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DOE OSTI2022

Roll to Roll (R2R) Manufacturing of Electrolysis Electrodes for Low Cost Hydrogen Production: Cooperative Research and Development Final Report, CRADA Number CRD-18-00780

NREL, Argonne National Laboratory (ANL) and Oak Ridge National Laboratory (ORNL), which are also referred to collectively herein as the "Contractors" will perform electrode ink development and characterization, focusing on 1) inks with appropriate properties for R2R (gravure and slot-die) coating onto PFSA membrane and 2) catalysts suitable for electrolysis. Participant will develop acceptance criteria and characterization methods for direct coating on the membrane. The purpose of this project is to show feasibility for cost reduction of the electrode through increased throughput and improved material utilization. Successful completion of this project will result in more affordable hydrogen production via proton exchange membrane (PEM) electrolysis by substantially reducing the anode precious metal content and catalyst-coated membrane processing costs. Assists laboratory in achieving programmatic scope, adds new capability to the laboratory's core competencies. This project uses and enhances the laboratory's core competencies, and enhances U.S. competitiveness by utilizing DOE developed intellectual property and/or capabilities. This project will benefit the Fuel Cell subprogram within the EERE Fuel Cell Technologies Office (FCTO) by actively developing materials, formulations, components, and processes for PEM electrolyzer stacks for overcoming critical technical barriers to widespread hydrogen production for zero-emission transportation applications. Through this JWS, NREL, ANL and ORNL are assisting a key domestic industry partner, Proton Energy Systems, Inc., in the area of low-cost electrolyzer electrode formulation and coating technology. After completion of this project, NREL, ANL and ORNL will be able to verify whether the direct deposit coating processes investigated are suitable for producing CCMs for PEM electrolyzers, which is of great interest and benefit to the DOE EERE Fuel Cell Technologies Office (FCTO) and H2@Scale missions.

08 HYDROGEN↗

DOE OSTI2021

In-situ Photophysical Monitors and Corrective Algorithms for Photovoltaic Film Deposition and Rapid Thermal Processing in Scalable Roll-to-Roll Manufacturing

This project evaluated three photophysics-based approaches for in situ process monitoring of the scalable deposition of perovskite photovoltaic films. Based on stakeholder input and the results of laboratory trials and literature analysis, two techniques, angle resolved elastic light scattering (ARLS) and time-resolved photoluminescence (TRPL) were prototyped and demonstrated with a mixture of simulation, offline and online tests. Also, a hybrid gas flow and humidity control enclosure was constructed and demonstrated to stabilize the ambient conditions around the slot die deposition process and were demonstrated to meet the target humidity control in situ. Due in part to a delayed start and COVID-related lab restrictions and personnel changes, some of the milestones were not met. In spite of these challenges, however, both techniques were prototyped through several iterations and demonstrated significant promise for rapid in line perovskite characterization within the targeted characterization time windows and these techniques are under further development for use in DE-FOA000235:2357-1586. The TRPL system was fully mounted and demonstrated on the scaled slot die roll to roll and sheet coating systems at the Washington Clean Energy Testbeds (WCET). Motivated by significant internal and stakeholder interest, the successful prototyping achieved here, the ongoing need for in-situ characterization for the scale-up of perovskite manufacturing, and the benefits of in situ photophysical characterization for future funded process development research, we are continuing with the principle aims of the project to develop effect in situ photophysical probes for fast analysis of the optoelectronic and structural quality of sheet based and roll to roll process perovskites. TRPLS and ARLS probes proposed in the project are to be completed with external support from the Washington Research Foundation at the WCET. We are currently actively engaged in the acquisition of components and plan to complete and test the probes within three months. It is our intention that these probes will then be used in ongoing perovskite development with our research and commercialization partners including First Solar and other member of the US MAP consortium in future funded development work.

14 SOLAR ENERGY↗

DOE OSTI2022

All Solid State Batteries Enabled by Multifunctional Electrolyte Materials

Solid Power has teamed with University of California San Diego to develop a high energy, long life, low cost, and safe all-solid-state-battery (ASSB). The battery is enabled by a multifunctional solid state electrolyte (SSE). The project enables scalable production of large format solid state batteries required by the vehicle market and building domestic battery manufacturers as leaders in the global vehicle ASSB production. In the project, the multifunctional SSE materials have been developed and optimized with ionic conductivity ≥ 5 mS/cm and electrochemical stability 0 – 4.5V. SSE separator films have been coated by using a roll-to-roll process with thickness ≤ 40 µm. All-solid-state NMC-Li pouch cells containing the developed SSE have been assembled. A cycle life of > 750 at 100% DOD and 45 °C has been demonstrated in a full pouch cell.

25 ENERGY STORAGE↗

DOE OSTI2022

Scalable Deposition of NiOxas a Hole Transport Layer for Perovskite Solar Cells on PET Substrates

Transition from laboratory scale fabrication to large scale perovskite fabrication processes remains a challenge. Upscaling perovskite fabrication requires the development of deposition methods that yield uniform charge transport layers at scale. By optimizing ink composition, we have developed a doped nickel oxide hole transport material for uniform large area deposition on a roll-to-roll system with a peak power conversion efficiency of 11.2%.

Armstrong, Peter↗

DOE OSTI2023

Bio-Based Phase Change Materials (PCMs) for Thermal Energy Storage (Final Scientific/Technical Report)

The goal of this project is to develop a novel bio-based phase change material (PCM) derived from squid ring teeth (SRT) proteins, and design a prototype heat exchanger based on these bio-based PCMs for energy storage and dynamic heat exchange for building thermal energy storage systems. The PCMs, derived from SRT proteins, will demonstrate room temperature energy storage capacities and switchable thermal conductivities that redefine the current state-of-the-art (SOA) for building thermal energy storage. Further, in a single material and with a single manufacturing processes, our proposed thermal battery will be developed with “on demand” thermal conductivity for rapid charging/discharging but superior insulation during energy storage periods. More specifically, our bio-based PCMs have demonstrated: 1) the potential for increased energy storage capacity (i.e., greater than paraffines at room temperature); 2) tunability in thermal conductivity with the largest thermal conductivity switching ratios for an intrinsic material reported to date, and 3) a 100% recyclable and biodegradable PCM with low volatility and toxicity and scalability in its manufacture for both residential and commercial applications. The already established ability for roll-to-roll processing of these non-toxic, non-flammable SRT composites along with their carbon-neutral manufacturing processes that has been pioneered by our team make this solution a disruptive and impactful technology to redefine the current SOA of energy storage technologies. The outcomes of this effort have been: 1) the identification of new bio-based PCM that establishes a new SOA for thermal conductivity and energy storage density at room temperature and 2) the development of a new experimental technique to measure the energy storage density via latent heat measurements during melting of thin films. This new technique can be applied to thin films (as thin as < 1 micrometer), and represents a novel approach for thin film energy storage density measurements. Dynamic thermal energy storage is the missing technology that will enable a grid- interactive efficient building (GEB). For a “smart” building capable of connecting with the power grid, the media must be inexpensive and possess thermal switching capabilities to control the time-dependent heat flow into (and out of) the PCM on demand. Unique to the material system in this program, programmable SRT-based PCM show improvements as compared to traditionally used PCMs, and thus its technical performance will represent a leap forward for the future GEB concept.

25 ENERGY STORAGE↗

DOE OSTI2023

Scalable and Cost-Effective Roll-To-Roll Additive Manufacturing of Highly Durable and Thermal Insulating Silica-Carbon Aerogel (Final Report)

The research objective of this project is to demonstrate low cost silica aerogel insulation materials with high R-value and low installed price of R7.5/inch, and $0.94/ft2-inch, respectively, which can meet the cost and performance targets of the Department of Energy’s 2030 Building Technology Office Emerging Technologies program. The main tasks of this project include the following three topics: a) Low-cost silica gel precursor: Repeat silica sol gel chemical approach which is reproducible and scalable. Also explore suitability of water-glass on silica aerogel system to further control cost efficiency. In addition, our aim is to synthesize hollow silica using low-cost precursors. Sodium silicate (water glass) was chosen as our silica source because of its availability and low price compared to the other precursors; b) In situ ambient pressure-drying (APD) and surface modification: confirm and improve silica aerogel under cost-effective continuous ambient pressure-drying and investigate silica aerogel performance under time and temperature dependence; c) Roll-to-Roll (R2R) manufacturing with the targeted structure, thermal and mechanical characteristics: evaluate 3D printing with silica aerogel precursor to modify aerogel formation.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Diffractive Multiplexing for High-Throughput Roll-to-Roll Laser Patterning of Flexible Organic Photovoltaic Modules (Final Report)

The purpose of this project is to demonstrate a cost-effective, high-throughput roll-to-roll (R2R) process for patterning of flexible, semitransparent organic photovoltaic (OPV) modules by developing diffractive optics-based laser multiplexing (DOL Multiplexing). DOL Multiplexing allows a single, high-powered laser source to perform parallel scribing across the R2R web width in a manner compatible with high process speeds. Such a process could have enormous benefits in terms of increased process speeds and reduced costs, both up-front capital costs, and long-term operational costs, over galvanometer-based step and scan methods or many-laser systems.

14 SOLAR ENERGY↗

DOE OSTI2023

From Deposition to Encapsulation: Roll-to-roll manufacturing of organic light emitting devices for lighting (Final Report)

Organic light emitting devices (OLEDs) are promising solid state light sources due to their high efficiency, high color quality and flexible form factors. The key to enable low cost OLED lighting, is to rapidly fabricate thin film organic layers on a continuous flexible roll, called R2R processing. This project aims to investigate the feasibility of mass production of OLED lighting using the R2R process, from deposition to encapsulation. A high efficiency white OLED is fabricated on 10 cm-wide substrate rolls in a pilot R2R tool comprising of two different organic deposition: vacuum thermal evaporation (VTE) and organic vapor phase deposition (OVPD). A high quality encapsulation process to package OLEDs is demonstrated using an atomic layer deposition tool integrated to the R2R system without air exposure. The method to achieve ultrahigh deposition rates required by R2R processing is demonstrated by OVPD. Uniform organic semiconductor thin films grown by OVPD at rates as high as 50 Å/s are achieved. A comprehensive numerical model that is capable of simulating complex, multilayer WOLED structures is developed to provide an alternative to experimental iterations of OLED design and tests. A cost estimate on the R2R production of WOLEDs for lighting is developed. Assuming a WOLED luminance of 10 klm/m 2 , the cost of a WOLED light engine is anticipated to be $\$ 12.5$ /klm. With incremental reduction in material and driver costs and improved luminance, the cost of WOLED lighting can be reduced to $\$ 6.3$ /klm in the near term. These findings suggest OLED lighting can be volume manufactured by R2R vapor deposition methods with much reduced costs compared to current batch processing methods, potentially positioning WOLEDs for use in numerous premium lighting applications.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2022

A Platform Technology for High-throughput Atomically Precise Manufacturing: Mechatronics at the Atomic Scale

The main objective of this project is to invent the necessary enabling technologies for high throughput atomically precise manufacturing (APM). APM is an emerging technology that refers to any manufacturing capability that enables fabrication of atomically precise structures, components, and devices under programmable control. APM will require positional assembly at the atomic and/or molecular scale, as well as at the nano and microscales using hierarchical assembly to create products ranging from nanoscale and quantum devices to macroscale systems and materials. This project builds on the expectation that commercial viability of APM will depend on a high level of parallelism to achieve the required throughput, a capability that currently does not exist. This project is the first attempt to address this key technological bottleneck.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2026

Non-Contact Eddy Current Method for Assessing Proton Conductivity in Nafion Membranes

Accurate measurement of proton conductivity in Proton Exchange Membranes (PEMs) is vital for fuel cell performance and durability. This study explores eddy current testing as a non-destructive, non-contact and high-rate quality control (QC) method for measuring Nafion membrane proton conductivity, with potential for high-volume manufacturing applications.

33 ADVANCED PROPULSION SYSTEMS↗

DOE OSTI2021

Large-Scale Synthesis of Semiconducting Cu(In,Ga)Se2 Nanoparticles for Screen Printing Application

During the last few decades, the interest over chalcopyrite and related photovoltaics has been growing due the outstanding structural and electrical properties of the thin-film Cu(In,Ga)Se2 photoabsorber. More recently, thin film deposition through solution processing has gained increasing attention from the industry, due to the potential low-cost and high-throughput production. To this end, the elimination of the selenization procedure in the synthesis of Cu(In,Ga)Se2 nanoparticles with following dispersion into ink formulations for printing/coating deposition processes are of high relevance. However, most of the reported syntheses procedures give access to tetragonal chalcopyrite Cu(In,Ga)Se2 nanoparticles, whereas methods to obtain other structures are scarce. Herein, we report a large-scale synthesis of high-quality Cu(In,Ga)Se2 nanoparticles with wurtzite hexagonal structure, with sizes of 10–70 nm, wide absorption in visible to near-infrared regions, and [Cu]/[In + Ga] ≈ 0.8 and [Ga]/[Ga + In] ≈ 0.3 metal ratios. The inclusion of the synthesized NPs into a water-based ink formulation for screen printing deposition results in thin films with homogenous thickness of ≈4.5 µm, paving the way towards environmentally friendly roll-to-roll production of photovoltaic systems.

36 MATERIALS SCIENCE↗

NASA NTRS1989

Deployable aerospace PV array based on amorphous silicon alloys

The development of the first commercial, ultralight, flexible, deployable, PV array for aerospace applications is discussed. It is based on thin-film, amorphous silicon alloy, multijunction, solar cells deposited on a thin metal or polymer by a proprietary, roll-to-roll process. The array generates over 200 W at AM0 and is made of 20 giant cells, each 54 cm x 29 cm (1566 sq cm in area). Each cell is protected with bypass diodes. Fully encapsulated array blanket and the deployment mechanism weigh about 800 and 500 g, respectively. These data yield power per area ratio of over 60 W/sq m specific power of over 250 W/kg (4 kg/kW) for the blanket and 154 W/kg (6.5 kg/kW) for the power system. When stowed, the array is rolled up to a diameter of 7 cm and a length of 1.11 m. It is deployed quickly to its full area of 2.92 m x 1.11 m, for instant power. Potential applications include power for lightweight space vehicles, high altitude balloons, remotely piloted and tethered vehicles. These developments signal the dawning of a new age of lightweight, deployable, low-cost space arrays in the range from tens to tens of thousands of watts for near-term applications and the feasibility of multi-100 kW to MW arrays for future needs.

Hanak, Joseph J.↗

NASA NTRS2007

Critical Issues for Cu(InGa)Se2 Solar Cells on Flexible Polymer Web

Elemental in-line evaporation on glass substrates has been a viable process for the large-area manufacture of CuInSe2-based photovoltaics, with module efficiencies as high as 12.7% [1]. However, lightweight, flexible CuInSe2-based modules are attractive in a number of applications, such as space power sources. In addition, flexible substrates have an inherent advantage in manufacturability in that they can be deposited in a roll-to-roll configuration allowing continuous, high yield, and ultimately lower cost production. As a result, high-temperature polymers have been used as substrates in depositing CuInSe2 films [2]. Recently, efficiency of 14.1% has been reported for a Cu(InGa)Se2-based solar cell on a polyimide substrate [3]. Both metal foil and polymer webs have been used as substrates for Cu(InGa)Se2-based photovoltaics in a roll-to-roll configuration with reasonable success [4,5]. Both of these substrates do not allow, readily, the incorporation of Na into the Cu(InGa)Se2 film which is necessary for high efficiency devices [3]. In addition, polymer substrates, can not be used at temperatures that are optimum for Cu(InGa)Se2 deposition. However, unlike metal foils, they are electrically insulating, simplifying monolithically-integrated module fabrication and are not a source of impurities diffusing into the growing film. The Institute of Energy Conversion (IEC) has modified its in-line evaporation system [6] from deposition onto glass substrates to roll-to-roll deposition onto polyimide (PI) film in order to investigate key issues in the deposition of large-area Cu(InGa)Se2 films on flexible polymer substrates. This transition presented unexpected challenges that had to be resolved. In this paper, two major problems, spitting from the Cu source and the cracking of Mo back contact film, will be discussed and the solution to each will be presented.

Eser, Erten↗

NASA NTRS2013

Carbon Nanotube Microarrays Grown on Nanoflake Substrates

This innovation consists of a new composition of matter where single-walled carbon nanotubes (SWNTs) are grown in aligned arrays from nanostructured flakes that are coated in Fe catalyst. This method of growth of aligned SWNTs, which can yield well over 400 percent SWNT mass per unit substrate mass, exceeds current yields for entangled SWNT growth. In addition, processing can be performed with minimal wet etching treatments, leaving aligned SWNTs with superior properties over those that exist in entangled mats. The alignment of the nanotubes is similar to that achieved in vertically aligned nanotubes, which are called "carpets. " Because these flakes are grown in a state where they are airborne in a reactor, these flakes, after growing SWNTs, are termed "flying carpets. " These flakes are created in a roll-to-roll evaporator system, where three subsequent evaporations are performed on a 100-ft (approx. =30-m) roll of Mylar. The first layer is composed of a water-soluble "release layer, " which can be a material such as NaCl. After depositing NaCl, the second layer involves 40 nm of supporting layer material . either Al2O3 or MgO. The thickness of the layer can be tuned to synthesize flakes that are larger or smaller than those obtained with a 40-nm deposition. Finally, the third layer consists of a thin Fe catalyst layer with a thickness of 0.5 nm. The thickness of this layer ultimately determines the diameter of SWNT growth, and a layer that is too thick will result in the growth of multiwalled carbon nanotubes instead of single-wall nanotubes. However, between a thickness of 0.5 nm to 1 nm, single-walled carbon nanotubes are known to be the primary constituent. After this three-layer deposition process, the Mylar is rolled through a bath of water, which allows catalyst-coated flakes to detach from the Mylar. The flakes are then collected and dried. The method described here for making such flakes is analogous to that which is used to make birefringent ink that is coated on U.S. currency. After deposition, the growth is carried out in a hot-filament chemical vapor deposition apparatus. A tungsten hot filament placed in the flow of H2 at a temperature greater than 1,600 C creates atomic hydrogen, which serves to reduce the Fe catalyst into a metallic state. The catalyst can now precipitate SWNTs in the presence of growth gases. The gases used for the experiments reported are C2H2, H2O, and H2, at rates of 2, 2, and 400 standard cubic centimeters per minute (sccm), respectively. In order to retain the flakes, a cage is constructed by spot welding stainless steel or copper mesh to form an enclosed area, in which the flakes are placed prior to growth. This allows growth gases and atomic hydrogen to reach the flakes, but does not allow the flakes, which rapidly nucleate SWNTs, to escape from the cage.

Schmidt, Howard K.↗

NASA NTRS2020

Current State of the Electrodynamic Dust Shield for Mitigation

The Electrodynamic Dust Shield (EDS) has been developed as a means to lift, transport and remove dust from surfaces for over 18 years in the Electrostatics and Surface Physics Laboratory at NASA Kennedy Space Center. Resent advances in the technology have allowed large-scale EDSs to be fabricated using roll-to-roll techniques for quick efficient processing. The aim of the current research is to demonstrate the 3-dimensional (3-D) version of the EDS and its applicability to various surfaces of interest throughout the Artemis program that require dust mitigation. The conventional two dimensional (2-D) EDS has been comprised of interdigitated electrodes across a surface of alternating polarity to setup non-uniform electric fields in the location of interest for which the particles need to be removed. The 2-D system can be designed to accommodate various phases. For example, the two phase EDS is comprised of two electrodes 180˚ out of phase, while the 3-phase EDS is 120˚ out of phase with the adjacent leg. 4-phase EDS configurations are also possible but for each square wave a high voltage signal is applied to each leg.

Buhler, C. R.↗

DOE OSTI2020

Group-III nitride devices and systems on IBAD-textured substrates

A multilayer structure including a hexagonal epitaxial layer, such as GaN or other group III-nitride (III-N) semiconductors, a <111> oriented textured layer, and a non-single crystal substrate, and methods for making the same. The textured layer has a crystalline alignment preferably formed by the ion-beam assisted deposition (IBAD) texturing process and can be biaxially aligned. The in-plane crystalline texture of the textured layer is sufficiently low to allow growth of high quality hexagonal material, but can still be significantly greater than the required in-plane crystalline texture of the hexagonal material. The IBAD process enables low-cost, large-area, flexible metal foil substrates to be used as potential alternatives to single-crystal sapphire and silicon for manufacture of electronic devices, enabling scaled-up roll-to-roll, sheet-to-sheet, or similar fabrication processes to be used. The user is able to choose a substrate for its mechanical and thermal properties, such as how well its coefficient of thermal expansion matches that of the hexagonal epitaxial layer, while choosing a textured layer that more closely lattice matches that layer. Electronic devices such as LEDs can be manufactured from such structures. Because the substrate can act as both a reflector and a heat sink, transfer to other substrates, and use of external reflectors and heat sinks, is not required, greatly reducing costs. Large area devices such as light emitting strips or sheets may be fabricated using this technology.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Influence of Coating Method on the Performance of Roll-to-Roll Coated PEM Fuel Cell Catalyst Layers

As production of fuel cell vehicles and power systems increases there is a need to understand the process science of fuel cell manufacturing. Industrial production of polymer electrolyte membrane fuel cell (PEMFC) electrodes will rely on continuous roll-to-roll (R2R) coating methods to meet the rates needed for mass production. There are a variety of coating methods that could be used to coat catalyst layers. The different physics of each method may result in different morphologies and performance. Here we present the results of a study comparing fuel cell catalyst layers coated using two R2R coating methods: slot-die and gravure. These two methods were selected because the physics of applying the liquid to the substrate is very different between the two cases. Pt/C catalysts layers were coated directly onto carbon-fiber gas diffusion media to create gas diffusion electrodes (GDEs), without the use of a decal transfer process. These GDEs were assembled into membrane electrode assemblies (MEAs) by hot pressing to Nafion membranes. In situ performance and other electrochemical diagnostics were used to determine the influence of coating method on catalyst layer electrochemical properties. Electron microscopy was utilized to understand the influence of coating method on electrode morphology and its influence on electrochemical properties. We also explored the influence of solvent ratio to understand the potential coupling between ink formulation and coating methodology.

DIRECT ENERGY CONVERSION,MATERIALS SCIENCE↗

DOE OSTI2020

Roll-to-Roll Direct Coating of Catalyst Inks on Membrane Films: Progress and Challenges

Further development of low temperature electrolysis (LTE) systems is of importance to ensure the renewable hydrogen production for hydrogen-based energy systems. The membrane electrode assembly (MEA) is a key component of the LTE system and typically contains a catalyst coated membrane (CCM). To enable the U.S. Department of Energy's hydrogen production cost goal of $2/kg, high volume manufacturing processes will be required to lower manufacturing costs of the CCM. A promising way for high-throughput manufacturing of CCM is using roll-to-roll (R2R) methods that allow the direct coating of electrodes on membrane films. However, there are many challenges with this methodology, both in the coating process as well as with web handling. In this talk, we discuss the membrane-ink interaction by evaluating the solvent uptake of a Nafion membrane system and verify the coatability of various inks through lab-scale coatings onto this system. Furthermore, rheology and surface tension data of the ink will be discussed together with the resulting morphology of the coated electrodes. The R2R-processed CCMs will finally be analyzed using electrochemical performance data and the results put in context with the challenges that the mass production of CCMs for LTE system faces to date.

39 EE - Hydrogen and Fuel Cell Technologies (EE-3F↗