Materials for 3D Printed Metal and Metal-Ion Batteries

Materials for 3D Printed Metal and Metal-Ion Batteries Tomás García Rodríguez,[a] Jesus I. Medina Santos,[b] João Coelho,[c, d] and Sergio Pinilla*[a] The review provides an overview of the latest innovations, trends, and challenges in the field of 3D-printed metal and metal-ion batteries. It focuses on the materials used in the printing of batteries, including electrodes, electrolytes, and other electroactive components. Compared to other highquality reviews on the topic, this review provides a broader selection of materials that are expected to gain attention in the next few years, such as redox-active polymers and metalorganic frameworks. This work gives an overview and insight into the latest trends in printing techniques as well as a statistical review of their uses and strengths. We have also gathered the latest works done for each of the material types, and we have taken the opportunity to put them in context and use them to exemplify in which direction is the field going. The review concludes with a critical view of the challenges ahead and a discussion of the direction that the field is taking as well as the external factors that might help to define its future. 1. Introduction The rising demand for portable consumer electronics and the impending widespread use of electric vehicles (EVs) have led to the need for sustainable and more efficient fabrication methods for electrochemical energy storage devices (EESDs).[1] Lithiumion batteries (LIBs) have been the primary energy storage system since their introduction in 1991, especially for portable electronics like computers, cell phones, and cameras. Modern LIBs are a well-established and mature technology, with production methods that have been optimized for industrial scale. The most used method for preparing electrodes is slurry casting. This method is based on simple and easily scalable steps, which partially explains its widespread adoption.[2,3] However, electrodes deposited by slurry casting are at most 100 μm thick.[2] Modern batteries are also regulated in specific sizes and usually restricted to specific form factors such as cylindrical, coin-cell, rectangular, and prismatic types.[4] Therefore, battery production by slurry casting is not an ideal process for novel applications such as the Internet of Things (IoT) concept, which typically require flexibility, miniaturization, easy integration, and adaptable geometries.[3] On the other hand, printing batteries allow for a cost-effective, customized, largearea, and high-volume layer deposition. To be considered a printed battery, at least one or more of its components (current collectors, electrodes, or separator/electrolyte) must be produced using printing technologies.[3] These printing methods include ink-jet printing (IJP), screen-printing, and flexographic printing, among others. Some manufacturing techniques allow the layering of material creating complex and controllable 3D structures, this is generally known as 3D printing or additive manufacturing (AM).[5–8] In recent years, this approach has rapidly developed into a research field that offers methodologies and solutions for various technological applications, including energy storage. The increasing adoption of additive manufacturing is revolutionizing the production of wearable electronics and EESDs such as batteries, supercapacitors, and fuel cells. This surge can be attributed to its outstanding process versatility, precise control over geometrical aspects, and potential to reduce costs and material waste.[7,9] In this comprehensive review, major AM processes like inkjet printing, direct ink writing (DIW), fused deposition modeling (FDM), and selective laser sintering/melting (SLS) along with possible configurations and architectures, are elaborately discussed. The application of 3D-printed energy storage devices in wearable electronics, IoT-based devices, and electric vehicles is also mentioned in the review. Extensive research and continuous progress in this field are expected to enhance the longevity, industrial scalability, and electrochemical performance of 3Dprinted energy storage devices in the future.[6] These include low waste generation, higher flexibility in the choice of electrode substrate, and one-step manufacturing in the micro to macro-scale. As digital technologies, AM manufacturing also provides significant versatility and freedom in electrode design for complex structures with controlled thicknesses. This provides a significant advantage over planar devices, enabling an increase in areal capacity without sacrificing power density due to improved ion flow.[10] This results in a separation of the energy and power density of the batteries, making it easier to [a] T. García Rodríguez, Dr. S. Pinilla Electrochemical Processes Unit, IMDEA Energy, Avda. Ramón de la Sagra 3, Móstoles, Madrid 28935, Spain, E-mail: [email protected] [b] Dr. J. I. Medina Santos CRANN/School of Chemistry Trinity College Dublin, College Green, Dublin 2, Ireland [c] Dr. J. Coelho Dpto. Física de La Materia Condensada Universidad de Sevilla Avda. Reina Mercedes SN, 41012, Seville, Spain [d] Dr. J. Coelho Instituto de Ciencia de Materiales de Sevilla CSIC – Universidad de Sevilla Avda. Américo Vespucio 49, 41092, Seville, Spain © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 136/154] 1 ChemElectroChem 2024,11, e202400206 (1 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem www.chemelectrochem.org Review doi.org/10.1002/celc.202400206 customize the batteries for specific applications. Compared to 2D printing techniques, AM offers more sustainable approaches due to its flexibility in the type and amount of solvent used for the ink formulation. Furthermore, it expands the range of printable materials, including polymer composites, metal alloys, concrete, ceramics, and more. This facilitates the printing of not only the electrodes but also the electrolytes, current collectors, and casings, reducing prototyping costs and streamlining the device. Cost efficiency is a significant advantage for both emerging applications and new battery chemistries, accelerating innovation cycles and the lab-to-fab process. Among the various types of possible 3D printed architectures, the most commonly reported are stacked, interdigitated, and fibrous structures (see Figure 1).[11] Stackable batteries have the same architecture as conventional LIBs, but they are composed of printed components which can have non-conventional shapes. The interdigitated configuration is a popular architecture known for its high aspect ratios, which optimize ion transport and enhance energy density. Finally, fiber-shaped or 1D batteries typically have a helical or parallel structure. Although they have lower capacities and power densities, their mechanical properties make them attractive for wearable and flexible technologies.[11] Electrodes are the most commonly printed battery component, but printed electrolytes and current collectors are also gaining popularity. These architectures, along with new fabrication techniques, offer numerous application opportunities, ways to overcome material limitations, and integration options. This review provides an overview of the latest innovations, trends, and challenges in this fast-paced field clearly and concisely. While there are already high-quality reviews available on printing techniques and mechanisms,[12] design,[4] and applications,[8] this review will focus on materials. We have expanded the range of materials compared to other reviews,[13,14] including those that have received less attention in the field, and it is expected that due to the shift of society towards sustainability, their popularity will increase in the next few years. This is the case, for instance, with redox-active organic materials. Additionally, we provide an overview of the latest advances and trends in other electroactive materials, printing technologies, and printed electrolyte choices. We conclude this review with a statistical analysis of the field and a critical assessment of the challenges ahead. Tomás García Rodríguez received his Bachelor’s degree in Physics (2022) and Master’s degree in Energies and Fuels for the Future (2023) from Universidad Autónoma de Madrid. He currently works as a predoctoral researcher under the supervision of Dr. Sergio Pinilla in Electrochemistry at IMEDA Energy. His research is mainly focused on next-generation lithium-ion batteries. Jesús Medina Santos is a post-doctoral researcher at Trinity College Dublin. He received his bachelor‘s (2017) and master‘s degree (2019) in Chemical Engineering from the University of Castilla la Mancha and his Ph. D. in Electrochemistry from Autonomous University of Madrid in 2024. His research has been focused on the characterization of lithium-ion batteries and the next battery generations. João Coelho has been a researcher at the Department of Condensed Matter Physics, Faculty of Physics, University of Seville, and the Seville Institute of Materials Science (ICMS), since 2023. He received his Ph.D. in Chemistry from Trinity College Dublin in 2016. He then moved to Portugal to work as a researcher at the NOVA School of Science and Technology in 2020. His research focuses on the sustainable development of 2D nanomaterials for supercapacitor and battery applications, mainly for flexible and wearable technologies. Sergio Pinilla has been a senior assistant researcher at the Electrochemical Processes Unit from IMDEA Energy, since 2022. He received his Ph.D. in Physics from Universidad Autónoma de Madrid in 2017 and then moved to Ireland to work as a post-doctoral researcher at Trinity College Dublin until 2022. His research interests lie in the development of batteries with advanced designs and unconventional battery characterization procedures for modeling purposes. Figure 1. All-printed batteries (APT) main structural configurations, along with device properties. Reproduced with permission.[11] Copyright (2023) Wiley-VCH. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 137/154] 1 ChemElectroChem 2024,11, e202400206 (2 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 2. Printing Techniques Although there are many additive manufacturing methods, not all can be employed in the fabrication of electrochemically active parts due to the material requirements of EESDs. Four big families of printing techniques can be identified based on how the material is fixed in place. These are: light-based, filamentbased, powder-based and jetting-based.[12] In addition, there is a fifth family known as template-assisted printing, which includes a variety of deposition techniques that traditionally would not be considered additive manufacturing methods, such as spray coating or screen printing. However, by the use of templates, they can produce 3D structures through the subsequent application of layers. In the following lines the strengths and weaknesses of each technique are discussed in the context of printed batteries and in Figure 2 is provided a qualitative radar map that broadly gathers the advantages of the mentioned families. 2.1. Light-Based This family of techniques is based on the use of light sources to cure resins or suspensions, as shown in Figure 3A.[12] The most common technique among these is SLA, which employs photocurable resins that react to ultraviolet (UV) light. This technique offers high resolution and good interconnection between layers.[17] However, the properties of the cured materials are not always compatible with the requirements of the EESDs and thus, this type of technique is generally employed just to build 3D polymeric substrates that are later covered or coated with active materials. This strategy has been used to prepare both electrodes[18] and solid electrolytes (SEs).[19] There are alternative options for using stereolithography (SLA) in printed batteries. For example, one of the most common polymeric SEs, polyethylene oxide (PEO), is photocurable and, therefore suitable for use in light-based techniques.[20] Another approach is to include photocurable resins in the inks. After printing, the piece is subjected to a thermal treatment to remove the cured resins. However, this is Figure 2. Radar map of the described five families of printing techniques. The scoring of each family was done based on the works of references.[4,14–16] Figure 3. Main 3D printing techniques families (A to E) with their respective schematic representation and literature examples. Example in (A) reproduced with permission of.[19] Copyright (2018) The Royal Society of Chemistry. Example in (B) reproduced with permission of Ref. [29] Copyright (2023) Wiley. Example in (C) reproduced with permission of Ref. [27]. Copyright (2021) Elsevier. Example in (D) reproduced with permission of Ref. [30] Copyright (2019) Wiley. Example in (E) reproduced with permission of Ref. [37]. Copyright (2021) Elsevier. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 138/154] 1 ChemElectroChem 2024,11, e202400206 (3 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License only possible with materials that have high thermal stability such as ceramic electrolytes as the ones printed by Sabato et al.[21] 2.2. Filament-Based Filament techniques are the most commonly used for fabricating 3D EESDs. These techniques involve depositing semisolid yarns through a nozzle that solidifies shortly after deposition (Figure 3B). Among this family of techniques, we find two main approaches, FDM and DIW. FDM involves depositing thermoplastic filaments that are heated to a semi-molten state at the nozzle and solidified upon deposition in the printing bed. Although is the most extended 3D printed methodology, its application in the field of printed batteries is hindered by the limited range of printable materials. The most extended strategy for this technique is based on mixing the active materials with a thermoplastic such as polylactic acid (PLA), acrylonitrile butadiene styrene (ABS), or polycarbonate (PC). However, the low conductivity of these matrixes restricts the selection of active materials and the amount of thermoplastic that can be used in the blends. This technique has been widely used for the printing of electrodes (Table 1) with comparable capacities, rates, and conductivities to those fabricated by slurry casting. This performance is due to the substitution of the binder with the thermoplastic which also allows a solvent-free deposition.[22,23] FDM has also been used to print electrolytes. In this case, the most common strategy is the infiltration of preprinted PLA-based membranes with liquid electrolytes forming quasi-solid electrolytes (QSEs).[24] However, there are also true solid-state electrolytes printed by FDM based on solid polymeric electrolytes (SPEs). In these cases, PLA is combined with a SPE such as PEO and lithium salts to form the electrolyte, as in the case of Ragones et. al.[25] On the other hand, DIW is a printing technique based on the extrusion of visco-elastic ink through a nozzle. DIW allows the use of a wide variety of active materials and additives.[14] The end composition and microstructure of the electrodes are mostly the same as in the slurry-based depositions traditionally employed in industrial battery production.[15] The critical aspect of this deposition technique is the ink formulation and its rheological properties. The inks must exhibit shear-thinning behavior to flow properly through the nozzle but then maintain the filament-like shape once deposited. The great flexibility of this deposition technique has allowed the printing of numerous materials for cathodes, anodes, and SEs (Table 1), including even ceramic electrolytes.[26] 2.3. Powder-Based This family of techniques is based on the sintering or melting of powders. High-energy lasers are projected on powder-containing beds to sinter the materials layer by layer until achieving the desired shape (Figure 3C). The most common technique is SLS, and it is usually used for the sintering of polymers and ceramics. Although it has been demonstrated its use for batteries, its material selection is still complex compared to filament-based techniques, it produces residual stress on the material, the control of the microstructure properties of the final material is still a challenge and the throughput is low.[8,12] It has been reported its use for the preparation of thick, solventfree Lithium Nickel Cobalt Aluminum Oxide, (LiNi0.8Co0.15Al0.05O2, NCA) cathodes, although due to the low maturity of the technique in the field, the obtained performance was very low (16 mAhg1compared to the nominal 167.7 mAhg1obtained by slurry-based techniques).[27] Similarly, Chen et al.[28] prepared a magnesium anode for LIBs through SLS, obtaining relatively low performances. 2.4. Jetting-Based Jetting techniques are based on the deposition of low-viscosity inks through small nozzles that move along the surface creating thin layers (Figure 3D). Resolution tends to be very high although it depends on the jetting mechanism, nozzle size, rheology, and surface tension of the inks used for deposition.[16] The two more representative exponents of jetting-based techniques are IJP and aerosol jet printing (AJP). IJP is based on the ejection of droplets onto a surface through a nozzle. It can be continuous inkjet (CIJ) or drop-ondemand (DOD).[4] IJP is very flexible in terms of printable materials and only requires a stable solution with a particle size compatible with the nozzle to avoid clogging. The control of IJP deposition is based on the ink formulation and its interaction with the substrate,[8] and its resolution is typically in the 10– 150 μm range although higher resolutions have been achieved.[4,16] The main disadvantages of IJP are its low throughput and inability to produce self-standing structures, which limits its use mainly to thin film applications. This is reflected in the literature, where films tend to be just a few microns thick, which limits the usable particle size[31] and favors the use of nanomaterials.[32] IJP has been extensively used in the preparation of both thin film cathodes[32,33] and anodes.[34,35] AJP is a contactless technique that achieves resolutions in the range of 10 μm by jetting material through the spraying of ink with pressurized gas. The annular sheath gas flow focuses the stream of ink, allowing for deposition over any substrate regardless of surface roughness.[36] This technique also enables the deposition of a wide variety of materials with looser ink requirements compared to IJP. To increase its throughput, prevent pooling, and achieve thicker electrodes, lasers can be used to assist in the solidification of inks.[30] However, controlling the microstructure can be challenging and may result in highly porous structures.[15] This technique has gained recent attention and there are examples of printed anodes,[15] cathodes,[30,37,38] and solid-polymeric electrolytes.[38] Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 139/154] 1 ChemElectroChem 2024,11, e202400206 (4 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Table 1. Summary of representative electrodes printed by different 3D printing techniques and available data from commercial electrodes. Materials within the same electrode are separated by ’/’, while ’–’ separates different electrodes. Materials Category Technique Chemistry Capacity Cycles Capacity retention (%) Year Ref. LFP Commercial Conventional Li-ion 170 mAhg1at 0.1 C Thickness=70 μm Mass loading=7.3 mgcm2 – – – [43] NMC811 Commercial Conventional Li-ion 200 mAhg1at 0.1 C Thickness=16 μm Mass loading=10 mgcm2 – – – [43] LMO Commercial Conventional Li-ion 100 mAhg1at 0.1 C Thickness=60 μm Mass loading=12.5 mgcm2 – – - [43] LCO Commercial Conventional Li-ion 160 mAhg1at 0.1 C Thickness=65 μm Mass loading=12.5 mgcm2 – – – [43] LTO Commercial Conventional Li-ion 165 mAhg1 at 0.1 C Thickness=60 μm Mass loading=7.6 mgcm2 – – – [43] Graphite Commercial Conventional Li-ion 370 mAhg1at 0.1 C Thickness=60 μm Mass loading=6.5 mgcm2 – – – [43] LFP Standard FDM Li-ion 116 mAhg1at 0.2 C – – 2024 [23] LFP Standard FDM Li-ion 150 mAhg1at 0.5 C 100 at 1 C 2023 [22] LFP Standard FDM Li-ion 145 mAhg1at 0.5 C 150 at 1 C 100 2018 [44] LFP Standard FDM Li-ion 160 mAhg1at 50 mA g130 97 2017 [45] LFP/PLA/CNT Standard+Nanomaterials FDM Li-ion 156 mAhg1at 0.1 C 200 at 0.5 C ~95 2021 [46] LFP/MgO Standard DIW Li-ion 160 mAhg1at 0.33 C 800 at 1 C 96 2022 [47] LFP Standard DIW Li-ion 155 mAhg1at 0.33 C - - 2020 [48] LFP Standard DIW Li-ion 160 mAhg1at 0.2 C - - 2019 [49] LFP/MWCNTs Standard+Nanomaterials DIW Li-ion 150 mAhg1at 0.5 C 500 at 5 C ~80 2021 [50] LFP/PEDOT:PSS/CMC Standard+Organic DIW Li-ion 2 layers: 150.9 mAh g1 12 layers: 100 mAh g1at 0.5 C 100 at 0.2 C Over 80 2021 [51] LFP Printed electrolyte AJP Li-ion 136 mAhg10.5 C 30 2019 [30] LFP Printed electrolyte AJP Li-ion 115 mAhg1at 1 C 50 2019 [37] LFP Printed electrolyte AJP Solid State Li 120 mAhg1at 1 C (60 °C) 150 2023 [38] LFP – LTO Standard FDM Li-ion 140 mAhg1at 50 mA g130 81 2017 [29] NMC Standard DIW Li-ion 192 mAhg1at 0.2 C 50 at C/3 89,7 2023 [52] NMC Standard Screen printing Li-ion 170 mAhg1at 0.2 C 100 at 1 C 50 2023 [53] Li1.15K0.05Mn0.54Ni 0.13Co0.13O2Printed electrolyte IJP Li-ion 240 mAhg1at 0.01 C 70 70% 2020 [33] LMO/PoPD/0D Carbon Standard+Organic FDM+electrodeposition Li-ion 69 mAhgat ~1.2 C 200 84.4 2021 [54] LMO Standard DIW Li-ion 103 mAhg1at 0.2 C 30 at 0.1 C 100 2020 [55] Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 140/154] 1 ChemElectroChem 2024,11, e202400206 (5 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Table 1. continued Materials Category Technique Chemistry Capacity Cycles Capacity retention (%) Year Ref. LCO Standard FDM Li-ion 83 mAhg1at 0.2 C – – 2023 [56] V2O5/Mxene Nanomaterial IJP Li-ion 321 mAhg1at 1 C 680 at 10.5 C 91.8 2021 [32] NaMnO2 Standard DIW Na-ion 120 mAhg1at 0.1 C – – 2023 [57] LTO Standard FDM Li-ion 148 mAhg1at 50 mA g130 75 2017 [58] LTO Standard DIW Li-ion 160 mAhg1at 0.2 C 100 at 1 C 82,6 2022 [59] LTO Standard DIW Li-ion ~140 mAhg1at 1 C 30 2019 [60] LTO Standard IJP Li-ion 125 mAhg1at 0.5 C 680 91.8 2021 [34] LTO Printed electrolyte AJP Li-ion ~115 mAhg1at 1 C – – 2023 [15] Graphite Standard DIW Li-ion 350 mAhg1at 0.2 C 100 at 0.2 C 100 2021 [61] Graphite Standard DIW Li-ion 345 mAhg1at 0.2 C 100 at 0.2 C 95 2022 [62] Graphene Nanomaterials IJP Li-ion ~942 mAhg1at 0.1 C 100 at 2 C ~87 2021 [63] Si/PEDOT:PSS/PEG Nanomaterials+Organic DLP Li-ion ~1600 mAhg1at 0.1 C 125 72 2022 [64] Si/PLA/Graphene/CB-doped Poly pyrrole Nanomaterials+Organic FDM Li-ion 345 mAhg1at 20 mAg1350 at 20 mAg1 96 2021 [65] Si/rGO Nanomaterials FDM Li-ion 16.2 mAhcm270 at 200 mAg1 75.4 2022 [66] Si/PEDOT:PSS Nanomaterials+Organic IJP Li-ion ~2300 mAhg1at 0.2 C 100 61 2017 [34] MoS2/rGO Nanomaterials 3D freeze-printing (3DFP) Na-ion 429 mAhg1at 100 mAg1– – 2019 [58] Si/rGO – LFP/rGO Nanomaterials FDM Li-ion ~100 mAhg1at 0.2 C 140 at 0.2 C ~62 2022 [67] TPU/LFP – TPU/LTO Standard+Organic FDM Li-ion 100 mAhg1at 0.33 C 50 2019 [66] Disperse blue 134 anthraquinone (DB) Organic AJP Li-ion ~70 mAhg1at 0.2 C – – 2019 [68] TFSI-ion ~70 mAhg1at 0.2 C – – DB – DB Organic AJP Li and TFSI ions ~60 mAhg1at 0.2 C 250 62 PAQS Organic Stencil/screen printing Li-ion 117 mAhg1at 0.2 C 100 at 0.2 C 84 2021 [69] Na-ion 127.6 mAhg1at 0.2 C – – PAQS – LTO Organic Stencil/screen printing Li-ion 64 mAhg1-at 0.2 C 500 at 0.5 C 73 R2R Stencil/screen printing Li-ion 57 mAhg1at 0.2 C 100 at 0.2 C 61 1D Carbon/PAA doped PANI Organic FDM+electrodeposition Zn-ion 214.6 mAhg1at 400 mA g11000 78.1 2022 [70] Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 141/154] 1 ChemElectroChem 2024,11, e202400206 (6 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 2.5. Template Assisted As mentioned earlier in this section, templates enable the production of 3D structures using techniques that typically are not considered additive manufacturing techniques. This is the case of 3D screen printing, which involves the application of inks or powders with the aid of a mask that can change its shape as it moves in the Z direction (Figure 3E). These are later sintered or dried, retaining their structure and achieving resolutions as low as 50 μm.[39] This technique has been used to prepare various types of objects, from small detailed metallic pieces[40] to layer-by-layer engineered drugs.[41] In the field of batteries, this methodology is behind the patent filed by Blackstone Technology GmbH for the 3D printing of solid-state batteries.[42] 3. Electroactive Materials for 3D-Printed Electrodes One of the main attractiveness that 3D printing has for battery manufacturing comes from the limitation of current manufacturing methods to maximize simultaneously energy and power density. While in planar devices increasing electrode thickness always results in reduced power density due to slower kinetics, by smart 3D patterning is possible to overcome this limitation. This opens a whole new set of possibilities where materials that were underperforming in planar devices can find new uses. In this section, we explore the latest trends and works done with standard battery materials, in which we include cathode and anode materials but also, we give special consideration to active materials and additives in the nanoscale. Afterward, we cover a very incipient yet important family of materials that are the redox active organic materials, which are gaining momentum in the light of sustainability considerations. 3.1. Standard Electrode Materials Commercially available LiBs use alloys, metal oxides, and carbon-based materials as electrodes. These materials are chosen for their balance between cost, performance, and safety. However, conventional electrodes encounter significant challenges, such as the requirement for rapid charging of electric vehicles[71] and high areal capacity to enhance overall energy density.[72] Recently, 3D printing technologies have shown potential in enhancing electrode materials, providing opportunities for improved performance and design flexibility. The following sections provide an overview of relevant examples of successfully 3D-printed cathodes and anode materials for battery applications. Due to their importance in the development of EESDs, an additional section is included to highlight the main advantages of nanomaterials in additive manufacturing and energy storage. 3.1.1. Printed Cathode Materials Among the positive electrode materials, lithium ferrophosphate (LFP) has a low theoretical capacity (170 mAhg1) and voltage (3.65 V vs Li/Li+). However, it has been widely used for LiBs owing to its good thermal stability, high cyclability, and low content on critical raw materials.[73] Therefore, LFP is a suitable candidate for testing 3D printing technologies where sustainability is a factor as important as performance. For example, Sun et al.[74] were pioneers in the use of 3D-printed electrode materials. They used FDM to fabricate a microbattery with LFP, achieving initial capacities of 160 mAhg1at 1 C in a half-cell and performing 30 cycles in a full cell. Wang et al. further demonstrated the versatility of 3D printing in battery applications by using FDM to prepare an all-fiber battery with LFP/ lithium titanate (LTO) electrodes. This resulted in a flexible and wearable battery with an initial capacity of 110 mAh g1and capacity retention of 81% after 30 cycles at a current density of 50 mAg1.[58] FDM was also used to prepare thick LFP electrodes for high energy density applications delivering 140 mAhg1for 150 cycles at 1 C. Electrodes prepared by FDM can be up to 1500 μm thick, which is significantly greater than the thickness of electrodes prepared by conventional techniques.[75] However, longer cycling performance tests should be carried out to compare with the cycling performance of conventional electrodes[76] and reach the autonomy requirements of commercial applications.[77] Nevertheless, these findings indicate that 3D printing allows for the preparation of various battery configurations by using commercially available materials (Figure 4). Finally, several attempts were also made to prepare LFP electrodes by DIW.[47–49,78] However, the work done by Li et al.[50] was remarkable because they were able to prepare a high areal capacity and power density electrode by DIW and freeze-drying processes. The obtained grid structure allowed the electrode to deliver an initial rate capacity of 140 mAhg1at 1 C and capacity retention of 80% after 500 cycles at a high rate (5 C). As previously stated, LFP has a low theoretical capacity and voltage; thus, making it unsuitable for high-energy and highpower applications. On the other hand, lithium cobalt oxide (LCO) electrodes have higher voltages (4.2 V vs Li/Li+) than LFP and have been the main industrial choice for portable applications.[79] Therefore this made it one of the prime choices for preparing 3D high-energy electrodes, as reported by TorreFigure 4. (A) SEM image from LFP/LTO microbattery. Reprinted with permission from[74]. Copyright (2013) WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. (B) Graphical illustration of fiber batteries (left) and optical image of textile fibers and electrodes (right). Reprinted with permission from Ref. [58]. Copyright (2017) WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. (C) Optical images of LFP electrodes prepared by 3D printing with different structures. Reprinted with permission from Ref. [44]. Copyright (2018), Americal Chemical Society. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 142/154] 1 ChemElectroChem 2024,11, e202400206 (7 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License Gamarra et al.[56] In this study, they were able to prepare an 850 μm thickness LCO electrode by FDM. However, the capacity achieved was 100 mAhg1at C/12, which is 36 % of the theoretical capacity and lower than that of LFP. Another alternative that can be considered is lithium manganese oxide (LMO) since it has a theoretical capacity of 460 mAhg1and a voltage of up to 4.5 V.[80] In contrast, it presents some disadvantages, such as low cycling performance and long-term storage owing to the dissolution of Mn and the decrease in Liion diffusion.[81] Despite these disadvantages, LMO have been prepared by 3D printing several times. For example, a robocasting process, such as the DIW process, was carried out to prepare thick LMO electrodes from highly concentrated aqueous inks.[55] This study is another example of using 3D printing to prepare thicker electrodes than conventional techniques; however, it also showed poor rate and cycling performance. These materials have not received significant attention in 3D printing applications, and other alternatives such as lithium nickel manganese cobalt oxide (NMC), have been the main choice for high-energy applications. NMC is at a mature stage of development because of its use in commercial electric vehicles.[82] Additionally, the theoretical capacity of NMC is 275 mAhg1with a voltage above 4.2 V vs Li/Li+,[83] making it a suitable candidate for preparing highenergy electrodes by 3D printing. However, to meet the current requirements for fast charging, the material structure must be optimized to increase the electrical conductivity and diffusion rate. 3D printing has the potential to improve electrode performance by allowing tuning of the material structure, as demonstrated by Wang et al.[53] In this study, channels of different sizes and distances were created in the NMC electrode (Figure 5A). The results showed that channels with a size of 0.1 mm and a distance of 0.2 mm improved the diffusion rate of lithium ions in the positive electrode, which resulted in higher charge current values of up to 6 C. A similar approach was adopted by Tao et al.,[52] who used DIW to deposit NMC ink on a hot plate. The obtained thick electrodes showed an enhanced diffusion rate, increasing the battery performance at 5 C compared to conventional slurry casting. 3.1.2. Printed Anode Materials LTO has been one of the earliest materials used for preparing micro batteries and one of the most used electrodes in 3D printing to prepare full cells[48,78,84] thanks to its zero-volume change and electrochemical stability. Most of the works done focusing on the 3D printing of this material were aimed towards achieving thick electrodes with good kinetics. A good example is the work developed by Liu et al.[59] where they used DIW at low temperatures, to create vertically aligned pores in the electrode structure reducing the transport distance of the ions (Figure 5B). Graphite is the most common negative material for the conventional slurry casting method due to its high theoretical capacity (372 mAhg1) and low potential (0.01 V vs Li/Li+). However, it has not received significant attention in 3D printing applications for preparing full cells, possibly due to its low working potential. Common electrolytes are reduced at this voltage, forming a solid electrolyte interphase (SEI),[85] which has a significant impact on the performance of conventional electrodes. Thus, it could add a new challenge to the study of complex structures made by 3D printing. Despite this fact, Gastol et al.[86] compared the performances of graphite electroFigure 5. (A) Representation of vertically align Li+channels for thick NMC electrodes. Reprinted with permission from Ref. [52]. Copyright © 2023 Wiley-VCH GmbH. (B) Top view magnified top view and side view of thick LTO electrode. Reprinted with permission from Ref. [58]. Copyright Copyright © 2022, The Author(s). (C) Front view and side view of thick graphite electrode. Reprinted with permission from Ref. [61]. Copyrigth © 2022 The Author(s). Published by Elsevier B.V. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 143/154] 1 ChemElectroChem 2024,11, e202400206 (8 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License des prepared by slurry casting and DIW. They demonstrated the importance of the rheological properties for slurry casting and 3D printing through the introduction of a secondary solvent. This addition enables modification of the graphite microstructure, enhancing Li-ion transport and carbon black dispersion. Furthermore, the 3D-printed electrode exhibited improved cycling performance due to its increased electrical conductivity and lower average tortuosity compared to slurrybased electrodes. Zhang et al.[61] also adopted a similar approach, comparing the performance of slurry casting and direct DIW EESDs. This study examines the impact of varying the number of layers and printing structures on the electrochemical performance of graphite electrodes. The results show that increasing the number of layers results in a higher initial capacity over a given area, indicating no negative influence on lithium diffusion. However, the cycling performance of electrodes with a thickness of 1 mm was poor, while those with a thickness of 0.6 mm demonstrated improved results but were only cycled for a limited period of 60 cycles. Another example of thick graphite electrodes can be found in the study by Xu et al.[62] (Figure 5C). They were able to prepare electrodes with a thickness of 786.7 μm and achieved a capacity of 13.68 mAhcm2at 0.1 C. However, their results showed poor high-rate performance. Thus, there is a clear trend for standard electrodes based on the preparation of thick electrodes by 3D printing. With the renewed interest that solid-state batteries have brought to the lithium metal anodes, many have seen in 3D printing technology one way to solve one of its main challenges: dendrite formation. By 3D structuring the current collector it has been observed how the plating/stripping of Li can be significantly enhanced compared to planar current collectors, stabilizing the surface and allowing a stable cycling.[87,88] This approach is not unique to Li-metal batteries and it has been further used in other chemistries such as aqueous Zn batteries.[89] 3D printing strategies have also reached sodium chemistry, where the similarities between lithium and sodium electrode materials have facilitated the transition. For example, sodium manganese oxide electrodes behave similarly to LMO, and thanks to the transferable experience it has been used in 3D printing.[57] While there have been advancements in sodium-ion technologies, they are still in the early stages of development compared to lithium-ion technologies. As such, research on 3D printing for sodium-ion battery electrode materials is currently in its infancy as well. 3.1.3. Nanomaterials for Printed Battery Electrodes It has been shown that standard electrode materials can make the transition towards printed technologies. However, it is important to stress the fact that these materials at nanoscale along with other novel nanomaterials, have played a crucial role in battery development. The integration of nanomaterials as active material has emerged as a promising electrode alternative, as well as a synergistic option when used as additives. Nanomaterials are defined as materials that have at least one spatial dimension between 1 and 100 nm. According to their shape can be categorized as zero D, 0D (nanoparticles and quantum dots), 1D (nanotubes and nanorods), and 2D (nanosheets, such as graphene and MXenes).[90,91] At this scale, materials exhibit unique properties that are not present in their bulk counterparts, even at the microscale.[92,93] As such, nanomaterials can impart mechanical, optical, thermal, magnetic, and biological properties to 3D printed architectures, such as sensors,[94,95] antennas,[96,97] energy storage devices,[1,63,98] among others. Regarding electrode fabrication, it is widely accepted that nanomaterials improve battery performance due to their low dimensionality, which shortens the ion diffusion path and reduces charge-transfer resistance.[99–101] In fact, the slow kinetics of Li+and e-diffusion in the electrode materials are the main factors hindering the achievement of high-power density batteries.[101] The mean diffusion time, tD, is defined as: tD¼L2 2D where, Dand L, are the diffusion coefficient and length, respectively.[101] Assuming that the commercially available electrode material has an Lvalue of approximately 10 μm, reducing the particle size to the nanoscale range (<100 nm) results in a four-order-of-magnitude reduction in the mean diffusion time.[101] As such, there has been significant research activity on the printing of nanomaterials for battery applications.[12,17,102] Nanoparticles can also facilitate the use of high-capacity materials in battery electrode fabrication. For instance, transition metal oxide (MO, where M is Co, Ni, Cu, or Fe) nanoparticle anodes can exhibit highly reversible electrochemical capacities as high as 1000 mAhg1(e. g., Fe2O3).[103,104] The energy storage mechanisms for these materials differ from the classical Li insertion/deinsertion or Li-alloying processes. Transition metal oxides undergo conversion reactions involving the reversible formation and decomposition of Li2O, accompanying the reduction and oxidation of metal nanoparticles:[103,105] MaObþ2�bð ÞLiþþ2�bð Þe$aM þbLi2O where Mis a transition metal oxide, such as Mn, Fe, Co, Ni, Cu, Ru, Cr, Mo, W, etc.[105] Silicon has also been considered as a suitable alternative to the conventional graphite anode due to its high specific capacity (~4200 mAhg1, lithiated to Li4.4Si).[106] However, the use of silicon as an anode material in batteries has been limited due to significant volume variation upon cycling, which leads to electrode pulverization and quick capacity fade.[107] Over the past decade, several strategies have been developed to alleviate these shortcomings. To prevent electrode pulverization, nanostructures such as nanoparticles, nanolayers, nanowires, and nanotubes have been designed to address Si volume variation.[66,107,108] As shown in Figure 6A, below a critical size threshold (Dc) of ~150 nm, particle fracture pulverization can be prevented. For example, Beydaghi et al.,[65] demonstrated demonstrated the fabrication of Si nanoparticlebased electrodes using a simple and cost-effective FDM Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 144/154] 1 ChemElectroChem 2024,11, e202400206 (9 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License processing in the light-based or as deposition with assisted drying in the AJP has helped with the improved performance.[21,30] Material-wise, a huge effort has been made to adapt common materials and inks to their implementation in printed devices. Due to how driven 3D printing is by sustainability, most of the work in the field has been focused on the use of LFP as cathode material and only high-energy applications have been using NMC and LCO. Regarding the anode choices, LTO has received significantly more attention in 3D printing than typical alternatives such as graphite due to its zero-volume expansion, especially in solid-state batteries. One of the main reasons for the use of 3D printing strategies with standard types of materials has been the higher thicknesses achievable compared to slurry cast procedures. This allows higher energy densities compared with typical electrodes even without the use of advanced architectures (Figure 12). Nanomaterials have been found in 3D printing as a natural ally. Despite their high promises, nanomaterials have not entered yet the production lines of state-of-the-art batteries, and their low maturity has only made them reach some niche fields such as IoT applications and wearables. One of their main limitations is the upscaling of nanomaterial-based battery electrodes. They suffer from the lack of standardized metrics and a plethora of materials synthesis routes, that might not be compatible with regular, industrial production lines. In this regard, their combination with 3D printing has been ideal both in the material processing perspective as well as in the application perspective. Some printing methodologies such as IJP have insurmountable limitations on material size and ink rheology, and nanomaterial-based colloidal dispersions are a perfect fit for them. This also applies to applications such as micro batteries, where the higher gravimetric capacities of the nanomaterials, their easy processability in inks, and extra functionalities such as flexibility compensate for their higher cost (Figure 12). Of course, the integration of nanomaterialbased printed devices is not free of challenges, and issues such as tab detachment from carbon substrates are still problematic. With the push for sustainable choices for energy storage materials, ROMs have been gaining momentum lately. Although CCs are largely unexplored for printed devices and only a few quinone-based examples exist, it is expected that their popularity will boom in the next few years. This is due to the rise of fields like smart packaging where the high volume requires a sustainable and cheap power source whose performances are not necessarily very high. Due to their sheer number, the waste management of this type of application is very challenging thus easy recycling or non-toxic degradation is a priority for the materials that compose them (Figure 12).[175] Reversely, CPs have been extensively used in printed electrodes. Their approach is very different from that of the CCs and is generally used as redox-active binders and conductive additives with high-performing materials such as nanomaterials. Their high cost prevents its wide adoption thus their integration is aimed at niche applications similar to nanomaterials and mostly accompanying them. Regarding printed electrolytes, since there are no commercial solid-state batteries that can serve as a reference for the industrially preferred type of solid electrolyte, it is not clear whether ceramic or polymeric SEs will become the main choice. It is likely that once the first solid-state batteries are commercially available, the printing field will adopt its electrolyte choice too. For now, polymeric, and composite SEs seem to be the most promising thanks to their easy printability and good interfaces. Additionally, they align well with some of the extra functionalities that are desired for printed devices, such as flexibility, and require minimal post-processing treatments. Still, fully SEs cannot compete in performance with liquid electrolytes, and thus QSEs are still the preferred way to achieve fully printed batteries. This field is rapidly evolving and heavily influenced by the trends marked by the EV sector. We are now at a crossroads between different technologies, and after the market deployment of solid-state batteries takes place, we will see a massive boom in the interest in the use of 3D printing strategies for their production. Figure 12. Schematic summary of the main advantages that the 3D printing technology brings to each of the electrode material class and the main applications for which each family is being proposed. Wiley VCH Dienstag, 25.06.2024 2413 / 351827 [S. 151/154] 1 ChemElectroChem 2024,11, e202400206 (16 of 19) © 2024 The Authors. ChemElectroChem published by Wiley-VCH GmbH ChemElectroChem Review doi.org/10.1002/celc.202400206 21960216, 2024, 13, Downloaded from https://chemistry-europe.onlinelibrary.wiley.com/doi/10.1002/celc.202400206 by Universidad De Sevilla, Wiley Online Library on [30/09/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License 6. Abbreviations 0DCFN Zero-Dimensional Carbon-based Filament Network ABS Acrylonitrile Butadiene Styrene AJP Aerosol Jet Printing AM Additive Manufacturing CCs Carbonyl Compounds CMC Carboxymethyl Cellulose CNTs Carbon Nanotubes COFs Covalent Organic Frameworks CPs Conducting Polymers CSEs Composite Solid Electrolytes DB Disperse Blue 134 anthraquinone DIW Direct Ink Writing EC Ethylene Carbonate EESDs Electrochemical Energy Storage Devices ESD Energy Storage Device EVs Electric Vehicles FDM Fused Deposition Modeling IJP Inkjet Printing IoT Internet of Things LAGP Lithium Aluminum Germanium Phosphate LCO Lithium Cobalt Oxide LFP Lithium Iron Phosphate LIBs Lithium-Ion Batteries LLZO Lithium Lanthanum Zirconium Oxide LMO Lithium Manganese Oxide LTO Lithium Titanate MOFs Metal-Organic Frameworks *NCA Lithium Nickel Cobalt Aluminum Oxide NMC Nickel Manganese Cobalt Oxide PAA Polyacrylic Acid PANI Polyaniline PAQS Poly (anthraquinone sulfide) PC Polycarbonate PEDOT:PSS Poly(3,4-ethylenedioxythiophene) Polystyrene Sulfonate PEG Polyethylene Glycol PEO Polyethylene Oxide PLA Polylactic Acid PoPD Poly(ortho-phenylenediamine) PPO Polypropylene Oxide PVDF Polyvinylidene Fluoride PVA Polyvinyl Alcohol QSEs Quasi-Solid Electrolytes rGO Reduced Graphene Oxide ROMs Redox-Active Organic Materials SEI Solid Electrolyte Interphase SEs Solid Electrolytes SiNPs Silicon Nanoparticles SLA Stereolithography SLS Selective Laser Sintering SPEs Solid Polymeric Electrolytes UV Ultraviolet ZIBs Zinc Ion Batteries Acknowledgements S.P. and T.G. gratefully acknowledge financial support from “Comunidad de Madrid” to the project ADEMOSSBat (2022-T1/ IND-23776). J.C. acknowledges the EMERGIA Junta de Andalucia program (EMC21_00174) for financial support. J.M. acknowledges the financial support from SFI AMBER and SFI Frontiers for the Future by two grants from Science Foundation Ireland under Grants Nos. 12/RC/2278_P2 and 20/FFPA/8950. Conflict of Interests The authors declare no conflict of interest. Keywords: additive manufacturing ·3D printing ·batteries · electrochemical energy storage ·metal-ion batteries [1] J. P. Mensing, T. Lomas, A. Tuantranont, Sustain. Mater. Technol. 2020, 25, e00190. [2] T.-S. Wei, B. Y. Ahn, J. Grotto, J. A. Lewis, Adv. Mater. 2018,30, 1703027. [3] C. M. Costa, R. Gonçalves, S. Lanceros-Méndez, Energy Storage Mater. 2020,28, 216–234. [4] Z. Lyu, G. J. H. Lim, J. J. Koh, Y. Li, Y. Ma, J. Ding, J. Wang, Z. Hu, J. Wang, W. Chen, Y. Chen, Joule 2021,5, 89–114. [5] Y. Mu, Y. Chu, L. Pan, B. Wu, L. Zou, J. He, M. Han, T. Zhao, L. Zeng, Int. J. Extreme Manuf. 2023,5, 042008. [6] D. Mouraliraman, A. Thiagarajan, S. 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