafer is removed initially by plasmabased reactive ion etching (RIE), and non-plasma dry etching with xenon difluoride (XeF2). In the second approach, the actuator film stack is immersed in a liquid such as deionized water. The adhesion between the actuator film stack and the substrate is relatively weak. Simply by seeping liquid between the film and the substrate, the actuator film stack is gently released from the substrate. The deformable mirror contains multiple piezoelectric membrane layers as well as multiple electrode layers (some are patterned and some are unpatterned). At the piezolectric layer, polyvinylidene fluoride (PVDF), or its co-polymer, poly(vinylidene fluoride trifluoroethylene P(VDF-TrFE) is used. The surface of the mirror is coated with a reflective coating. The actuator film stack is fabricated on silicon, or silicon on insulator (SOI) substrate, by repeatedly spin-coating the PVDF or P(VDFTrFE) solution and patterned metal (electrode) deposition. In the first approach, the actuator film stack is prepared on SOI substrate. Then, the thick silicon (typically 500-micron thick and called handle silicon) of the SOI wafer is etched by a deep reactive ion etching process tool (SF6-based plasma etching). This deep RIE stops at the middle SiO2 layer. The middle SiO2 layer is etched by either HF-based wet etching or dry plasma etch. The thin silicon layer (generally called a device layer) of SOI is removed by XeF2 dry etch. This XeF2 etch is very gentle and extremely selective, so the released mirror membrane is not damaged. It is possible to replace SOI with silicon substrate, but this will require tighter DRIE process control as well as generally longer and less efficient XeF2 etch. In the second approach, the actuator film stack is first constructed on a silicon wafer. It helps to use a polyimide intermediate layer such as Kapton because the adhesion between the polyimide and silicon is generally weak. A mirror mount ring is attached by using adhesive. Then, the assembly is partially submerged in liquid water. The water tends to seep between the actuator film stack and silicon substrate. As a result, the actuator membrane can be gently released from the silicon substrate. The actuator membrane is very flat because it is fixed to the mirror mount prior to the release. Deformable mirrors require extremely good surface optical quality. In the technology described here, the deformable mirror is fabricated on pristine substrates such as prime-grade silicon wafers. The deformable mirror is released by selectively removing the substrate. Therefore, the released deformable mirror surface replicates the optical quality of the underlying pristine substrate.

Toda, Risaku↗
NASA NTRS1991

Integrated 119-micron linear corner-cube array

An integrated corner-cube antenna has been designed, fabricated, and measured at 119 microns. The structure consists of a traveling-wave antenna integrated on a 1-micron dielectric membrane and suspended in a longitudinal cavity etched in silicon wafers. The patterns at 119 microns agree well with millimeter-wave patterns measured on a scaled antenna at 222 GHz. A directivity of 18 +/- 0.5 dB is calculated from E- and H-plane measurements. This work demonstrates that high-efficiency integrated corner-cube antennas are easily scalable to terahertz frequencies and could be used for radio-astronomical and plasma-diagnostic applications.

Gearhart, Steven S.↗
NASA NTRS2009

Fabrication of an Antenna-Coupled Bolometer for Cosmic Microwave Background Polarimetry

We describe the development of a detector for precise measurements of the cosmic microwave background polarization. The detector employs a waveguide to couple light between a pair of Mo/Au superconducting transition edge sensors (TES) and a feedhorn. Incorporation of an on-chip ortho-mode transducer (OMT) results in high isolation. The OMT is micromachined and bonded to the microstrip and TES circuits in a low temperature wafer bonding process. The wafer bonding process incorporates a buried superconducting niobium layer with a single crystal silicon layer which serves as the leg isolated TES membrane and as the microstrip dielectric. We describe the micromachining and wafer bonding process and report measurement results of the microwave circuitry operating in the 29-43GHz band along with Johnson noise measurements of the TES membrane structures and development of Mo/Au TES operating under '00mK.

Denis, K.L.↗
NASA NTRS2009

Microwell arrays with nanoholes

A device for conducting parallel analysis or manipulation of multiple cells or biomolecules is disclosed. In one embodiment, the device comprises a silicon chip with a microwell, and at least one membrane suspended at the bottom opening of the microwell. The suspended portion of the membrane defines a nanohole that provides access to the material on the other side of the membrane.

Folch, Albert↗
NASA NTRS2002

CARES/Life Used for Probabilistic Characterization of MEMS Pressure Sensor Membranes

Microelectromechanical systems (MEMS) devices are typically made from brittle materials such as silicon using traditional semiconductor manufacturing techniques. They can be etched (or micromachined) from larger structures or can be built up with material deposition processes. Maintaining dimensional control and consistent mechanical properties is considerably more difficult for MEMS because feature size is on the micrometer scale. Therefore, the application of probabilistic design methodology becomes necessary for MEMS. This was demonstrated at the NASA Glenn Research Center and Case Western Reserve University in an investigation that used the NASA-developed CARES/Life brittle material design program to study the probabilistic fracture strength behavior of single-crystal SiC, polycrystalline SiC, and amorphous Si3N4 pressurized 1-mm-square thin-film diaphragms. These materials are of interest because of their superior high-temperature characteristics, which are desirable for harsh environment applications such as turbine engine and rocket propulsion system hot sections.

Nemeth, Noel N.↗
NASA NTRS2004

Curved-Focal-Plane Arrays Using Deformed-Membrane Photodetectors

A versatile and simple approach to the design and fabrication of curved-focal-plane arrays of silicon-based photodetectors is being developed. This approach is an alternative to the one described in "Curved Focal-Plane Arrays Using Back- Illuminated High-Purity Photodetectors" (NPO-30566), NASA Tech Briefs, Vol. 27, No. 10 (October 2003), page 10a. As in the cited prior article, the basic idea is to improve the performance of an imaging instrument and simplify the optics needed to obtain a given level of performance by making an image sensor (in this case, an array of photodetectors) conform to a curved focal surface, instead of designing the optics to project an image onto a flat focal surface. There is biological precedent for curved-focal-surface designs: retinas - the image sensors in eyes - conform to the naturally curved focal surfaces of eye lenses. The present approach is applicable to both front-side- and back-side-illuminated, membrane photodetector arrays and is being demonstrated on charge-coupled devices (CCDs). The very-large scale integrated (VLSI) circuitry of such a CCD or other array is fabricated on the front side of a silicon substrate, then the CCD substrate is attached temporarily to a second substrate for mechanical support, then material is removed from the back to obtain the CCD membrane, which typically has a thickness between 10 and 20 m. In the case of a CCD designed to operate in back-surface illumination, delta doping can be performed after thinning to enhance the sensitivity. This approach is independent of the design and method of fabrication of the front-side VLSI circuitry and does not involve any processing of a curved silicon substrate. In this approach, a third substrate would be prepared by polishing one of its surfaces to a required focal-surface curvature. A CCD membrane fabricated as described above would be pressed against, deformed into conformity with, and bonded to, the curved surface. The technique used to press and bond the CCD membrane would depend on the nature of the supporting material (see figure). For example, if the third substrate were made of quartz frit, the substrate would be prepared by suffusing it with epoxy. Then one would take advantage of the porosity of the frit by applying a partial vacuum to the opposite surface of the frit, causing atmospheric pressure to push the CCD membrane against the curved surface. The curing of the epoxy would bond the CCD membrane to the curved surface. Alternatively, if the third substrate were made of a nonporous material, the curved substrate surface would be prepared by coating it with a wax or an uncured epoxy. The CCD membrane would be pressed against the coated, curved surface by use of a suitably pressurized balloon. The CCD membrane would then become bonded to the curved surface by curing of the epoxy or freezing of the wax.

Nikzad, Shouleh↗
NASA NTRS1991

Integrated 222-GHz corner-reflector antennas

A high-gain monolithic millimeter-wave antenna has been designed, fabricated, and tested at 222 GHz. The structure consists of a traveling-wave antenna integrated on a 1.2-micron dielectric membrane and suspended in a longitudinal cavity etched in a silicon wafer. A new traveling-wave antenna design yields a wideband input impedance and a low cross-polarization component in the E- and quasi-H-plane patterns. A directivity of 17.7 dB and a main-beam efficiency of 88.5 percent are calculated from the 222-GHz pattern measurements. The integrated corner-reflector antenna is well suited for millimeter- and submillimeter-wave imaging applications in large f-number systems.

Gearhart, Steven S.↗
NASA NTRS1991

Integrated millimeter-wave corner-cube antennas

An integrated corner-reflector antennas has been designed, fabricated, and measured at millimeter-wave frequencies. The structure consists of a traveling-wave antenna integrated on a 1.2-micron dielectric membrane, and suspended in a longitudinal cavity etched in a silicon wafer. A novel traveling wave antenna design, the modified-bend antenna, with an antenna length of 1.2 lambda and spacing 0.96 lambda from the apex, results in a wideband input impedance centered at 140 Ohm and low cross-polarization levels. Measurements at 180-270 GHz show a well-defined pattern with low sidelobe levels, and a main-beam efficiency of 93 percent and 83 percent at 180 and 222 GHz, respectively. The monolithic approach allows the integration of a matching network and a Schottky-diode or SIS detector at the base of the antenna to yield a low-noise monolithic millimeter-wave receiver.

Gearhart, Steven S.↗
NASA NTRS1995

Micromachined Silicon Waveguide Circuits

Rectangular waveguides are commonly used as circuit elements in remote-sensing heterodyne receivers at millimeter wavelengths. The advantages of waveguides are low loss and mechanical tunability. However, conventional machining techniques for waveguide components operating above a few hundred GHz are complicated and costly. Waveguides micromachined from silicon however would have several important advantages including low-cost; small size for very high frequency (submillimeter wave) operation; high dimensional accuracy (important for high-Q circuits); atomically smooth walls, thereby reducing rf losses; and the ability to integrate active and passive devices directly in the waveguide on thin membranes, thereby solving the traditional problem of mounting thin substrates.

Silicon Waveguide↗
NASA NTRS2008

Progress in Development of Improved Ion-Channel Biosensors

Further improvements have recently been made in the development of the devices described in Improved Ion-Channel Biosensors (NPO-30710), NASA Tech Briefs, Vol. 28, No. 10 (October 2004), page 30. As discussed in more detail in that article, these sensors offer advantages of greater stability, greater lifetime, and individual electrical addressability, relative to prior ion-channel biosensors. In order to give meaning to a brief description of the recent improvements, it is necessary to recapitulate a substantial portion of the text of the cited previous article. The figure depicts one sensor that incorporates the recent improvements, and can be helpful in understanding the recapitulated text, which follows: These sensors are microfabricated from silicon and other materials compatible with silicon. Typically, the sensors are fabricated in arrays in silicon wafers on glass plates. Each sensor in the array can be individually electrically addressed, without interference with its neighbors. Each sensor includes a well covered by a thin layer of silicon nitride, in which is made a pinhole for the formation of a lipid bilayer membrane. In one stage of fabrication, the lower half of the well is filled with agarose, which is allowed to harden. Then the upper half of the well is filled with a liquid electrolyte (which thereafter remains liquid) and a lipid bilayer is painted over the pinhole. The liquid contains a protein that forms an ion channel on top of the hardened agarose. The combination of enclosure in the well and support by the hardened agarose provides the stability needed to keep the membrane functional for times as long as days or even weeks. An electrode above the well, another electrode below the well, and all the materials between the electrodes together constitute a capacitor. What is measured is the capacitive transient current in response to an applied voltage pulse. One notable feature of this sensor, in comparison with prior such sensors, is a relatively thick dielectric layer between the top of the well and the top electrode. This layer greatly reduces the capacitance of an aperture across which the ion channels are formed, thereby increasing the signal-to-noise ratio. The use of a relatively large aperture with agarose support makes it possible to form many ion channels instead of only one, thereby further increasing the signal-to-noise ratio and effectively increasing the size of the available ionic reservoir. The relatively large reservoir makes it possible to measure AC rather than DC. This concludes the recapitulation from the cited previous article.

Nadeau, Jay L.↗
NASA NTRS1993

Quantitative Mapping of Pore Fraction Variations in Silicon Nitride Using an Ultrasonic Contact Scan Technique

An ultrasonic scan procedure using the pulse-echo contact configuration was employed to obtain maps of pore fraction variations in sintered silicon nitride samples in terms of ultrasonic material properties. Ultrasonic velocity, attenuation coefficient, and reflection coefficient images were obtained simultaneously over a broad band of frequencies (e.g., 30 to 110 MHz) by using spectroscopic analysis. Liquid and membrane (dry) coupling techniques and longitudinal and shear-wave energies were used. The major results include the following: Ultrasonic velocity (longitudinal and shear wave) images revealed and correlated with the extent of average through-thickness pore fraction variations in the silicon nitride disks. Attenuation coefficient images revealed pore fraction nonuniformity due to the scattering that occurred at boundaries between regions of high and low pore fraction. Velocity and attenuation coefficient images were each nearly identical for machined and polished disks, making the method readily applicable to machined materials. Velocity images were similar for wet and membrane coupling. Maps of apparent Poisson's ratio constructed from longitudinal and shear-wave velocities quantified Poisson's ratio variations across a silicon nitride disk. Thermal wave images of a disk indicated transient thermal behavior variations that correlated with observed variations in pore fraction and velocity and attenuation coefficients.

Roth, Don J.↗
NASA NTRS2011

Microfabrication of a High-Throughput Nanochannel Delivery/Filtration System

A microfabrication process is proposed to produce a nanopore membrane for continuous passive drug release to maintain constant drug concentrations in the patient s blood throughout the delivery period. Based on silicon microfabrication technology, the dimensions of the nanochannel area, as well as microchannel area, can be precisely controlled, thus providing a steady, constant drug release rate within an extended time period. The multilayered nanochannel structures extend the limit of release rate range of a single-layer nanochannel system, and allow a wide range of pre-defined porosity to achieve any arbitrary drug release rate using any preferred nanochannel size. This membrane system could also be applied to molecular filtration or isolation. In this case, the nanochannel length can be reduced to the nanofabrication limit, i.e., 10s of nm. The nanochannel delivery system membrane is composed of a sandwich of a thin top layer, the horizontal nanochannels, and a thicker bottom wafer. The thin top layer houses an array of microchannels that offers the inlet port for diffusing molecules. It also works as a lid for the nanochannels by providing the channels a top surface. The nanochannels are fabricated by a sacrificial layer technique that obtains smooth surfaces and precisely controlled dimensions. The structure of this nanopore membrane is optimized to yield high mechanical strength and high throughput.

Ferrari, Mauro↗
NASA NTRS2010

Solid-state curved focal plane arrays

The present invention relates to curved focal plane arrays. More specifically, the present invention relates to a system and method for making solid-state curved focal plane arrays from standard and high-purity devices that may be matched to a given optical system. There are two ways to make a curved focal plane arrays starting with the fully fabricated device. One way, is to thin the device and conform it to a curvature. A second way, is to back-illuminate a thick device without making a thinned membrane. The thick device is a special class of devices; for example devices fabricated with high purity silicon. One surface of the device (the non VLSI fabricated surface, also referred to as the back surface) can be polished to form a curved surface.

Nikzad, Shouleh↗
NASA NTRS1979

Strong thin membrane structure

A continuous process is described for producing strong lightweight structures for use as solar sails for spacecraft propulsion by radiation pressure. A thin reflective coating, such as aluminum, is applied to a rotating cylinder. A nylon mesh, applied over the aluminum coating, is then coated with a polymerizing material such as a para-xylylene monomer gas to polymerize as a film bound to the mesh and the aluminum. An emissivity increasing material such as chromium or silicon monoxide is applied to the polymer film to disperse such material colloidally into the growing polymer film, or to the final polymer film. The resulting membrane structure is then removed from the cylinder. Alternately, the membrane structure can be formed by etching a substrate in the form of an organic film such as a polymide, or a metal foil, to remove material from the substrate and reduce its thickness. A thin reflective coating (aluminum) is applied on one side of the substrate, and an emissivity increasing coating is applied on the reverse side of the substrate.

Frazer, R. E.↗