Search NASA⌕ Search

SEARCH · Search NASA

Results for “Coating processes”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 361 records · Page 20

Advancements in Manufacturing of High-Performance Perovskite Solar Cells and Modules Using Printing Technologies

Perovskite photovoltaic technology carries immense opportunity for the solar industries because of its remarkable efficiency and prospect for cost-effective production. However, the successful deployment of perovskite solar modules (PSMs) in the solar market necessitates tackling stability-based obstacles, scalability, and environmental considerations. This paper unveils a comprehensive examination of the cutting-edge advancements in the manufacturing of perovskite solar cells (PSCs) and modules, with an emphasis on high-speed, large-area printing. The paper underscores the substantial progress achieved in printed PSCs and PSMs, demonstrating promising electrical performance and long-term device durability. This review paper categorizes printing techniques compatible with large-area high-speed manufacturing into three distinct families: blade coating, slot die coating, and screen printing, as these common printing practices offer precise control, scalability, cost-effectiveness, high resolution, and efficient material usage. Additionally, this paper presents an in-depth investigation and comparison of superior PSCs and PSMs fabricated by printing on power conversion efficiency (PCE), stability, and scalability.

14 SOLAR ENERGY↗

Silicon carbide reinforced zirconium based cladding

A method for making an improved nuclear fuel cladding tube includes reinforcing a Zr alloy tube by first winding or braiding ceramic yarn directly around the tube to form a ceramic covering, then physically bonding the ceramic covering to the tube by applying a first coating selected from the group consisting of Nb, Nb alloy, Nb oxide, Cr, Cr oxide, Cr alloy, or combinations thereof, by one of a thermal deposition process or a physical deposition process to provide structural support member for the Zr tube, and optionally applying a second coating and optionally applying a third coating by one of a thermal deposition process or a physical deposition process. If the tube softens at 800° C.-1000° C., the structural support tube will reinforce the Zr alloy tube against ballooning and bursting, thereby preventing the release of fission products to the reactor coolant.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Ultra-High Temperature Thermal Barrier Coating Development and Validation

The most effective method to improve industrial gas turbine power is to increase firing temperature. To maintain component durability at these higher temperatures, thermal barrier coatings (TBC’s) are playing an increasing role in protecting turbine hardware. TBC’s have been successfully used on Solar Turbines’ combustor liners and turbine airfoils, but there is a need for TBC’s that can operate at higher temperatures. Based on recent, favorable rig testing experience, Solar recognized that yttrium aluminum garnet (YAG) TBC’s made by the Solution Precursor Plasma Spray Process (SPPS) has great potential for higher turbine temperatures. This testing verified the thermal cycle durability of the SPPS YAG TBC’s, as well as demonstrated that the temperature drop through the SPPS YAG TBC was twice that measured across a companion APS YSZ TBC. The SPPS YAG TBC with the potential for a 200°C improvement in temperature capability represents a materials breakthrough. The SPPS process also produces a number of unique microstructural features that confer superior properties. SPPC TBC’s have ultra-fine splats that increase toughness and erosion resistance, and the process can be tailored to produce through-thickness cracks for strain-tolerance and control porosity for lower thermal conductivity and increase coating abradability. This proposal would include further development of SPPS YAG density-graded coatings, optimization of the application process, and validation of higher temperature capability and durability through rig and engine testing of coated combustion liners and turbine outer air seals. The technology would be advanced from a TRL 3 to a proposed TRL 6 by overcoming processing concerns on efficiency, application distance and optimization of a graded coating without impacting coating durability by demonstrating the coating performance on components in rig and development gas turbine engine testing.

36 MATERIALS SCIENCE↗

Direct Recycling of Lithium-Ion Battery Cathodes: A Multi-Stage Annealing Process to Recover the Pristine Structure and Performance

Direct recycling is an alternative low-cost process that retains the structure of the lithium-ion battery cathode rather than going through materials dissolution and repurification. While the process shows promise, various steps need to be better understood and studied to identify possible roadblocks, cost intensive steps, and needed variations in protocol that may be necessary based on the feedstock of recycled cathodes available. In this study, we have evaluated the process of thermal relithiation as it applies to end-of-life cathode materials. For recovered end-of-life cathodes, approximately 20% of the useable lithium has been lost due to solid electrolyte interface formation, parasitic reactions, and particle isolation; this lost lithium contributes to higher cell impedance and a gradual shift in electrode potentials. As a first step in the direct recycling process, this lithium needs to be restored not only to recover capacity but also to eliminate surface vacancies and hinder surface reconstruction that may increase impedance and impact performance. Here, we have optimized a coating method followed by a two-stage annealing process that restores a model delithiated NMC333 material to pristine performance. Comparisons to single-stage processes are made, and new characterization tools have been used to better understand the processes.

25 ENERGY STORAGE↗

Improving knife milling performance for biomass preprocessing by using advanced blade materials

Mechanical preprocessing of biomass, including size reduction, is a crucial step in converting biomass into biofuel. However, feedstock inevitably contains abrasive intrinsic and extrinsic inorganics that may cause excessive tool wear in preprocessing. Here, this work demonstrates that performance of a knife mill can be significantly improved by applying a more wear-resistant blade material. A series of full-scale knife mill tests were performed for size reduction of forest residue using blades of tungsten carbide (WC–Co), iron-borided tool steel, and diamond-like carbon (DLC) coated tool steel. Blade material loss was quantified in correlation to the amount of feedstock processed and wear mechanisms were investigated via worn surface characterization. While the thin DLC coating was removed quickly, the WC-Co and iron-borided blades improved the tool life by 8X and 3X compared with the M2 tool steel blades (baseline), respectively. The in-situ throughput and power consumption measurements provided additional insights. The WC-Co and iron-borided blades had ~3X higher throughput than the baseline blades by the end of the test with lower normalized power consumption. The experimental results were then used as input for a techno-economic analysis, which suggested that the more wear resistant blades could cut the knife milling cost by $2–3 per ton of biomass processed with downtime reduced by 65–85%.

36 MATERIALS SCIENCE↗

Chromium Tolerant, Highly Active and Stable Electrocatalytic Internal Surface Coating for Cathode of Commercial SOFCs (Final Report)

This project is aimed to develop a chromium (Cr) tolerant, highly active, and stable coating layer on the internal surfaces of the porous composite cathode from commercially available SOFCs. Such coating layer was developed using the additive manufacturing process of Atomic Layer Deposition (ALD) and has been applied on the cathode consisting of either an electronic conductor of LaxSr 1-x MnyO 3-δ (LSM) or mixed ionic and electronic conducting La x Sr 1-x Co y Fe 1-y O 3-δ (LSCF). PI's work has demonstrated that the internal surface of cathode from the commercial cells, can be further tailored using ALD coating to dramatically enhance the cell performance. For instance, ALD layer consisting heterostructured nano composite of nano-Pt and nano-(Mn 0.8 Co 0.2 ) 3 O 4 oxide on the internal surface of porous LSM/YSZ cathode from SOFCs, has resulted in the large reduction of the cell polarizations resistance by up to 53%, and enormous increase of power density over 370%. For the cells with LSCF/Sm 2 O 3 doped CeO 2 (SDC) cathode, the conformal layer of nano-composite consisting of superjacent CoOx and subjacent minimum amount of Pt nano-grains has resulted in the power density enhancement by 126% for the large scale industry tubular cells at 750°C, and both the performance enhancement and nanostructure of the ALD layer are stable over ~ 2000 h continuous operation performed at industry test station. In the meanwhile, those ALD coating layer developed by PI's work is also inherently Cr-tolerant, and could act as physical barrier for preventing Cr diffusion into the cathode backbone, so as to mitigate the Cr poisoning effect on the cathode. In this project, the impact of Cr on the performance of those ALD coated commercial cells has been evaluated. Based on evolution of the cell performance, the ALD coating layer chemistry and ALD coating layer thickness has been optimized to maximize the overall Cr tolerance, cell power density and cell longevity. Different ALD coating has been applied onto the internal surface of LSM/YSZ and LSCF/SDC backbone respectively. The architecture/scaffold structures on the internal surface of different cathode, designed by this project, was catalogued and analyzed using High Resolution Transmission Electron Microscopy (HRTEM), and cell power/durability performance are assured via comprehensive electrochemical performance testing in the industry operation relevant conditions. The impact of the electrochemical operation current density, the water humidity, the cell operation temperature, and cell operation duration on the Cr tolerance of ALD coated cells has been systematically investigated. There is completely different nanostructure degradation mechanisms between LSM and LSCF cells induced by Cr contamination. For the LSCF/SDC baseline cell, With the Cr source, there is no apparent Sr surface segregation phase even for the baseline cell operated for 3000 h at 750 °C. With the Cr source, there is significant amorphous (SrCr)Ox phase accumulated in the original pore region. For the commercial baseline cells, Cr contaminants on the LSM electrode severely impacted the entire cell's electrochemical performance and nanostructure degradation. Those degradations include (1). Peak power density loss of 64 % after 109 h of operation. The dramatic increase in Rp (2). They are cracking at LSM/SSZ interface, LSM grains. SSZ remains intact but with (CrMn)Ox. By contrast, ALD coating (MnCo)Ox/Pt dramatically improves the Cr resistance, as follows (1). ALD-coated cell with a power density is 280-380 % of the baseline cell, depending on the ALD layer thickness. (2). For a cell with a 20 nm thick ALD layer, there is a large performance enhancement (> 200 % power density) induced by ALD coating of Cr-tolerant Mn 0.8 Co 0.2 Ox. (3). For a cell with a 20 nm thick ALD layer, after 168 h at 750 °C power density of the ALD-coated cell is ~ 600% of that baseline cell upon operation with Cr contamination for 109 h. The ALD coating on the internal surface of cathode developed by this project integrated multi-functions. Those multi-functions include (1). Dramatically improving the cell power density for the commercial cells; (2). Dramatically improving contamination resistance of the cathode, for being an excellent protection coating layer sealing off Cr contamination. (3). Dramatically increasing the cell longevity by potentially preventing the microstructure evolution and grain coarsening of the cathode. Overall, this project will provide a simple solution to simultaneously enhance power density and increase the reliability, robustness, and endurance of commercial SOFCs, over the entire operating temperature range of 650-800 °C. For the inherently functional SOFC, the ALD coating of LSM based cathode mitigate the Cr-contamination. Power density of ALD-coated cell is ~ 600% of that baseline cell upon operation with Cr contamination. In addition to SOFCs, the novel on-demand design approach and creation of multifunctional heterogeneous architecture on the electrode surface presented in this work opens further research for their application in other types of fuel cells, batteries, and sensors for which electrochemical reactions on the surface are similarly critical.

36 MATERIALS SCIENCE↗

Spray coating for washout tooling by binder jet additive manufacturing

We report washout tooling is a process in which a removable mold or fixture is disintegrated using a solvent. Binder Jet (BJ) additive manufacturing holds promise for creating customized washout molds from common materials. BJ-based washout tooling provides an advanced strategy in manufacturing fiber-reinforced composites (FRCs), especially for customized hollow FRCs. However, washout tools formed by BJ require an impermeable barrier between the porous tooling surface and the parts laid up on the surface to prevent the resin from infiltrating the tooling surface and bonding the tool to the FRC. The conventional method for preventing resin migration into the washout mold from the FRC is winding Teflon® tape over the entire surface, which is labor-intensive and very difficult to deploy for specific geometries. Here, we report the development of a polymer spray coating method to seal the tooling surface and prevent resin infiltration without affecting the washout properties needed for sacrificial tooling. Two water-soluble polymers, poly(sodium 4-styrenesulfonate) (PSS–Na) and poly(vinylsulfonic acid, sodium salt) (PVS–Na), were investigated for spray coating. PVS-Na maintained tighter geometric tolerances and provided excellent thermal stability with the onset of decomposition at 320 °C and glass transition temperature of 280 °C. Spray coating with PVS-Na streamlines the process of forming a protective layer for the washout molds by BJ, reduces migration of the resins from the FRC, and significantly improves the production efficiency of complex washout tools.

42 ENGINEERING↗

Development and Understanding of Nb 3 Sn films for radiofrequency applications through a sample-host 9-cell cavity

Nb 3 Sn is a promising advanced material under development for superconducting radiofrequency cavities. Past efforts have been focused primarily on small development-scale cavities, but large, often multi-celled cavities, are needed for particle accelerator applications. In this work, we report on successful Nb 3 Sn coatings on Nb in a 1 m-long 9-cell Nb sample-host cavity at Fermilab. The geometry of the first coating with only one Sn source made it possible to study the influence of Sn flux on the microstructure. Based on these results, we postulate a connection between recently observed anomalously large thin grains and uncovered niobium spots observed in the past by other authors (Trenikhina et al 2018 Supercond. Sci. Technol. 32 015004). A phenomenological model to explain how these anomalously large grains could form is proposed. Overall, this model is invoked to provide possible explanations for literature results from several groups and to guide key process parameters to achieve uniform vapor-diffusion coatings, when applied to complex structures as the multi-cell cavity under study.

43 PARTICLE ACCELERATORS↗

Biomass burning and marine aerosol processing over the southeast Atlantic Ocean: a TEM single-particle analysis

This study characterizes single-particle aerosol composition from filters collected during the ObseRvations of Aerosols above CLouds and their intEractionS (ORACLES) and CLoud–Aerosol–Radiation Interaction and Forcing: Year 2017 (CLARIFY-2017) campaigns. In particular the study describes aged biomass burning aerosol (BBA), its interaction with the marine boundary layer and the influence of biomass burning (BB) air on marine aerosol. The study finds evidence of BBA influenced by marine boundary layer processing as well as sea salt influenced by BB air. Secondary chloride aerosols were observed in clean marine air as well as in BB-influenced air in the free troposphere. Higher-volatility organic aerosol appears to be associated with increased age of biomass burning plumes, and photolysis or oxidation may be a mechanism for the apparent increased volatility. Aqueous processing and interaction with the marine boundary layer air may be a mechanism for the presence of sodium on many aged potassium salts. By number, biomass burning potassium salts and modified sea salts are the most observed particles on filter samples. The most commonly observed BC coatings are inorganic salts. These results suggest that atmospheric processes such as photolysis, oxidation and cloud processing are key drivers in the elemental composition and morphology of aged BBA. Fresh BBA inorganic salt content, as it has an important role in the particles' ability to uptake water, may be a key driver in how aqueous processing and atmospheric aging proceed.

54 ENVIRONMENTAL SCIENCES↗

Perspectives on the relationship between materials chemistry and roll-to-roll electrode manufacturing for high-energy lithium-ion batteries

As lithium-ion battery (LIB) active material and cell manufacturing costs continue to drop with wider adoption of electric vehicles, electrode and cell processing costs remain too high in terms of reaching the ultimate U.S. Department of Energy (DOE) cell cost target of $80/kWh. This paper primarily covers major materials chemistry advancements made over the last 10 years at Oak Ridge National Laboratory (ORNL) in the space of advanced manufacturing science for LIBs with the aim of simultaneously meeting the ultimate cost target, 500 Wh/kg gravimetric energy density, 10-15-min fast charge times, and 1000 deep discharge cycles. Aqeous electrode processing with a variety of active anode and cathode materials is now a standard procedure at the DOE Battery Manufacturing R&D Facility at ORNL (BMF), including the latest processes developed for Ni-rich cathodes. New results on cobalt-free LiNi 0.8 Fe 0.1 Al 0.1 O 2 (NFA 811) are also included and discussed in an electrode processing advantage context. In addition, colloidal processing advancements have been made for Si/C composite anodes for achieving >600 mA h/g capacities. Optimization of electrode coating parameters and drying protocols have been completed, which has elucidated how key processing variables need to be changed when parameters such as slurry solids loading, solvent type, and wet electrode thickness are changed. ORNL has also increased the line speeds at which thick cathodes can be processed using ultra-fast electron beam (EB) curing and substantially decreased formation cycling times to <1 day. Finally, key details of these advancements are discussed in the context of materials chemistry and process-property-performance relationships.

25 ENERGY STORAGE↗

Conditioning the Surface and Bulk of High-Nickel Cathodes with a Nb Coating: An In Situ X-ray Study

Surface coating is commonly employed by industries to improve the cycling and thermal stability of high-nickel (Ni) transition metal (TM) layered cathodes for their practical use in lithium-ion batteries. Niobium (Nb) coating or substitution has been shown to be effective in stabilizing LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) cathodes; in addition, the electrochemical performance of the final products varies depending on the postprocessing. In this follow-up study, we use in situ synchrotron X-ray diffraction to investigate the kinetic processes and the involved structural evolution in Nb-coated NMC811 upon heat treatment. Furthermore, quantitative structure analysis reveals thermally driven concurrent changes in the bulk and surface, in particular, the phase evolution of the coating layer and Nb/TM interdiffusion that facilitates penetration of Nb into the bulk and particle growth at the increased temperatures. Findings from this study highlight the new opportunities for the intended control of the structure and surface properties of high-Ni cathodes through surface coating in conjunction with postprocessing.

36 MATERIALS SCIENCE↗

Cladding and Butt-Joining Dissimilar Aluminum Alloys Simultaneously via Shear Assisted Processing and Extrusion

Shear assisted processing and extrusion has been used to fabricate multi-metallic tubing that incorporates regions with clad and butt-joined structures. In this work, aluminum alloys 6061, 7075, and 1100 are combined to create a monolithic extruded tubing with weldable ends (6061), a high strength center (7075), and a corrosion-resistant cladding (1100). Optical microscopy shows a gradual, defect-free, transition between alloys at the butt-joint interfaces and a sharp transition between alloys at the clad interface. Tensile testing proved the mechanical coherency of the joint, with failure occurring outside the tri-metallic structure. In conclusion, smoothed particle hydrodynamic simulations identified a spiral pattern of the cladding alloy that leads to inconsistent cladding thickness, and identified a simplified 2-alloy combination of aluminum alloys 6082 and 2014 that accomplished the design objectives of the tri-metallic structure.

Coatings↗

Electrochemical Synthesis of Zeolite Coatings with Controlled Crystal Polymorphism and Self-Regulating Growth

Zeolite coatings are studied as molecular sieves for membrane separation, membrane reactors, and chemical sensor applications. They are also studied as anticorrosive films for metals and alloys, antimicrobial and hydrophobic films for heating, ventilation, and air conditioning, and dielectrics for semiconductor applications. Zeolite coatings are synthesized by hydrothermal, ionothermal, and dry-gel conversion approaches, which require high process temperatures and lengthy times (ranging from hours to days). Here, we report the first zeolite coatings synthesized via electrochemical deposition on a cathodic electrode, with controlled crystal polymorphism achieved within subhourly duration. We demonstrate this approach by developing sodium zeolite (e.g., sodalite (SOD), NaA (LTA), and Linde Type N (LTN)) coatings on a titanium electrode and extending the synthesis method to porous stainless steel. The coating morphology and crystallinity depend on the temperature, time, and applied current. The coating thickness is independent of the applied current, showing the presence of a self-regulating mechanism to ensure a uniform coating thickness across the metal surface. The electrochemical zeolite growth mechanism was elucidated with high-resolution transmission electron microscopy, and applications of the resultant zeolite coatings for oil/water separation and ethanol/water pervaporation were exploited. Electrochemical synthesis represents a novel, simple, fast, and environmentally friendly approach to preparing zeolite coatings. It can potentially be generalized for developing zeolite materials with diverse framework structures, morphologies, and orientations for substrates with complicated geometries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterizing the combined impact of nucleation-driven precipitation and secondary passivation on carbon mineralization

The evolution of mineral reactive surface area is one of the primary phenomena controlling the progression and extent of mineral carbonation. The CO 2 mineralization begins with nucleation of crystals that provide initial surface area for subsequent growth of the mineral. However, many reactive transport models (RTMs) for CO 2 mineralization do not include the nucleation process. The few RTMs that do include it are yet to be validated against experimental data. Similarly, many RTMs ignore passivating effects of the secondary mineral, which coats the surface of the dissolving mineral, slow down the reaction process, and reduce the total extent of carbonation. Furthermore, the combined impact of nucleation and passivation on carbon mineralization is yet to be properly characterized. In this study, we consider the coupled effects of passivation and nucleation on the mineralization extent. The nucleation-driven precipitation model relies on the formation of nuclei to provide a surface area for crystal growth, while a new model is proposed to account for passivation effects. Our analysis shows that (i) omission of nucleation leads to overestimation of extent of mineralization, and (ii) omission of passivation leads to overestimation of host rock reactivity. The model was evaluated via comparison with CO 2 mineralization data from the literature and models that ignore these processes. We observed that including nucleation and passivation lead to closer predictions of the CO 2 mineralization extent. Therefore, this study highlights the importance of including the coupled nucleation-driven precipitation and secondary passivation in RTMs. Here, the findings from the study can be applied in various scientific and engineering applications such as petroleum production, cement carbonation, CO 2 sequestration, chemical weathering, and concrete degradation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Time-Dependent 600 °C Post-Weld Heat Treatment Response of Laser-Wire-Directed Energy Deposited Austenitic Stainless Steel Claddings on Carbon Steel

Austenitic stainless steel overlay claddings are often used to protect nuclear reactor pressure vessels from corrosion. Arc welding processes are traditionally employed, which require a high heat input to bond the dissimilar metals, creating a large heat-affected zone and high residual stress that demands a lengthy stress-relieving post-weld heat treatment, up to 48 hours. High energy beam (e.g., laser, electron beam) directed energy deposition-based overlay cladding processes show promise for fabricating claddings with superior performance compared to arc welded ones because of their localized heat input; however, their necessity and time of post-weld heat treatment are currently unclear. In this research, we investigate the time dependence of a 600 C stress-relieving post-weld heat treatment of austenitic stainless steel clad on low carbon steel by laser-wire-directed energy deposition, comparing the microstructure and mechanical properties of the as-fabricated condition to 2-, 10-, and 48-hour heat treatment times. Diffusion simulations and microscopy show a gradual carburization of the stainless steel cladding and decarburization of the heat-affected zone/base metal. Nanoindentation testing shows up to a 1.8–2.69 embrittlement in the cladding and a 0.33 to 0.69 softening in the heat-affected zone after the 48-hour post-weld heat treatment. Tensile testing of the cladding composites reveals that increasing post-weld heat treatment time raises clad cracking susceptibility due to intergranular carbide formation and shows that laser-wire-directed energy deposition claddings may not require post-weld heat treatment.

Coating↗

High Temperature Oxidation Behavior of Aluminized Haynes 230

The effect of reactive air aluminizing (RAA) on the high-temperature oxidation behavior of the H230 superalloy is studied at 850 °C for 600 hours. Mass gain values are measured and microstructure is studied by XRD, SEM, and EDX. Post oxidation mass gain for the aluminized alloy is reduced compared to wrought alloy. A three-zone microstructure of diffusion coating is observed in RAA H230. Formation and growth of alumina scale during RAA process and oxidation is attributed to the complementary roles of ß-NiAl + ?'-Ni3Al phases in the composite coating.

Rashidi, S↗

Electrodialysis through nafion membranes coated with polyelectrolyte multilayers yields >99% pure monovalent ions at high recoveries

Separation of monovalent and multivalent ions is important in processes ranging from water softening to recycling of Li. Previous studies show that cation-exchange membranes coated with multilayer polyelectrolyte films exhibit monovalent/divalent ion selectivities as high as 1000 in electrodialysis (ED) under ideal conditions with low ion recoveries. This work shows that even at 60-80% monovalent-ion recoveries, ED through Nafion membranes coated with protonated poly(allylamine)/poly(4-styrenesulfonate) multilayers can separate equimolar K + and Mg 2+ or Li + and Mg 2+ to give 99.5% pure monovalent ion. Moreover, the use of a low-volume receiving phase allows ED to concentrate the monovalent ion. Typical current efficiencies are around 70% for these separations. Selectivities appear to increase when the membrane-coating procedure uses a higher polyelectrolyte concentration in the deposition solution. Because the limiting current declines with ED time due to depletion of the monovalent ion in the source phase, use of a gradually decreasing applied current enhances current efficiency compared to ED at a constant high current. Further, the membranes also show Li + /Mg 2+ selectivities around 100 when Mg 2+ is in a 20-fold excess in the source phase at an ionic strength of 0.6 M, but selectivity decreases at even higher ionic strengths.

15 GEOTHERMAL ENERGY↗

Freestanding high-aspect-ratio gold masks for low-energy, phase-based x-ray microscopy

High-resolution, x-ray phase contrast microscopy, a key technique with promising potential in biomedical imaging and diagnostics, is based on narrow-slit high-aspect-ratio gold gratings. Here we present the development, fabrication details, and experimental testing of the freestanding 10 μm thick gold membrane masks with an array of 0.9–1.5 μm void slit apertures for a novel low-energy x-ray microscope. The overall mask size is 4 mm × 4 mm, with a grating pitch of 7.5 μm, 6.0–6.6 μm wide gold bars are supported by 3 μm wide crosslinks at 400 μm intervals. The fabrication process is based on gold electroplating into a silicon mold coated with various thin films to form a voltage barrier, plating base, and sacrificial layer, followed by the mold removal to obtain the freestanding gold membrane with void slit apertures. We discuss key aspects for the materials and processes, including gold structures homogeneity, residual stresses, and prevention of collapsing of the grid elements. We further demonstrate the possibility to obtain high-resolution, high contrast 2D images of biological samples using an incoherent, rotating anode x-ray tube.

77 NANOSCIENCE AND NANOTECHNOLOGY↗