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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Materials Combustion Testing and Combustion Product Sensor Evaluations in FY12

NASA Centers continue to collaborate to characterize the chemical species and smoke particles generated by the combustion of current space-rated non-metallic materials including fluoropolymers. This paper describes the results of tests conducted February through September 2012 to identify optimal chemical markers both for augmenting particle-based fire detection methods and for monitoring the post-fire cleanup phase in human spacecraft. These studies follow up on testing conducted in August 2010 and reported at ICES 2011. The tests were conducted at the NASA White Sands Test Facility in a custom glove box designed for burning fractional gram quantities of materials under varying heating profiles. The 623 L chamber was heavily instrumented to quantify organics (gas chromatography/mass spectrometry), inorganics by water extraction followed by ion chromatography, and select species by various individual commercially-available sensors. Evaluating new technologies for measuring carbon monoxide, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and other species of interest was a key objective of the test. Some of these sensors were located inside the glovebox near the fire source to avoid losses through the sampling lines; the rest were located just outside the glovebox. Instruments for smoke particle characterization included a Tapered Element Oscillating Microbalance Personal Dust Monitor (TEOM PDM) and a TSI Dust Trak DRX to measure particle mass concentration, a TSI PTrak for number concentration and a thermal precipitator for collection of particles for microscopic analysis. Materials studied included Nomex®, M22759 wire insulation, granulated circuit board, polyvinyl chloride (PVC), Polytetrafluoroethylene (PTFE), Kapton®, and mixtures of PTFE and Kapton®. Furnace temperatures ranged from 340o to 640o C, focusing on the smoldering regime. Of particular interest in these tests was confirming burn repeatability and production of acid gases with different fuel mixture compositions, as well as the dependence of aerosol concentrations on temperature.

Smoke↗
NASA NTRS2013

Materials Combustion Testing and Combustion Product Sensor Evaluations in FY12

NASA Centers continue to collaborate to characterize the chemical species and smoke particles generated by the combustion of current space-rated non-metallic materials including fluoropolymers. This paper describes the results of tests conducted February through September 2012 to identify optimal chemical markers both for augmenting particle-based fire detection methods and for monitoring the post-fire cleanup phase in human spacecraft. These studies follow up on testing conducted in August 2010 and reported at ICES 2011. The tests were conducted at the NASA White Sands Test Facility in a custom glove box designed for burning fractional gram quantities of materials under varying heating profiles. The 623 L chamber was heavily instrumented to quantify organics (gas chromatography/mass spectrometry), inorganics by water extraction followed by ion chromatography, and select species by various individual commercially-available sensors. Evaluating new technologies for measuring carbon monoxide, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and other species of interest was a key objective of the test. Some of these sensors were located inside the glovebox near the fire source to avoid losses through the sampling lines; the rest were located just outside the glovebox. Instruments for smoke particle characterization included a Tapered Element Oscillating Microbalance Personal Dust Monitor (TEOM PDM) and a TSI Dust Trak DRX to measure particle mass concentration, a TSI PTrak for number concentration and a thermal precipitator for collection of particles for microscopic analysis. Materials studied included Nomex(R), M22759 wire insulation, granulated circuit board, polyvinyl chloride (PVC), Polytetrafluoroethylene (PTFE), Kapton(R), and mixtures of PTFE and Kapton(R). Furnace temperatures ranged from 340 to 640 C, focusing on the smoldering regime. Of particular interest in these tests was confirming burn repeatability and production of acid gases with different fuel mixture compositions, as well as the dependence of aerosol concentrations on temperature.

Combustion↗
NASA NTRS2019

Further Development Of Aperture: A Precise Extremely Large Reflective Telescope Using Re-Configurable Elements: NASA Innovative Advanced Concepts (NIAC) - Phase II

One of the pressing needs for space ultraviolet-visible astronomy is a design to allow larger mirrors than the James Webb Space Telescope primary. The diameter of the rocket fairing limits the mirror diameter such that all future missions calling for mirrors up to 16 meters in diameter or larger will require a mirror that is deployed post-launch. In response to the deployment requirement, we address the issues of this concept called "A Precise Extremely Large Reflective Telescope Using Reconfigurable Elements (APERTURE) with both hardware experiments and software simulations... We designed and built several fixtures with O-rings to hold a membrane. We established a coating process to make a membrane that was coated on one side with Cr and the other side with Cr-Terfenol-D-NiCo. The Terfenol-D (T-D hereafter) is the MSM (Magnetic Smart Memory) we use. We bought and established a procedure for measuring a deformation over time and purchased a Shack Hartmann system from Imagine Optic (https://www.imagine-optic.com). The first substrate we used was DuPont (TM) Kapton® polyimide film. Due to material creep, we found the stability over a 48-hour period with a Kapton substrate was not as good as desired (greater than 1 micron). We then switched to CP1 Polyimide. We found the CP1 much more stable to creep, being stable from about 3 hours to 48 hours to within a measurement error to below approximately 0.1 micron. We produced a 13 micron maximum deviation on a 50-millimeter-diameter piece of CP1 (25 microns thick). The T-D coating was about 2 microns, and the other layers, about 10 nanometers. The magnetic field at the base was about 0.1 teslas. We can make the T-D film at least 5 times thicker and the magnetic field at least 5 times stronger, and hence make deformations as much as 25 times larger. We have a formed a collaboration produced at the NIAC (NASA Innovative Advanced Concepts) mid-term review with Dr. Ron Shiri of Goddard Space Flight Center (GSFC) to explore making controlled deviations on lambda/14-lambda/20 scales which are required to bring a surface to the diffraction limit. We carried out only preliminary work on Si using a Coordinate Measuring Machine (CMM), which produced deviations on the 1 micron level. We are still working on a program to bring to GSFC a flat enough (radius of curvature greater than 10 microns) -coated a Si piece with Cr, T-D, NiCo. Then we plan to carry out tests with an interferometer. Further, we formed a new collaboration with Prof. Rajan Vaidyanathan of the University of Central Florida to replace the CP1 with a shape memory alloy (SMA). With his collaboration, we acquired new Federal funding outside of NASA to explore the use of SMAs (we use NiTi). Our preliminary results indicate that we can produce deformations greater than 1 micron on approximately 100 microns thick. Furthermore we have shown that the NiTi can deploy to better than 1 micron of its set original and then trained shape.

Re-Configurable Elements↗
NASA NTRSDate not supplied

TPSAS-NF1676L-32151-DND

Sail Quadrants (Beginning): - Previous quadrants that were made used a Mylar material with tape used for seams and edges - Heat seaming with just the sail material was proving to be difficult and ineffective - Seaming with the meltable adhesives had not been adequately tested for use as an option Sail Quadrants (Ending): - Experimenting with meltable adhesives proved they were viable to be used in sail creation adhesives proved they were viable - Created 6 full size quadrants (2 Kapton and 4 PEN) using the new seaming methods - Created a detailed procedure defining the process for sail quadrant creation from initial material set up to final rolling onto a spool - Quadrants were used for direct comparison of weight and volume between a Kapton or PEN based sail

Randall Barfield↗
NASA NTRSDate not supplied

Short Circuiting the Controller – Missteps in Maintenance and Inspection of Process and Wiring in STS-93

The primary objective of the Space Transportation System mission 93 (STS-93) was to deploy the Chandra X-Ray Observatory. Chandra, the world's most powerful X-Ray telescope, allowed scientists from around the world to study some of the most distant and dynamic objects in the universe. Stripped of nearly 7,000 pounds of its own gear to make room for the payload, the orbiter assigned to this mission was Space Shuttle Columbia. Prior to STS-93, Columbia had flown 25 flights and was NASA's oldest and heaviest orbiter. On July 23, 1999, after two prior launch scrubs, Eileen Collins and her crew of four launched from Kennedy Space Center. About five seconds after launch, Mission Control at Johnson Space Center detected a voltage drop on one of Columbia's electrical buses. As a result of this power fluctuation, a primary and back-up Main Engine controller dropped offline. Given design redundancy, the two remaining controllers supported all three engines. If there had been any other AC bus issues, one engine of the three on the Orbiter would have shut down. The redundant set of digital computer units in each engine controller saved Columbia and her crew from a very risky contingency abort. Post-flight inspection revealed soot on a screw head and a hole in an adjacent Kapton insulated wire. The single strand of polyimide wire was located nearly half-way down the payload bay. The Shuttle Independent Assessment Team (SIAT) reported that the wire had rubbed and chaffed against a burred screw head. The burr was later determined to be the result of overtightening of the screw by a technician during a maintenance refurbishment. Alone, the burr may not have been problematic, but later, during another ground processing event, possibly years after, someone inadvertently stepped on the wiring harness. With the pressure and motion of unintended contact, some of the Kapton insulation rubbed off against the burred screw head. The SIAT suspected the wire damage was pre-existing and was caused 4 or 5 years prior to the flight. Finally, the intense vibrations during the launch sequence allowed contact between the exposed conductor and exposed metal area on the burred screw head, resulting in the arcing and shorting of the wire. Due to the quick turnaround times of Space Shuttle Orbiters, wiring issues caused from multiple maintenance events were often overlooked. Additionally, failing to incorporate thorough and early inclusion of human systems integration (HSI) applications as a crucial part of the decision process can result in these types of misshaps. In order to reduce human error associated with integrated manufacturing, maintenance, refurbishment and flight preparations, wire inspection criteria should be refined and standardized, visual inspection processes should be quantified, and technicians should be certified by specially trained instructors. This case, among many others, unveils why human error management and development of safety metrics is a vital piece in the development of complex systems, and why it should be supported aggressively and implemented program wide.

Human Systems Integration↗
NASA NTRS1995

Test-Derived Effective Emittance for Cassini MLI Blankets and Heat Loss Characteristics in the Vicinity of Seams

Thermal performance of Cassini MLI blankets was characterized in thermal vacuum tests. Effective emittance was derived for the standard and high-temperature layups, with or without micrometeoroid protection standoffs, and for a high-performance duo-layup with staggered seams. The all-Kapton layup wa shown to have a 19% higher effective emittance than the hybrid Kapton-Mylar layup, and the duo-layup exhibited a dramatic capability of reducing heat dissipation by 2.6 fold. Several different definitions of effective emittance are discussed, and their relations to distinct hardware-MLI configurations and corresponding modeling techniques clarified. Large temperature differences (up to 70 C) were observed between the center and seam of a blanket. Heat losses in the vicinity of seams are qualified, and a major MLI heat loss mechanism elucidated.

Cassini↗
NASA NTRS1995

Cassini MLI Blankets High Temperature Exposure Tests

The Saturn-bound Cassini spacecraft will be subjected to a high temperature environment at 0.61 AU. Thermal vacuum tests demonstrated that the hybrid Kapton-Mylar MLI layup can withstand an outer layer temperature of 250 degrees Centigrade without incurring any damage, and the all Kapton layup, 430 degrees Centigrade. The latter will be applied to locales of extremely high temperatures, while the former more than 85 percent of the spacecraft's blanketed surfaces.

Cassini↗
NASA NTRSDate not supplied

Evaluation of Coatings for the Electrodynamic Dust Shield Application on Thermal Radiators

Dust acts as a blackbody, becoming hot if left in direct sunlight. This is a problem for thermal radiators where the main function is to radiate heat away from an object. If dust lands on the thermal radiator, the unit will less effectively reject heat, and it will overheat. This can lead to electrical or system failure. The current state-of-the-art in active dust mitigation is the Electrodynamic Dust Shield (EDS) which uses an electric field generated by alternating high positive and negative voltages (low current) to eject the charged dust off surfaces. An EDS made from copper coated Kapton is an ideal candidate to be bonded to a thermal radiator and coated with a low solar absorptance, high heat-emitter coating. This work compares the dust removal of copper-Kapton EDSs covered with different thermal radiator coatings in air and vacuum environments. The coatings include AZ-93 paint, Thermal Bright, and Solar White, a coating developed by the Applied Physics Lab (APL) at NASA Kennedy Space Center (KSC). The resistance and the thickness of the various coatings impact how well it works as an insulative layer for the EDS. Preliminary results indicate that Solar White may have better properties for dust removal and thermal rejection than the other coatings.

Krystal L Acosta↗
NASA NTRSDate not supplied

Evaluation of Coatings for the Electrodynamic Dust Shield Application on Thermal Radiators

Space dust acts as a blackbody, becoming hot if left in direct sunlight. This is a problem for thermal radiators used in space missions, where the main function is to radiate heat away from an object. If dust lands on the thermal radiator, the unit will less effectively reject heat, and it will overheat, leading to electrical or system failure. The current state-of-the-art in active dust mitigation is the Electrodynamic Dust Shield (EDS) which uses an electric field generated by alternating high positive and negative voltages (low current) to eject the charged dust off surfaces. An EDS made from copper coated Kapton is an ideal candidate to be bonded to a thermal radiator and coated with a low solar absorptance, high heat-emitter coating. This work compares the dust removal of copper-Kapton EDSs covered with different thermal radiator coatings in air and vacuum environments. The coatings include AZ-93 paint, Thermal Bright, and Solar White, a coating developed by the Applied Physics Lab (APL) at NASA Kennedy Space Center (KSC). The resistance and the thickness of the various coatings impact how well it works as an insulative layer for the EDS. Preliminary results indicate that Solar White may have better properties for dust removal and thermal rejection than the other coatings.

Krystal L. Acosta↗
DOE OSTI2026

Triboelectric Nanogenerator Repeatability and Reproducibility Study

The development of triboelectric nanogenerators (TENGs) has largely focused on optimizing output performance, often at the expense of other critical research considerations such as the development of reliable technical procedures. In particular, the reliability of reported results—specifically repeatability and reproducibility—remains underexplored and is frequently limited to brief discussion within available literature. Without rigorous validation through repeatability and reproducibility studies, the credibility and broader applicability of reported findings remain uncertain. This study addresses this gap by systematically evaluating the repeatability and reproducibility of TENG performance data. Five polymer materials—Kapton, polyethylene (PE), polyethylene terephthalate (PET), polytetrafluoroethylene (PTFE), and polyvinylidene fluoride (PVDF)—were investigated across all pairwise combinations of 25 total combinations for the reproducibility study and three selected pairs of the 25 samples were selected for the repeatability study. For each TENG pairing, we analyzed the methodology, experimental procedures, and resulting performance data to quantify consistency and reliability. The objective of this work is to assess the validity of the collected dataset and determine whether the observed performance trends are consistent for use in future TENG design and optimization studies. Establishing reliable and reproducible data is essential for advancing the development of high-output TENG systems and ensuring their dependable implementation in practical applications.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Detection and Signal Processing for Near-Field Nanoscale Fourier Transform Infrared Spectroscopy

Researchers from a broad spectrum of scientific and engineering disciplines are increasingly using scattering-type near-field infrared spectroscopic techniques to characterize materials non-destructively with nanoscale spatial resolution. However, a sub-optimal understanding of a technique's implementation can complicate data interpretation and act as a barrier to entering the field. Here the key detection and processing steps involved in producing scattering-type near-field nanoscale Fourier transform infrared spectra (nano-FTIR) are outlined. The self-contained mathematical and experimental work derives and explains: i) how normalized complex-valued nano-FTIR spectra are generated, ii) why the real and imaginary components of spectra qualitatively relate to dispersion and absorption respectively, iii) a new and generally valid equation for spectra which can be used as a springboard for additional modeling of the scattering processes, and iv) an algebraic expression that can be used to extract an approximation to the sample's local extinction coefficient from nano-FTIR. The algebraic model for weak oscillators is validated with nano-FTIR and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra on samples of polystyrene and Kapton and further provides a pedagogical pathway to cementing some of the technique's key qualitative attributes.

36 MATERIALS SCIENCE↗
DOE OSTI2025

A new tubular ironless linear induction motor using non-interrupted winding method

The ironless linear induction motor device can be used for any application which requires a large motion span or rotation restrictedly by the ironless feature due to the strong magnetic field environment. One of the possible applications is ITER diagnostics shutters. The tokamak reactor systems have a severe radiation issue during the operation. The traditional Kapton-insulated wires have significantly lower radiation resistance than an expected large radiation dose at ITER Motion Stark Effect (MSE) shutter location. Furthermore, the traditional single-sided linear induction motor winds the wire to make the N-turn pitch coils independently and then connect them in series to make a one-phase winding. Therefore, it is a big challenge to make so many radiation-protection connectors in such a limited space as inside the vacuum vessel of fusion reactors. The approved mineral-insulated kinds of cables need a large bend radius for the end turns, so the traditional single-sided linear motor with two-layer three-phase windings need to be upgraded to the tubular linear motors. The new proposed tubular ironless linear induction motor can not only overcome the large bend radius issue with the mineral-insulated cables but also allow the motor coils wound continuously around the tubular-shaped stator, forward and backward N times to make a N-turn winding for each phase, in order to resolve the radiation protection issue with the winding connection. The 3D transient Maxwell electromagnetic model with a tubular three-phase linear induction motor has been analyzed. Furthermore, this paper will present the detailed design and winding method of ironless linear induction motor actuators, and results of the 3D transient numerical simulation of the actuator performance.

Ironless↗
DOE OSTI2025

The STAR Forward Silicon Tracker

The Forward Silicon Tracker (FST) is a pivotal component of the forward upgrade of the Solenoidal Tracker at RHIC (STAR), designed to discern hadron charge signs with a momentum resolution better than 30% for 0.2 < p T < 2GeV/c in the 2.5 < η < 4 pseudorapidity range. Its compact design features three disks along the beam direction, minimized material budget, and scattering effects. The FST uses Hamamatsu’s p-in-n silicon strip sensors with a double metal layer that enables efficient signal routing to the readout electronics, enhancing overall detector performance. The flexible hybrid boards, essential for the readout system, are constructed with Kapton and copper layers to optimize signal handling and power distribution. These boards connect silicon strips to analogue pipeline ASIC APV25-S1 chips, which read up to 128 channels each. A cooling system with nonconducting, volatile NOVEC 7200 coolant at 22.2 °C mitigates ASIC-generated heat. Furthermore, the FST enhances forward tracking performance at STAR as an integral part of the forward upgrade.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Ultra-Fast Vertical Ordering of Lamellar Block Copolymer Films on Unmodified Substrates

To utilize the full potential of block copolymer (BCP) thin films for use in technological devices ranging from ion conduction membranes, transistors to nanowire array antennas, rapid self- assembly of lamellar block copolymers (l-BCPs) with vertically oriented lamellar domains on a variety of unmodified substrates is needed. l-BCPs have an inherently larger interfacial area for transport compared to their cylindrical counterpart. Our observations demonstrate that the as-cast weakly ordered vertically oriented state of l-BCP films of polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) from directional evaporation of select solvents, act as “seed templates” for their ultra-fast evolution (~30 s) into well-ordered vertically oriented nanostructures, using a thermal gradient-based Cold Zone Annealing (CZA) technique. Furthermore, vertical lamellae are obtained on unmodified substrates, Quartz and Kapton, and the kinetics of l-BCP ordering is much faster by CZA as compared to the isotropic oven annealing. The rapid ordering kinetics of vertical l-BCPs is tested and found applicable to different molecular weights and film thicknesses ranging from 20 nm to 480 nm, which ultimately flip over to their equilibrium parallel morphology at upper limits of annealing times. This rapid ordering strategy for vertical orientation of l-BCPs using roll-to-roll compatible CZA would be highly relevant for fundamental studies of interfacial transport as well as for industrial applications from membranes to nanowires.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Flexible and Extensive Platinum Ion Gel Condensers for Programmable Catalysis

Catalytic condensers composed of ion gels separating a metal electrode from a platinum-on-carbon active layer were fabricated and characterized to achieve more powerful, high surface area dynamic heterogeneous catalyst surfaces. Ion gels comprised of poly(vinylidene difluoride)/1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide were spin coated as a 3.8 μm film on a Au surface, after which carbon sputtering of a 1.8 nm carbon film and electron-beam evaporation of 2 nm Pt clusters created an active surface exposed to reactant gases. Electronic characterization indicated that most charge condensed within the Pt nanoclusters upon application of a potential bias, with the condenser device achieving a capacitance of ∼20 μF/cm 2 at applied frequencies of up to 120 Hz. The maximum charge of ∼10 14 |e – | cm –2 was condensed under stable device conditions at 200 °C on catalytic films with ∼10 15 sites cm –2 . Grazing incidence infrared spectroscopy measured carbon monoxide adsorption isobars, indicating a change in the CO* binding energy of ∼19 kJ mol –1 over an applied potential bias of only 1.25 V. Condensers were also fabricated on flexible, large area Kapton substrates allowing stacked or tubular form factors that facilitate high volumetric active site densities, ultimately enabling a fast and powerful catalytic condenser that can be fabricated for programmable catalysis applications.

Catalysis↗
DOE OSTI2021

Probabilistic effects of porosity and chemical kinetics on the shock initiation of an octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) based explosive

In this work, we investigate the effects of porosity and chemical reactivity on the shock initiation of an HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine)-based polymer bonded explosive due to thin flyer impact using two-dimensional mesoscale simulations. Microstructural samples are computationally generated, and the calculated shock response is compared to experiments. The sample dimensions are 0.1×1.05 mm 2 , and each sample accounts for grain scale heterogeneities, including randomized grain morphology and pore spacing. Simulations are performed using the Lawrence Livermore National Laboratory (LLNL) arbitrary Lagrangian–Eulerian multi-physics code ALE3D. Chemistry and equation of states are handled with LLNL's thermochemical code Cheetah. We employ a modified Arrhenius-based chemical kinetics model that scales the temperature exponent fitting parameter with flyer shock conditions. This new model is calibrated to the mean response of experimental shock initiation thresholds for three separate Kapton flyer thicknesses. A simplified shock initiation criterion is proposed, which classifies the macroscale initiation response based on cross-sectional temperature profiles of the shocked sample. This criterion is used to further investigate the probabilistic response of the sample to variations in the mean porosity and chemical kinetics rate, and we find an inverse correlation between the shock pressure and the confidence interval of the experimental threshold velocity. Furthermore, the methodology presented in this work for quantifying the probabilistic nature of shock initiation is material agnostic. These mesoscale studies may be used to inform continuum scale models and expedite the development of future, tailored energetic formulations.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Magnetic functionalization and catalytic behavior of magnetic nanoparticles during laser photochemical graphitization of polyimide

We report laser-assisted photochemical graphitization of polyimides (PIs) into functional magnetic nanocomposites using laser irradiation of PI in the presence of magnetite nanoparticles (MNPs). PI Kapton sheets covered with MNP were photochemically treated under ambient conditions using a picosecond pulsed laser (1064 nm) to obtain an electrically conductive material. Scanning electron microscopy of the treated material revealed a layered magnetic nanoparticle/graphite (MNP/graphite) nanocomposite structure. Four probe conductivity measurements indicated that the nanocomposite has an electrical conductivity of 1550 ± 60 S/m. Superconducting quantum interference device magnetometer-based magnetic characterization of the treated material revealed an anisotropic ferromagnetic response in the MNP/graphite nanocomposite compared to the isotropic response of MNP. Raman spectroscopy of the MNP/graphite nanocomposite revealed a fourfold improvement in graphitization, suppression in disorder, and decreased nitrogenous impurities compared to the graphitic material obtained from laser treatment of just PI sheets. X-ray photoelectron spectroscopy, x-ray diffraction, and energy-dispersive x-ray spectroscopy were used to delineate the phase transformations of MNP during the formation of MNP/graphite nanocomposite. Post-mortem characterization indicates a possible photocatalytic effect of MNP during MNP/graphite nanocomposite formation. Under laser irradiation, MNP transformed from the initial Fe 3 O 4 phase to γ-Fe 2 O 3 and Fe 5 C 2 phases and acted as nucleation spots to catalyze the graphitization process of PI.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In situ counter-diffusion crystallization and long-term crystal preservation in microfluidic fixed targets for serial crystallography

Compared with batch and vapor diffusion methods, counter diffusion can generate larger and higher-quality protein crystals yielding improved diffraction data and higher-resolution structures. Typically, counter-diffusion experiments are conducted in elongated chambers, such as glass capillaries, and the crystals are either directly measured in the capillary or extracted and mounted at the X-ray beamline. Despite the advantages of counter-diffusion protein crystallization, there are few fixed-target devices that utilize counter diffusion for crystallization. In this article, different designs of user-friendly counter-diffusion chambers are presented which can be used to grow large protein crystals in a 2D polymer microfluidic fixed-target chip. Methods for rapid chip fabrication using commercially available thin-film materials such as Mylar, propylene and Kapton are also detailed. Rules of thumb are provided to tune the nucleation and crystal growth to meet users' needs while minimizing sample consumption. These designs provide a reliable approach to forming large crystals and maintaining their hydration for weeks and even months. This allows ample time to grow, select and preserve the best crystal batches before X-ray beam time. Importantly, the fixed-target microfluidic chip has a low background scatter and can be directly used at beamlines without any crystal handling, enabling crystal quality to be preserved. The approach is demonstrated with serial diffraction of photoactive yellow protein, yielding 1.32 Å resolution at room temperature. Fabrication of this standard microfluidic chip with commercially available thin films greatly simplifies fabrication and provides enhanced stability under vacuum. These advances will further broaden microfluidic fixed-target utilization by crystallographers.

Liu, Zhongrui↗