By Kevin Barry, vp of Engineering, Ateios Systems, and Sage Schissel, applications specialist, PCT Ebeam and Integration

Battery electrodes are made by roll-to-roll coating a composite slurry of several materials onto a metal foil. These films – whose production accounts for 80% of total battery cell cost – then are cured, calendered, diecut and assembled into a battery. Through the deployment of an electrode manufacturing platform that utilizes electron beam, Ateios has developed a scaled electrode solution using PFAS-free polymers, no VOC solvents and existing manufacturing infrastructure. The resulting LCO electrode solution proves to be more robust than its traditional PVDF counterpart, maintains high-voltage (>4.25 V) stability and displays superior electrochemical performance in long-term battery cycling. The company also is utilizing this platform to develop and deploy a unique, safe, solid-state battery solution for the Department of Defense (DoD) that otherwise would not be scalable. This article explores the progress that the company has made in advancing battery electrode manufacturing through electron beam curing and how this approach provides solutions to many challenges and limitations currently present with existing thermal curing techniques.

Batteries are ubiquitous in their deployment and usage in our society; from laptops and cellular devices to electric vehicles and other mobility applications, batteries are everywhere, and our reliance on them as a society is only growing with time. As the world’s energy needs constantly are increasing, so are its requirements for a diversified set of energy sources. Lithium-ion batteries have taken up the mantle as the preferred choice to power a clean energy evolution due to their high energy density (Wh/kg, Wh/L), operating voltage, long lifespan and the abundance of the materials required to fabricate them [1]. It has been estimated that the growing Li-ion battery demand, combined with the Net Zero goal (reduction in greenhouse emissions by 2050), will require the annual worldwide lithium-ion battery production to increase by 15x the capacity established at the end of 2023 [2]. To meet these demands, major innovations will need to be made to increase battery output, while also ensuring sustainability and low-cost solutions.

Battery electrodes are one of the key components used to fabricate batteries. Utilizing the Battery Manufacturing Cost Estimation tool from Argonne National Laboratory (BatPaC) [3-5], it can be found that 80% of the costs associated with the production of lithium-ion batteries for electric vehicles revolve around the materials and manufacturing process of producing battery electrodes. Electrodes traditionally are made via a roll-to-roll manufacturing process utilizing VOC (volatile organic compounds) -producing solvents and PFAS (per- and polyfluoroalkyl materials) polymers, and are coated at line speeds of 25-50 meters/min [6,7] (see Figure 1, left). Recently, more light has been shed on the overall cost of utilizing PFAS, both environmentally and economically. While the global PFAS market size is about only 0.5% of total chemical production (~$28 billion), these materials cause an estimated healthcare cost in Europe of between $56-90 billion, and their removal from the environment could cost $20-7,000 trillion/year globally based on current emissions rates [8,9]. Thus, there is a real motivation to advance battery electrode manufacturing to both meet the projected demands of the industry at large and simultaneously eliminate the requirements for harmful chemicals. Ateios has found that the incorporation of an electron beam (EB) into the manufacturing process has enabled the company to make significant strides toward both goals.

The status quo

The conventional method for producing Li-ion batteries is to use an electrode slurry composed of active materials, conductive additives, polymer binder and a solvent that dissolves the binder. This slurry then is coated onto metal foil, thermally dried and calendered (see Figure 1, left) [10]. Next, the coated foil is diecut into electrodes, the battery cell is assembled and liquid electrolyte is added. At an industrial scale, effectively all positive electrodes (cathodes) are produced with the polymer binder PVDF (polyvinylidene difluoride) and the organic solvent NMP (N-methyl-2-pyrrolidone) with negative electrodes (anodes) being produced this way as well, although alternatives exist [11].

Despite leading to excellent product performance, the combination of PVDF and NMP leaves much to be desired in terms of manufacturing. In general, conventional, solvent-based, thermal-drying lines all suffer from similar drawbacks – the need for solvent-based infrastructure, including oxidizers to capture VOCs, explosion-proof equipment and transportation and storage of an evaporative fraction not present in the final product; natural-gas-fueled ovens that are energy-intensive; throughput limitations tied to oven length and required dwell time; and temperature inconsistencies over multiple oven zones. In addition, cathode processing generally is done in a dry-room environment, which increases energy consumption and operational limitations.

The polymer binder PVDF primarily has been chosen for Li-ion cathodes due to its mechanical properties, chemical inertness in typical carbonate-based electrolytes and electrochemical stability over a wide voltage window [11-15]. PVDF is produced by utilizing PFAS or forever chemicals. PFAS substances have come under much scrutiny recently due to their persistence in drinking water and their potential harmful health impacts, resulting in restrictions by both the EPA and EU on their usage across multiple industries [16]. PVDF also is difficult to dissolve in many common organic solvents, thus it often is paired with NMP. NMP is an expensive solvent ($1.5-3.0 per liter) that requires significant energy to be removed via thermal drying (approximately 10x that of water) and needs to be recovered to prevent environmental exposure [17,18]. Moreover, NMP presents a hazard to human health as a reproductive toxicant and eye/skin/respiratory irritant. Prolonged exposure to NMP can damage the liver, kidneys and central nervous system. NMP is facing increasing restrictions in both the EU and the US because of these risks [19]. Due to the impacts of PVDF and NMP on human health and the environment, there is much desire to find other classes of polymer binders to facilitate the scaled production of composite battery electrodes that don’t require such restrictive and expensive manufacturing practices.

The electron beam alternative

When searching for an alternative to PVDF and NMP for battery electrode manufacturing, a few key characteristics are desired: (1) lower production costs, (2) elimination of PFAS and VOCs, (3) no loss in electrode quality/performance, (4) compatibility with existing manufacturing equipment and (5) wide availability of raw materials from a robust supply chain. Many classes of polymers have been investigated to achieve these characteristics, including styrene-butadiene-rubber (SBR) [11,14], acrylic rubber (AR) [13] and polyacrylic acid (PAA) [15], among others [12]. Much success has been found at the industrial scale in deploying SBR as an alternative to PVDF in graphitic anodes [11], which typically operate at lower voltages (<2.0 V). However, the instability of SBR when going to higher oxidizing voltages (between 4.0 – 4.2 V), due to electrochemical oxidation of a double bond in its structure [13,20], means that it has limited applicability for deployment at scale in the production of battery cathodes.

Researchers at Oakridge National Laboratory (ORNL) were some of the first to investigate the applicability of electron beam in battery manufacturing, recognizing that EB had been implemented successfully as a more sustainable alternative to thermal drying in other applications. EB is a robust technology that can polymerize and crosslink materials without solvents and with less energy than a thermal process [21]. High throughputs, with line speeds up to 1,300 fpm (400 mpm), and immediate post-processing are achievable while maintaining a compact footprint because of the near-instantaneous (ms) chemical reactions. The dose (absorbed EB energy) is integral to these chemical reactions and the material properties (e.g., crosslink density) that result; this relationship empowers flexibility as dose is an easily adjusted variable. Moreover, the prevailing chemistry in most EB-curable inks and coatings is the acrylate – a class of materials that widely is available with a variety of molecular backbones (i.e., epoxy acrylates, urethane acrylates, etc.) because they are relatively simple to modify [22]. This diversity of acrylates enables a various range of solutions, depending on the cathode active material (CAM) chemistry and battery application.

ORNL investigated EB-curable acrylates for their use as an alternative to PVDF in battery cathodes [24-26]. With these initial efforts, Lithium Nickel Manganese Cobalt Oxide (NMC) electrodes were produced using the combination of acrylate binders and an electron beam while maintaining other traditional aspects of electrode processing. It was found that using these acrylic materials facilitated an improved mixing protocol and that the resulting electrodes displayed similar performance to their conventional PVDF-based counterparts. One of the key characteristics of these materials is that they can start out as monomers, short oligomer chains or low molecular weight polymers that then are polymerized or crosslinked into higher molecular weight polymers when exposed to an electron beam. This characteristic allows for an improved approach over traditional PVDF-based mixing as the initially smaller molecules are optimal for wetting out the active material and conductive additives in the battery slurry, while the crosslinked polymers formed after EB exposure display excellent substrate adhesion and mechanical robustness. It also was found that these polymers display excellent electrochemical stability over a wide range (tested up to 4.6 V) and that thick, high-quality electrodes could be produced even when cured at speeds of up to 500 fpm (150 mpm), a ≥3x increase over traditional thermal-based processing.

EB cathode processing

Ateios Systems has been working to translate these initial findings from ORNL for the scaled deployment of EB-curable binders into cathode electrodes since 2020. The company’s chosen focus, as one of the most common types of Li-ion batteries, has been Lithium Cobalt Oxide (LCO). LCO makes up 33% of the total battery market and primarily has been applied historically in consumer electronics applications. In recognizing that EB technology offers a possibility that many new battery manufacturing technologies do not – the possibility of a near drop-in solution – the company’s goal was to develop a process that could, at least in part, make use of existing battery manufacturing infrastructure.

The challenge in utilizing existing infrastructure, however, is that, in general, solventless EB slurries are not expected to have the same properties as those slurries comprised of PVDF and NMP. The polymer binder in an electrode typically is minimized (ideally ≤5% by weight) in order to optimize the energy density of the final battery. Abiding by this guideline, a solvent-free EB slurry would consist of ≥95% solids. Compared to a conventional PVDF/NMP slurry, where the percentage of NMP commonly is 40-50%, the EB slurry is unlikely to flow in the same manner. In order to facilitate compatibility with traditional manufacturing equipment, the company’s solution was to employ aqueous-based polymer dispersions. A much-touted advantage of EB production lines is that they can be oven-free (and most often are). In this case, this compromise – the inclusion of an oven step to dry the electrode before EB processing – is balanced by the advantage of scaling up production on existing infrastructure. This approach can be scaled much more quickly in comparison to other competing technologies that require new mixing/coating equipment and potentially are limited by coating speed. In addition, this method still realizes significant energy savings and eliminates the problems associated with organic solvent usage [17-19, 26].

In these scale-up endeavors, it was found that aqueous EB slurries could be produced through traditional planetary-type mixing that maintained the rheological properties of existing NMP-slurries for compatibility with slot-die coating. Furthermore, the EB slurries contained >70% solids (compared to 50-60% solids with an NMP-based slurry [27]), which was facilitated by the wettability of the short EB polymer dispersions. The benefit of this high solids content is the versatility to produce cathodes at a large range of areal loadings at a lower cost, even on a traditional thermal drying setup, due to the reduction in and choice of solvent used. The high solids content also improves quality by diminishing the drying stresses that can occur with thick electrodes [17, 26]. Further, the electron beam curing process is compatible with thick electrodes as the electrons used easily can penetrate opaque materials that are at weight loadings of >25 mg/cm [12, 24].

It also has been proven that the electron beam does not have to be in-line with the coating and drying steps. After drying, the coated electrode is stable enough to be rewound and transported, allowing for the beam to even be offsite. The company has been performing the EB step outside of a dry-room environment and has obtained good results (see above). This flexibility supports swift scaling of the technology. The only required infrastructure addition would be that of an EB line, which has a relatively small facility footprint (see Figure 1) and maintains a capital cost of less than one year’s operational savings from the reduction in natural gas as compared to the traditional coating approach [25]. The combination of these factors – the use of existing infrastructure and an off-line EB – also means that transfer to EB-produced electrodes can be incremental. Conventional electrodes can be produced until shift change, for example, and then with a switch to the EB slurry and a few dial adjustments, the line can be coating and drying electrodes for EB processing. What’s more, while seamless scaling of the technology mitigates much risk and drives faster revenue, it likewise does not preclude further applications of the EB platform that facilitate dry or solvent-free/oven-free electrode production, allowing key benefits now and proofing for the future.

Through work with a US-based toll manufacturing partner for electrode coating, the company found cost savings that are consistent with ORNL’s original predictions when transitioning from the incumbent electrode manufacturing approach to electron beam production (see Figure 2). It has been found that this technology enables up to a 94% reduction in overall electrode processing cost when considering just the energy consumption difference as compared to PVDF-NMP, as well as an 80% reduction in CO₂ emissions [25]. In addition, the electrodes produced are cost-competitive in a global marketplace. The company’s scaled LCO cathode product is manufactured without any VOCs or PFAS, without the need for solvent recovery and on existing manufacturing equipment previously utilized for PVDF and NMP-based electrode coating. The EB binder materials deployed in this product are widely available off-the-shelf solutions utilized for other established industries. This work has demonstrated that the anticipated benefits of EB technology implementation can be translated to the scaled production of battery electrodes.

EB-cured cathode performance

PVDF is the standard polymer binder in Li-ion batteries today because of its excellent performance across multiple metrics. While process improvements – including worker health and safety, sustainability and reduced manufacturing costs – obviously are much desired, widespread adoption of a new binder technology in electrode production is unlikely if it cannot match the benchmark established by PVDF. As a part of the development of the company’s LCO cathode product, much testing was undertaken to compare the two binder systems. Overall, the EB binders display similar electrochemical performance to the incumbent PVDF counterpart (see Figures 4 and 5) while displaying superior substrate adhesion for enhanced post processing [10].

One benefit of PVDF is its stability at high voltages (>4.25 V), which provides broad compatibility with cathode chemistries that can operate reversibly up to these higher values, such as high-voltage LCO (commercially available up to ~4.53 V [28]) and lithium nickel manganese oxide (LNMO, up to ~4.75 V [29]). The key benefit of going to higher voltages in a lithium-ion battery would be to extract more lithium out of the CAM structure, leading to higher battery energy density; thus, working with polymers, active materials and electrolytes that are stable to higher voltages is extremely desirable [30].

In Figure 3, voltage vs. specific capacity plots of electrochemical half (LCO cathode against a lithium metal anode) CR2032 coin cells for both charge (left) and discharge (right) cycles at different current rates are shown. Utilizing high-voltage LCO as the active material in the cathode with a traditional PVDF system, one would expect a specific capacity of ~175 mAh/g (interpreted as the amount of lithium contained in the structure per gram of LCO present in the electrode) when charging to a voltage of 4.45 V [28]. When charging the EB-manufactured half cells up to 4.45 V (left), a smooth charging profile is observed with no spikes or other features present in the curve, and a specific capacity of 175 mAh/g obtained. 

These results indicate that the desired electrochemical reactions (removing lithium from the LCO structure) occur without any unwanted side reactions with the polymer binder. When discharging the cells (right), the lithium reversibly is put back into the LCO structure, obtaining 175 mAh/g again when discharged at the same (C/5) rate (black, solid curve). The other discharge currents present within the discharge plot – C/2, 1C and 1.3C (where C denotes the capacity of the battery and 1C would mean the battery would fully discharge after 1 hour at this rate) – also display the expected performance with a slightly diminished specific capacity as compared to the lower C/5 standard reference rate. 

A common test of battery performance is how the capacity of a battery changes when the battery repeatedly is cycled (discharged and charged). This test is one of the most relevant tests of battery quality because ensuring good cyclability of a rechargeable battery is critical for a broad range of applications, from mobile devices and laptops to electric vehicles. Figure 4 shows the cycling data of pouch cells created with a high-voltage LCO cathode against a graphite anode; the left curve contains a PVDF cathode and the right an EB-produced cathode. The data presented is an average of a batch of batteries for each cell type. The cells were cycled at a 1C charge and discharge current (blue) over ~1,000 cycles in the voltage window between 3.0 and 4.4 V, with state of health checks at lower discharge currents every 50 and 100 cycles (other rates indicated by colors, see legend). The pale blue border in the plot indicates the standard deviation across the batch of cells for the specific capacity obtained at 1C for each cycle.

It is observed that in the first ~150 cycles the rate capability of the PVDF-based batteries is up to 10 mAh/g greater for the 1C charge rate (blue); however, after this early difference, the retention of the EB-produced batteries is superior throughout the rest of the cycling. The PVDF-based batteries cross the 80% capacity retention threshold at approximately 900 cycles (1C charge rate) whereas the EB-produced batteries remain above that threshold for 1,100 total cycles. The EB-produced batteries also demonstrated improved consistency compared to their PVDF-based counterparts. For example, at 1,100 cycles, the standard deviation of the PVDF-based cells is ±11.48 mAh/g while the standard deviation of the EB-produced cells is only
±5.8 mAh/g.

EB solid-state electrolyte

An advantage of EB technology in battery manufacturing is its versatility. The initial interest by ORNL, and now Ateios, has been to use EB to address the shortcomings of the PVDF/NMP binder system, yet there are multiple application possibilities [31]. Another example of how EB is being utilized to advance battery technology is through the development of solid-state battery solutions.

Solid-state batteries widely are considered the next evolutionary step in battery design as they furnish key benefits in terms of safety as well as functionality [32]. Solid-state batteries are created with a solid electrolyte as an alternative to the liquid electrolyte found in most Li-ion batteries. Liquid electrolyte is comprised of a lithium salt dissolved in one or more organic solvents with additives to optimize battery functionality. Acting to eliminate these flammable organic solvents through their deployment, solid-state electrolytes aim to increase safety dramatically for all types of batteries in which they are incorporated [32, 33]. There are many different approaches to create solid-state batteries [34]; however, one of the most common designs involves working with a polymer to create a solid or gel layer that sits in between the anode and cathode in the battery [33].

Although solid-state electrolytes promise increased safety, implementation is not necessarily straightforward. Solid-state electrolytes place new requirements on battery manufacturing [32] and typically display inferior ionic conductivity (broadly, the measurement of the speed to move lithium throughout the battery) as compared to their liquid counterparts [34]. They also require careful design to ensure proper interfacing with the active material particles in the electrode, in order to provide optimal lithium conduction pathways [35]. EB-curable materials have been shown to be promising candidates to balance these challenges of performance, electrode-electrolyte interfacing and to furnish unique avenues for optimized battery cell design [36-38].

Since 2022, the company has been working on an ongoing project with the Department of Defense (DoD) to scale a unique solid-state battery that delivers extreme safety to warfighters that are deployed in the field. Since the war on terrorism, the battery demand for warfighters has increased more than 15x, resulting in a load of over 20 pounds of batteries per person. These batteries often ignite if pierced by a bullet or damaged in other combat scenarios. Thus, the drive to find a solution that provides robust power and safety in a large variety of working conditions is strong.

The solid-state solution created to address these problems originally was developed by the DoD and utilizes EB-modifiable materials to produce high-quality, highly functional, safe batteries. It was designed to utilize non-harmful materials and prevent thermal runaway (battery temperature increasing uncontrollably, causing fire and possibly explosion) in the event of the battery being penetrated by an external object (such as a bullet). Originally, the solution was evaluated with ultraviolet (UV) technology, which initially demonstrated promise; however, UV ultimately was determined to be a limiting factor as it could not be used to fully polymerize the electrolyte once interfaced with the battery electrodes.

The company’s use of EB in battery manufacturing, as well as its extensive experience in thin-film electrode coating, has made scaling this solution a reality. EB is critical as it can penetrate throughout the depth of the electrode. This penetration ensures polymerization and crosslinking through the full thickness of the polymeric materials that are utilized to produce the solid-state electrolyte, while also encouraging appropriate interfacing (wetting) of the bulk of the electrode. This strategy creates a unique avenue to provide optimal lithium-ion conduction pathways that would not be feasible with other designs.

Through implementation of this technology, at the end of 2022, the company was able to produce 1Ah test batteries to be evaluated via a shoot test at a DoD site (see Figure 5). These batteries underwent live fire rounds and continued functioning after being penetrated, with no thermal event occurring. Subsequently, the company has been awarded two follow-up contracts with the DoD to advance the technology and provide EB solid-state battery solutions with multiple different chemistries and battery designs [39, 40]. Through these contracts, the company has optimized the original solid-state design for scalable manufacturing and significantly have increased the pilot manufacturing yields. The company is aiming to advance the technology readiness level (TRL) of the innovation to a level 6 – simulated environment pilot – through further field testing with transition partners in 2026.

Conclusions

Electron beam manufacturing of battery electrodes furnishes key cost, health and environmental advantages over the traditional (thermal-based) manufacturing method, including higher line speeds, reduced energy consumption and elimination of PFAS and toxic solvents. Ateios Systems has been working to translate the original findings of EB manufacturing of battery electrodes from Oakridge National Laboratory to a scalable production environment. The company has found great success in deploying aqueous-based EB polymer dispersions within existing battery electrode manufacturing infrastructure previously used to produce PVDF and NMP-based electrode coatings. The company has successfully demonstrated enhanced performance over the incumbent solution with a high-voltage LCO cathode at scale with a US-based electrode toll manufacturing partner and has found a 94% reduction in overall electrode processing cost. The company also is deploying this technology to produce a unique, safe, shootable, solid-state battery solution based around EB-curable composites. 

Dr. Kevin Barry, vp of Engineering, Ateios Systems, is a materials physicist with extensive experience in thin film growth and characterization, battery slurry formulation development and scalable battery electrode manufacturing. He has more than a decade of thin film fabrication and materials characterization experience and has worked in the energy storage industry for nearly half a decade. Dr. Barry currently leads research and development efforts for Ateios Systems as the VP of Engineering and manages projects for customers in both the commercial and defense sectors. Dr. Barry possesses a diverse skill set having received a B.S. in Astrophysics and a B.S. in Physics from Michigan State University, as well as an M.S. and Ph.D. in Physics from Florida StateUniversity. Dr. Barry can be reached at email: kbarry@ateios.com, www.ateios.com.

Sage Schissel is the Applications Specialist at PCT Ebeam and Integration. In this role, she introduces customers to electron beam technology and works with them to enhance their existing processes by using ebeam or to develop entirely new processes and applications. Schissel graduated from Wartburg College with a Bachelor’s degree in Engineering Science and earned her Doctoral degree in Chemical and Biochemical Engineering from the University of Iowa. She has been involved in ebeam research for the past decade. Schissel can be reached at email: sage.schissel@pctebi.com,  www.pctebi.com.

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